1 s2.0 S0003267019302259 Main

Analytica Chimica Acta xxx (xxxx) xxx
Contents lists available at ScienceDirect
Analytica Chimica Acta

journal homepage: www.elsevier.com/locate/aca
Review
QuEChERS - Fundamentals, relevant improvements, applications and

future trends
Rosa Perestrelo a, *, Pedro Silva a, Priscilla Porto-Figueira a, Jorge A.M. Pereira a,
Catarina Silva a, Sonia Medina a, Jose S. Ca^mara a, b
a
CQM e Centro de Química da Madeira, Universidade da Madeira, Campus da Penteada, 9020-105, Funchal, Portugal
b
Departamento de Química, Faculdade de Ci^
encias Exatas e Engenharia, Universidade da Madeira, Campus da Penteada, 9020-105, Funchal, Portugal
h i g h l i g h t s g r a p h i c a l a b s t r a c t
Modification and miniaturization of

QuEChERS method.
An updated overview of the most
recent QuEChERS applications.
QuEChERS combined with GC- and
LC-MS/MS provided low detection
limits and high recoveries.
QuEChERS performance compared to
other extraction approaches.
a r t i c l e i n f o a b s t r a c t
Article history: The Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method is a simple and straightforward
Received 13 September 2018 extraction technique involving an initial partitioning followed by an extract clean-up using dispersive
Received in revised form solid-phase extraction (d-SPE). Originally, the QuEChERS approach was developed for recovering pesti-
16 February 2019
cide residues from fruits and vegetables, but rapidly gained popularity in the comprehensive isolation of
Accepted 24 February 2019
Available online xxx
analytes from different matrices. According to PubMed, since its development in 2003 up to November
2018, about 1360 papers have been published reporting QuEChERS as extraction method. Several papers
have reported different improvements and modifications to the original QuEChERS protocol to ensure
Keywords:
QuEChERS
more efficient extractions of pH-dependent analytes and to minimize the degradation of labile analytes.
Fundamentals This analytical approach shows several advantages over traditional extraction techniques, requiring low
Relevant improvements sample and solvent volumes, as well as less time for sample preparation. Furthermore, most of the
Novel applications published studies show that the QuEChERS protocol provides higher recovery rate and a better analytical
performance than conventional extraction procedures.
This review proposes an updated overview of the most recent developments and applications of
QuEChERS beyond its original application to pesticides, mycotoxins, veterinary drugs and pharmaceu-
ticals, forensic analysis, drugs of abuse and environmental contaminants. Their pros and cons will be
discussed, considering the factors influencing the extraction efficiency. Whenever possible, the perfor-
mance of the QuEChERS is compared to other extraction approaches. In addition to the evolution of this
technique, changes and improvements to the original method are discussed.
© 2019 Elsevier B.V. All rights reserved.
* Corresponding author.
E-mail address: rmp@uma.pt (R. Perestrelo).
https://doi.org/10.1016/j.aca.2019.02.036
0003-2670/© 2019 Elsevier B.V. All rights reserved.
Please cite this article as: R. Perestrelo et al., QuEChERS - Fundamentals, relevant improvements, applications and future trends, Analytica
Chimica Acta, https://doi.org/10.1016/j.aca.2019.02.036
2 R. Perestrelo et al. / Analytica Chimica Acta xxx (xxxx) xxx
Contents
1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
2. The original QuEChERS method and relevant improvements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
2.1. Overview of QuEChERS improvements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
2.1.1. Sorbents for clean-up QuEChERS extracts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
2.1.2. QuEChERS miniaturization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
3. QuEChERS applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
3.1. Food analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
3.2. Food safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
3.2.1. Pesticides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
3.2.2. Mycotoxins . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
3.2.3. Other food contaminants . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
3.3. Pharmaceutical and clinical analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
3.4. Environmental contaminants . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
3.5. Multiclass analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
4. Comparison of QuEChERS with other extraction methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
5. Recommendations and future outlooks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
Declaration of interest . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
Acknowledgments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
Supplementary data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
Abbreviations HPLC-UV High performance liquid chromatography with

ultraviolet detection
ACFs Activated carbon fibres IAC Immunoaffinity columns
Al2O3 Aluminium oxide IL-DLLME Ionic liquid-dispersive liquideliquid microextraction
ASE Accelerated solvent extraction (or equivalent IMS Ion mobility spectrometry
pressurized solvent extraction, PSE, or pressurized K2CO3 Potassium carbonate
liquid extraction, PLE) LC-MS/MS Liquid chromatography tandem mass spectrometer
C18 Octadecyl silica LDS-DLLME Low-density solvent dispersive liquideliquid
CaCl2 Calcium chloride microextraction
CCl4 Carbon tetrachloride LLE Liquid-liquid extraction
C6H5Na3O7 Sodium citrate LOD Limit of detection
COPs Cholesterol-oxidation products LOQ Limit of quantification
DCM Dichloromethane MAE Microwave-assisted extraction
DLLME Dispersive liquid-liquid microextraction ME (%) Matrix effect
d-SPE Dispersive solid-phase extraction MeCN Acetonitrile
d-mSPE Dispersive microsolid-phase extraction ME-IL-VALLME Micellar extraction combined with ionic liquid-
EDTA Ethylenediaminetetraacetic acid based vortex-assisted liquid-liquid
EDTA-Na2 Ethylene diamine tetraacetic acid disodium microextraction
EFSA European Food Safety Authority Meo-PBDEs Methoxylated polybrominated diphenyl ethers
ELISA Enzyme linked immunosorbent assay MeOH Methanol
EMR-lipid Enhanced matrix removal-lipid MCPD 3-Monochloropropane-1,2-diol
EPA Environmental Protection Agency m-FC Multi-filtration clean-up
EtAc Ethyl acetate MgSO4 Magnesium sulfate
FA Formic acid MMLs Mycotoxins maximum levels
Fe3O4-PSA Iron oxide - primary secondary amine m-PFC Multi-plug filtration clean-up
FLR Fluorescence detector MRLs Maximum residue limits
FS Fluorinated sorbent MS Mass spectrometry
GCB Graphitized carbon black MWCNTs Multi-walled carbon nanotubes
GC-ECD Gas chromatography electron capture detector NaOAc Sodium acetate
GC-mECD Gas chromatography micro-electron capture detector NAC Nitrogen-enriched activated carbon
GC-MS Gas chromatography mass spectrometry NaCl Sodium chloride
GC-MS/MS Gas chromatography tandem mass spectrometry NaHCO3 Sodium bicarbonate
GPC Gel permeation chromatography NaOH Sodium hydroxide
H2O Water Na2SO4 Sodium sulfate
HAc Acetic acid NBFRs Novel brominated flame retardants
HEX Hexane NH4CH3CO2 Ammonium acetate
HMF Hydroxymethylfurfural NH4Cl Ammonium chloride
HPLC-PDA High performance liquid chromatography tandem NH4HCO2 Ammonium formate
photodiode array detector NOAA National Oceanic and Atmospheric Administration
R. Perestrelo et al. / Analytica Chimica Acta xxx (xxxx) xxx 3
OCPs Organochlorine pesticides ESCF European Commission's Scientific Committee for

OPPs Organophosphorus pesticides Food
PAEs Phthalates SCTD Sodium citrate tribasic dihydrate, C6H5Na3O7$2H2O
PAHs Polycyclic aromatic hydrocarbons SCX Strong cation exchange
PBDEs Polybrominated diphenyl ethers SE Solvent extraction
PCBs Polychlorinated biphenyls Si Silica gel
PCDD/Fs Polychlorinated dibenzodioxins and dibenzofurans SLE Solid-liquid extraction
PPCPs Pharmaceutical and personal care products SMCs Synthetic musk compounds
PDA Photodiode array detector SnO2 Tin (IV) oxide
PLE Pressurized liquid extraction SPE Solid-phase extraction
POPs Persistent organic pollutants SPME Solid-phase microextraction
PPT Protein precipitation TFA Trifluoroacetic acid
PSA Primary secondary amine tri-BuA-rGO Tributylamine-functional reduced graphene oxide
QACs Quaternary ammonium compounds UHPLC-MS/MS Ultrahigh-performance liquid chromatography
QuEChERS Quick, Easy, Cheap, Effective, Rugged and Safe tandem mass spectrometer
Rec (%) Recovery USE Ultrasonic solvent extraction
r-DSPE Reversed-dispersive solid-phase extraction UV Ultraviolet detection
RSD (%) Relative standard deviation UVFs Ultraviolet filters
SAX Strong anion exchange ZEA Zearalenone
SBSE Stir bar sorptive extraction ZnO Zinc oxide
SCDS Sodium citrate dibasic sesquihydrate, Z-Sep Zirconium dioxide based sorbents
C6H6Na2O7∙1.5H2O
1. Introduction of extract and sorbent, and allows the reduction or elimination of

additional centrifugation, filtration and/or precipitation steps
Analytical chemists are continuously challenged to develop [22,23].
faster, greener, precise and accurate methods capable of guaran- Despite this simple experimental layout, the effectiveness of the
teeing quality, authenticity, safety and traceability of target com- QuEChERS method depends on the target analyte properties, ma-
pounds in a diversity of sample matrices [1]. In this context, the trix composition, equipment and analytical techniques available in
Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method the laboratory. Thus, during the development of a QuEChERS pro-
is one of the most promising user-friendly and high throughput tocol, several parameters affecting the extraction efficiency should
extraction procedure, involving reduced sample amounts and be considered and optimized. In this context, and as a first
organic solvents in addition to laboratory glassware, in agreement approach, researchers should consider the extraction solvent,
of green chemistry principles. sample amount, extraction solvent, sample/solvent ratio, pH, type
The QuEChERS method was first introduced at the European and amount of partitioning salt to improve the salting-out effect.
Pesticide Residue Workshop (EPRW) 2002 in Rome, published in Regarding the clean-up step, both the sorbent types (and eventu-
2003 by Anastassiades et al. [2], and subsequently validated by ally partitioning salts) and sorbent amount should be optimized. In
Lehotay et al. [3]. The original approach was developed to recover sum, the selectivity of extraction can be adjusted and improved by
pesticide residues from fruit and vegetables covering a broad an- the selection of the most efficient extraction solvents, partitioning
alyte spectrum, ranging from nonpolar to very polar pesticides. salts and their relative amounts and proportions, and buffer con-
Following these initial reports [2,3], the method was rapidly and ditions (acid/basic buffer) [24].
widely adopted by the scientific community. In fact, according to In this paper, the fundamentals, relevant improvements and
PubMed, around 1360 papers focused on the QuEChERS approach high-throughput applications of QuEChERS method in different
were published, most of which involving multiresidue pesticide fields including-food, pharmaceutical, forensic and environmental
analysis in food matrices [4e14]. Based on its inherent advantages sciences, is reviewed. Based on the literature mining performed
and great versatility, the QuEChERS method has gained significant using the PubMed search engine, several works reported in peer
popularity and has expanded its range of application, outside of its reviewed journals since 2014, in these different fields of research,
traditional domain, to the extraction of different analytes (e.g. are presented. In addition, the performance of the QuEChERS
polyphenols, amines, antidepressants, environmental pollutants, method is compared with that of other extraction methods,
among others) from several matrices including, foods [4,10,13,15], including solid-phase extraction (SPE), liquid-liquid extraction
biological fluids [16e19], and environmental samples [20,21]. (LLE), accelerated solvent extraction (ASE), ultrasound assisted
QuEChERS is an effective sample preparation approach based on extraction (UAE), and microwave-assisted extraction (MAE).
the dispersion of salts to extract (salting-out effect), isolate a wide Whenever possible, the advantages (pros) and disadvantages
range of analytes from very complex matrices in addition to the (cons) of each extraction method relative to the QuEChERS method
clean-up of the extract. This effective and easy preparation are critically reviewed.
approach involves two steps: i) an extraction step based on parti-
tioning via salting-out extraction where an equilibrium between an 2. The original QuEChERS method and relevant
aqueous and an organic layer (acetonitrile - MeCN) is promoted; improvements
followed by ii) a dispersive solid-phase extraction (d-SPE) step that
involves further clean-up using several combinations of porous Overall, QuEChERS is a cheap and flexible method. Its key pa-
sorbents and salts to remove matrix interfering substances (Fig. S1, rameters can be easily modified and optimized to improve
Supplementary Material). The latter step requires a smaller amount extraction efficiency and increase its potential application in a wide
range of different fields and matrices. It is viewed as a reliable [42,43]) were used to enhance the extraction efficiency. Both op-
alternative for the extraction of a huge diversity of analytes from tions are currently used by numerous researchers and have become
different chemical families and from different matrices [7,8,25,26]. the official method for pesticide residue analysis (AOAC Official
Method 2007.01, and CEN Standard Method EN 15662). In the
2.1. Overview of QuEChERS improvements meantime, additional buffer systems have been proposed, namely
phosphate buffer for more alkaline extractions [44,45].
Sample preparation is often a key parameter in the development The nature of the extraction solvent can be modified according
of new analytical methods, particularly in the isolation/detection of to the target analyte. In the original QuEChERS procedure [2], MeCN
residual/trace analytes [8,27]. Since its introduction by Anas- was selected because it was shown to extract the broadest range of
tassiades et al., in 2003 [2], and in order to improve the overall organic compounds without co-extraction of large amounts of
technique performance, the original QuEChERS method has been lipophilic material. Shabeer et al. [7], for instance, used MeCN in the
submitted to several modifications (Fig. 1). The salts commonly determination of 243 pesticides in cardamom (Elettaria cardamo-
used in the original and citrate QuEChERS versions were magne- mum) using gas chromatography tandem mass spectrometry (GC-
sium sulfate (MgSO4) and sodium chloride (NaCl) in either 2:1 or MS/MS). The limit of quantification (LOQ) was lower than 0.01 mg/
4:1 ratio (MgSO4:NaCl, w/w) [25,28e30]. In case of the citrate kg, and the recovery ranged from 70 to 120%, with a relative
version, sodium citrate tribasic dihydrate (C6H5Na3O7$2H2O, SCTD) standard deviation (RSD) lower than 20% for the majority of pes-
and sodium citrate dibasic sesquihydrate (C6H6Na2O7∙1.5H2O, ticides. Zheng et al. [44] also used MeCN in the determination of
SCDS) were also added in a 2:1 ratio (w/w) [8,31,32]. In contrast, the cymiazole, fipronil, coumaphos, fluvalinate, amitraz, and its me-
salts used in the acetate version were MgSO4 and sodium acetate tabolites in various types of honey and royal jelly, while Bessaire
(NaOAc) in a 6:1.5 ratio (w/w) [33e35]. et al. [45] reported MeCN as a solvent for screening b-lactam an-
Most of the improvements associated with the QuEChERS tibiotics in foodstuffs. Faraji et al. [46] also used the same solvent in
method include the optimization of amount and combinations of the determination of pesticides in pistachio. As can be observed in
solvents and salts, according to the chemical nature of target ana- Table 1, lower LOQs and good recoveries were achieved (70e120%),
lytes. These key parameters can play a relevant impact on the from QuEChERS application in different fields. However, to improve
extraction efficiency [10,12,36e40]. The reduction of matrix effects, the extraction efficiency of target analytes some solvent modifica-
the increase in sensitivity and the recovery of target analytes in tions have been proposed, namely acidified MeCN with formic acid
complex matrices, which improve the analytical performance of (FA) [10,25,47,48], acetic acid (HAc) [4,27,33,49] and citric acid [50],
the entire method, are some of the reasons that justify the opti- as well as a combination of MeCN with other solvents such as ethyl
mization of the QuEChERS protocol [9]. In the original method, the acetate (EtAc) [12,51], methanol (MeOH) [37,52,53], dichloro-
first step of the experimental layout was performed under unbuf- methane (DCM) [54], and hexane (HEX) [55]. In this context,
fered conditions [2]. Under such conditions the analysis of sensitive Reichert et al. [4] optimized and validated a MeCN-based QuECh-
compounds that degrade at high or low pH values may be limited. ERS method for the simultaneous extraction of 117 pesticides and
To overcome this drawback, citrate buffer (relatively low buffering 30 mycotoxins from raw coffee beans followed by liquid chroma-
capacity [41]) and/or acetate buffer (strong buffering capacity tography tandem mass spectrometry (LC-MS/MS) determination.
Fig. 1. Relevant improvements in QuEChERS protocol. Abbreviation: d-SPE - dispersive solid-phase extraction, EtAc e ethyl acetate, FLR - fluorescence detector, GC - gas chro-
matography, LC - liquid chromatography, LOD - limit of detection, LOQ - limit of quantification, MeCN e acetonitrile, MeOH e methanol, MS - mass spectrometry, PDA - photodiode
array detector, PSA - primary secondary amine, SCDS - Sodium citrate dibasic sesquihydrate, SCTD - sodium citrate tribasic dihydrate, Z-Sep - Zirconium dioxide based sorbents.
Table 1
Application fields of QuEChERS.
Matrices (target analytes)a QuEChERS Analytical method Validation parameters Ref
Extraction Solvents Partition salts/Buffers Clean-up Rec. (%) LOQ
Food analysis
Baby foods (12 Phenolic compounds) MeCN 200 mg of salts (MgSO4, d-SPE (75 mg MgSO4, 12.5 mg PSA) UHPLC-PDA 71e100 0.13e1.54 mg/g [97]
NaCl, SCTD, SCDS, 4:1:1:0.5
w/w)
Food sample (Methyl eugenol) EtAc 2 g MgSO4, 500 mg NaCl d-SPE (500 mg MgSO4, 100 mg PSA) GC-MS/MS 94e100 1e50 mg/kg [106]
Grapes (Trans-resveratrol) MeCN:EtAc (1:1 v/ 4 g MgSO4, 1 g NaCl, 1 g d-SPE (150 mg MgSO4, 25 mg PSA, UHPLC-PDA 75e100 10 ng/mL [12]
v) with 1% FA SCTD, 0.5 g SCDS 25 mg C18)
Guava leaves (Ursolic acid, oleanolic MeOH None d-SPE (150 mg MgSO4, 50 mg PSA, HPLC-UV 97e111 0.6e1.2 mg/mL [105]
acid) 50 mg C18)
Meat (Cholesterol, 7 COPs) Acetone 4 g MgSO4, 1 g NaOAc d-SPE (300 mg C18EC, 900 mg MgSO4, GC-MS 0.32e400 ng/g [107]
300 mg PSA)
Red wines (4-Ethylphenol, 4- MeCN 4 g MgSO4, 1.5 g NaCl d-SPE (100 mg CaCl2, 25 mg PSA) HPLC-UV 73e116 24e40 mg/L [6]
ethylguaiacol, 4-vinylphenol, 4-
vinylguaiacol)
Red and white wines (3-Isopropyl-, 3- Toluene 12 g MgSO4, 3 g NaCl d-SPE (25 mg CaCl2, 25 mg MgSO4, GC-MS 71e87 13.9e23.6 ng/L [14]
isobutyl- and 3-sec-butyl-2- 10 mg PSA)
R. Perestrelo et al. / Analytica Chimica Acta xxx (xxxx) xxx

methoxypyrazine)
Red wines (Trans-resveratrol) MeCN 3 g MgSO4, 1 g NaCl d-SPE (300 mg MgSO4, 300 mg PSA) LC-MS/MS 75e111 5 ng/mL [57]
Food Safety Pesticides
Apple, mushroom, tea (15 Carbamate MeCN 1 g NaCl, 2 g Na2SO4 d-SPE (200 mg Na2SO4, 150 mg PSA, LC-MS/MS 88e118 0.5e5 mg/kg [108]
pesticides) 50 mg C18)
Baby foods (Haloxyfop, haloxyfop- MeCN 4 g MgSO4, 1 g NaCl d-SPE (150 mg MgSO4, 50 mg C18) UHPLC-MS/MS 92e114 0.003 mg/kg [66]
methyl)
Beans, soils (Chlorpyrifos, fluopyram, MeCN 9 g MgSO4, 3 g NaCl d-SPE (1.15 g MgSO4, 400 mg PSA) LC-MS/MS 88e110 <0.05 mg/kg [67]
fluopyram benzamide, tebuconazole)
Beef meat (188 Pesticides) MeCN with 1% 4 g MgSO4, 1 g NaOAc d-SPE (150 mg MgSO4, 30 mg PSA, LC-MS 70e120 10e25 mg/kg [26]
HAc:EtAc (70:30 v/ 30 mg C18)
v)
Brown rice, orange, spinach (310 MeCN with 0.1% FA 4 g MgSO4, 1 g NaCl d-SPE (25 mg PSA, 150 mg MgSO4, UHPLC-MS/MS 87e96 10e20 ng/g [25]
Pesticides) 7.5 mg GCB)
Cardamom (243 Pesticides) MeCN 4 g MgSO4, 1 g NaCl d-SPE (25 mg PSA, 100 mg C18, 10 mg GC-MS/MS 70e120 ˂ 0.01 mg/kg [7]
GCB)
Cereals (Ethoxysulfuron, halosulfuron- MeCN with 1% FA 10 g MgSO4, 1 g NaCl d-SPE (1200 mg MgSO4, 150 mg PSA, LC-MS/MS 70e120 0.5e1.0 mg/kg [109]
methyl, mesosulfuron-methyl and 200 mg C18)
orthosulfamuron)
Cheese (28 Carbamate residues) MeCN with 1% HAc 4 g MgSO4, 1 g NaCl d-SPE (100 mg Z-Sepþ) UHPLC-MS/MS 70e115 0.5e4.7 mg/kg [29]
Chicken egg, muscle, cake (Fipronil and MeCN 1 g NaCl d-SPE (100 mg MgSO4, 50 mg PSA, LC-MS/MS 87e119 0.2e5 ng/kg [110]
its metabolites) 100 mg C18)
Citrus, soil (Spirotetramat and its 4 MeCN with 1% HAc 3 g NaCl d-SPE (50 mg PSA, 50 mg C18) LC-MS/MS 71e115 0.02e0.40 mg/ [111]
metabolites) kg
Coffee leaf extracts (52 Pesticides) MeCN 6 g MgSO4, 1.5 g NaCl, 1.5 g d-SPE (150 mg MgSO4, 50 mg PSA, UHPLC-MS/MS 87e94 0.075e2.25 ng/ [112]
SCTD, 0.75 g SCDS 50 mg C18) g
Cucumbers, soil (Boscalid, triflumizole MeCN 4 g MgSO4, 1 g NaCl d-SPE (150 mg MgSO4, 50 mg PSA) LC-MS/MS 82e102 0.01e0.05 mg/ [68]
and FM-6-1) kg
Cucumbers, soil (8 Neonicotinoid MeCN 4 g MgSO4, 1 g NaCl d-SPE (800 mg MgSO4, 400 mg C18) HPLC-MS/MS 82e96 0.26e20 ng/g [36]
insecticide residues and 2 primary
metabolites)
Cucumbers, soil (5 Neonicotinoid MeCN:DCM (1:2 v/ 5 g NaCl d-SPE (400 mg C18) HPLC-DAD 98e102 0.018 [54]
insecticide residues) v) e0.366 mg/g
Cucumber, soil (Fluopyram, benzamide) MeCN with 1% HAc 6 g MgSO4, 1.5 g NaOAc d-SPE (900 mg MgSO4, 300 mg PSA) LC-MS/MS 87e108 0.05 mg/kg [34]
Food commodities (Propoxycarbazone, MeCN with 1% HAc 4 g MgSO4, 1 g NaOAc d-SPE (150 mg MgSO4, 50 mg PSA, UHPLC-MS/MS 73e110 10e25 mg/kg [113]
2-hydroxy-propoxycarbazone) 50 mg C18)
Fish tissue (13 OCPs) MeCN 4 g MgSO4, 1 g NaCl d-SPE-DLLME-SFO (50 mg PSA; GC-ECD 88e121 1.94e4.93 mg/ [114]
6 mL H2O, 40 mL 1-undecanol) kg
(continued on next page)
5
Table 1 (continued )
6
Fish tissue (5 OCPs) Acetone: HEX (1:1 4 g MgSO4, 1 g NaCl, 2 g d-SPE (100 mg PSA, 23 mg C18, 400 mg GC-ECD 77e111 0.8e9.6 mg/kg [99]
v/v) Na2SO4 MgSO4)
Fruit, soil (Carbendazim) MeCN 6 g MgSO4, 1.5 g NaOAc d-SPE (100 mg C18, 200 mg PSA, 600 mg LC-MS/MS 79e96 0.005e0.1 mg/ [115]
MgSO4) kg
Fruits, vegetables (20 Pesticides) MeCN 3 g NaCl d-SPE (10 mg MgSO4, 10 mg PSA) GC-ECD 80e120 0.01e0.05 mg/ [38]
kg
Fruits, vegetables (4 Pesticides and its MeCN 4 g MgSO4, 1 g NaCl, 1 g d-SPE (750 mg MgSO4, 125 mg PSA) GC-MS/MS e 0.010 mg/kg [31]
transformation products) SCTD, 0.5 g SCDS
Grape (Difenoconazole) MeCN with 1% HAc 2 g MgSO4, 0.5 g NaOAc d-SPE (1.5 g MgSO4, 450 mg PSA, SERS e e [58]
450 mg C18)
Grape, soil (Boscalid, pyraclostrobin) Acetone 4 g MgSO4, 1 g NaCl d-SPE (150 mg MgSO4, 50 mg PSA, 8 mg RRLC-QqQ-MS/MS 82e104 0.001 mg/kg [62]
MWCNT)
Grape (Carbendazim tebuconazole, MeCN 4 g MgSO4, 1 g NaCl d-SPE (150 mg MgSO4, 50 mg PSA, 3 mg LC-MS/MS 83e105 0.021e0.87 mg/ [63]
thiophanate-methyl) MWCNT) L
Honey, royal jelly (5 Pesticides, 1 MeCN 4 g MgSO4, 1 g NaCl, 1 g d-SPE (150 mg PSA, 150 mg C18, 900 mg LC-MS/MS 62e109 1e5 mg/kg [44]
metabolite) SCTD, 0.5 g SCDS MgSO4)
Honeybees (8 Pesticides) MeCN with HAc 0.5 g MgSO4, 2 g NaOAc d-SPE (1.25 g, PSA:C18:MgSO4:GCB, UHPLC-MS/MS 79e115 0.03e0.35 ng/ [116]

(0.1 N) 1:1:3:0.15 (w/w/w/w)) mL
Honeybee wax comb (160 Pesticides) MeCN 4 g MgSO4, 1 g NaCl, 1 g d-SPE (125 mg PSA, 125 mg C18, 750 mg GC-QqQ-MS 60e120 0.01e0.02 mg/ [117]
SCTD, 0.5 g SCDS MgSO4) kg
Kiwifruit (49 Pesticides) MeCN 4 g MgSO4, 1 g NaCl, 1 g d-SPE (25 mg PSA, 2.5 mg GCB, 150 mg LC-MS/MS 70e120 <5 mg/kg [118]
SCTD, 0.5 g SCDS MgSO4)
Lettuce, radish, strawberry (74 MeCN with 1% HAc 6 g MgSO4, 1.5 g NaOAc d-SPE (125 mg PSA, 125 mg C18, 750 mg LC-MS/MS 70e120 0.01e2 ng/g [35]
Pesticides) MgSO4)
Milk (30 Pesticides) MeCN 8 g MgSO4, 2 g NaCl d-SPE (125 mg PSA, 25 mg Z-Sep, 5 mg HPLC-PDA 70e120 0.07e0.19 mg/ [9]
Z-Sep Plus) mL
Milk, cheese, cream (167 Pesticides) MeCN 4 g MgSO4, 1 g NaCl, 1 g d-SPE (150 mg PSA, 400 mg C18, 900 mg LC-MS/MS 80e117 1.1e13.1 mg/kg [8]
Organic lettuce (16 Pesticides) MeCN 4 g MgSO4, 1 g NaCl, 1 g d-SPE (175 mg PSA, 35 mg GCB, UHPLC-MS/MS 70e120 3e3200 mg/kg [32]
SCTD, 0.5 g SCDS 1050 mg MgSO4)
Pear (Thiophanate-methyl, MeOH None d-SPE (75 mg C18) LC-MS/MS 75e85 4e20 mg/kg [119]
carbendazim)
Pistachio (Acetamiprid, imidacloprid, MeCN 4 g MgSO4, 1 g NaCl, 4 g d-SPE (150 mg PSA, 15 mg GCB) LC-MS/MS 73e125 5 mg/kg [46]
spirotetramat and their relevant NaHCO3, citrate buffer
metabolites)
Polyphenol-rich agricultural products MeCN 2 g MgSO4, 2 g NaCl d-SPE (150 mg PVPP, 50 mg PSA, 10 mg UHPLC-MS/MS 73e106 0.01e0.02 mg/ [64]
(20 Pesticides) GCB) kg
Potatoes, soil (Fluazinam, MeCN 3 g NaCl d-SPE (150 mg PSA, 150 mg C18, 150 mg UHPLC-MS/MS 87e114 2e5 mg/kg [59]
dimethomorph) MgSO4)
Raw honeys (24 Pesticides) MeCN with 1% HAc 6 g MgSO4, 1.5 g NaOAc d-SPE (1200 mg MgSO4, 400 mg PSA) GC-mECD/FTD, GC-MS 86e108 8.4e27.3 ng/g [120]
Red Swamp Crayfish (60 Pesticides) MeCN 3 g NaCl d-SPE (50 mg PSA) HPLC-MS/MS 70e120 1e16 ng/g [121]
Rice (20 Pesticides and 1 related MeCN with 1% HAc 6 g MgSO4, 1.7 g NaOAc d-SPE (250 mg MgSO4, 125 mg chitosan LC-MS/MS 70e120 5e20 mg/kg [80]
metabolite) or 75 mg C18)
Rice, wheat, soybean (50 Pesticides and MeCN 4 g MgSO4, 1 g NaCl d-SPE (30 mg Fe3O4-PSA, 10 mg C18, LC-MS/MS 70e130 10 mg/kg [122]
8 related metabolites) 150 mg MgSO4)
Spices (205 Pesticides) MeCN 4 g MgSO4, 1 g NaCl, 1 g d-SPE (4 g MgSO4, 1 g NaCl) GC-MS/MS 41e122 50 ng/g [123]
SCTD, 0.5 g SCDS
Strawberries (7 OPPs) MeCN 4 g MgSO4, 1 g NaCl d-mSPE (10 mg Fe3O4@TEOS@MPS, GC-FPD, GC-MS 72e115 <13 mg/kg [124]
10 mg PSA)
Sugarcane, soil (Fipronil, fipronil EtAc 5 g MgSO4, 1.5 g NaOAc d-SPE (150 mg MgSO4, 50 mg PSA, GC-MS/MS 81e99 0.005 mg/g [125]
desulfinyl and fipronil sulfone) 50 mg C18)
Sweet green pepper (13 Pesticides) MeCN with 5% FA 4 g MgSO4, 1 g NaCl, 1 g d-SPE (1050 mg MgSO4, 175 mg PSA) LC-MS/MS 70e120 1e200 mg/kg [5]
SCTD, 0.5 g SCDS
Tea (33 Pesticides) MeCN 2.5 g NaCl d-SPE (100 mg tri-BuA-rGO) UHPLC-MS/MS, GCeMS/MS 72e120 1.0e54.9 mg/kg [126]
Teas (47 Pesticides) MeCN with 1% HAc 4 g MgSO4, 1 g NaCl d-SPE (45 mg MWCNTs, 75 mg PSA); GC-MS/MS 70e120 0.1e52.5 mg/kg [127]
DLLME (200 mL CCl4, 4 mL H2O)
Tomato (81 Pesticides) MeCN 2 g MgSO4, 1.5 g NaOAc d-SPE (60 mg MgSO4, 20 mg PSA) GC-MS 72e116 7.5e20 ng/g [128]
Tomato (Metribuzin, desamino- MeCN 2 g NaCl d-SPE (150 mg PSA, 180 mg GCB, GC-MS/MS 72e96 60e280 mg/kg [129]
metribuzin, diketo-metribuzin, 150 mg MgSO4)
desamino-diketo-metribuzin)
Tomato, sweet pepper (21 Pesticides) MeCN with 1% HAc 4 g MgSO4, 1.7 g NaOAc d-SPE (150 mg MgSO4, 75 mg FS) UHPLCeMS/MS 70e120 2.6e5.4 mg/kg [130]
Vegetables (35 Pesticides) MeCN 1.3 g MgSO4, 0.33 g NaCl, d-SPE (50 mg PSA, 15 mg GCB, 300 mg GC-MS/MS 67e126 0.3e14.2 mg/kg [131]
0.33 g SCTD, 0.16 g SCDS MgSO4)
Vegetables, fruit, soil (Afidopyropen MeCN 4 g MgSO4, 1 g NaCl d-SPE (150 mg MgSO4, 50 mg PSA) UHPLC-MS/MS 83e104 0.001 mg/L [132]
and its metabolite M440l007)
Virgin olive oil (162 Pesticides) MeCN with 1% HAc 4 g MgSO4, 1 g NaCl d-SPE (1 g EMR-lipid, 400 mg NaCl, Nanoflow LC-MS/MS 75e119 0.05e50 mg/kg [49]
1600 mg MgSO4)
Wheat, soil (Afidopyropen and its H2O:MeCN (3:10 v/ 2 g MgSO4, 1 g NaCl d-SPE (50 mg C18, 20 mg GCB, 150 mg UHPLC-MS/MS 81e114 1 ng/g [133]
metabolite) v) MgSO4)
Mycotoxins
Breakfast cereals (12 Mycotoxins and MeCN 4 g MgSO4, 1 g NaCl d-SPE (1350 mg MgSO4, 450 mg PSA) LC-MS/MS 46e93 0.004e18.4 mg/ [134]
theirs related metabolites) kg
Feed (13 Mycotoxins) MeCN:H2O (80:20 2 g MgSO4, 1.5 g NaCl d-SPE (90 mg MDN@Fe3O4) UHPLCeMS/MS 89e113 0.2e40 mg/kg [135]
v/v) with 3% HAc
Grape-, animal-derived products MeCN or MeCN 4 g MgSO4, 1 g NaCl d-SPE (150 mg MgSO4, 50 mg C18) UHPLC-MS/MS 70e115 0.1 mg/kg [136]
(Ochratoxin A) with 5% HAc
Grapes, wines (20 Mycotoxins) MeCN with 1% HAc 4 g MgSO4, 1 g NaCl d-SPE (450 mg MgSO4) UHPLC-MS/MS 86e118 0.18e30 mg/L [137]

Jujube (Tenuazonic acid, alternariol, MeCN with 0.1% 4 g MgSO4, 1 g NaCl d-SPE (1.2 g MgSO4, 400 mg PSA) UHPLC-MS/MS 83e109 0.47e0.87 mg/ [138]
alternariol monomethyl ether, HAc kg
tentoxin)
Liquorice (15 Mycotoxins) MeCN with 5% FA 4 g MgSO4, 1 g NaCl, 0.5 g d-SPE (900 mg MgSO4, 600 mg C18, UHPLC-MS/MS 81e105 0.13e2.5 mg/kg [139]
SCTD, 1 g SCDS 150 mg PSA, 150 mg Si)
Nuts, dried fruits (16 Mycotoxins) MeCN with 10 4 g MgSO4, 1 g NaCl d-SPE (300 mg C18) LC-MS/MS e e [50]
mMol/L citric acid
Ready-to-eat food (27 Mycotoxins) MeCN 4 g MgSO4, 1 g NaCl d-SPE (300 mg MgSO4, 100 mg C18) LC-MS/MS e e [140]
Red wine (Ochratoxin A) MeCN 2 g MgSO4, 500 mg NaCl SPE (60 mg ISOLUTE Myco cartridge) LC-MS/MS 89e105 0.05 mg/L [141]
Strawberries (Patulin) MeCN with 1% HAc 4 g MgSO4, 1 g NaCl, 1 g d-SPE (25 mg PSA, 7.5 mg GCB, 150 mg HPLC-DAD 99e103 5 mg/kg [142]
Tomate-based products (Alternariol, MeCN with 1% FA 4 g MgSO4, 500 mg NaCl d-SPE (25 mg PSA) LC-MS/MS 99e109 4e160 mg/kg [143]
tentoxin, alternariol monomethyl
ether, tenuaznic acid)
Vegetables (13 Mycotoxins) MeCN with 1% FA 4 g MgSO4, 1 g NaCl d-SPE (180 mg MgSO4, 180 mg C18, UHPLC-MS/MS 62e114 0.25e20 mg/kg [144]
60 mg Carbon SPE)
Vegetables oils (16 Mycotoxins) MeCN 4 g MgSO4, 1 g NaCl d-SPE (200 mg C18) LC-MS/MS 73e106 0.13e10 ng/g [145]
Food Contaminants
Animal-derived food products MeCN with 0.1% FA 4 g MgSO4, 1 g NaCl, 1 g d-SPE (150 mg C18, 900 mg MgSO4) LC-MS/MS 80e94 0.25 mg/kg [146]
(Bithionol residue) SCTD, 0.5 g SCDS
Animal-derived products (105 MeCN with 0.1% FA 4 g Na2SO4, 1 g NaCl, 1 g d-SPE (900 mg Na2SO4, 50 mg PSA, LC-MS/MS 70e120 e [56]
Veterinary drugs) SCTD, 0.5 g SCDS 150 mg C18)
Aquatic foods, edible oil, eggs, fruits, Acetone:HEX (1:1 4 g MgSO4, 1 g NaCl d-SPE (50 mg C18, 50 mg PSA, 50 mg GC-mECD 84e99 0.01e0.04 pg/g [147]
vegetable, cereals (8 PBDEs) v/v) ENVI-Carb)
Baby foods (Sulfonamides and their five MECN with 1% HAc 1.5 g NaOAc, 6 g MgSO4 d-SPE (150 mg PSA, 150 mg C18, 900 mg UHPLC-MS/MS 76e97 0.10e0.55 mg/ [148]
acetylated metabolites) MgSO4) kg
Baby foods (12 PAHs) MeCN 4 g MgSO4, 1 g NaCl d-SPE (600 mg MgSO4, 100 mg PSA, GC-MS 81e112 0.25e1 mg/kg [149]
100 mg C18), LDS-DLLME (75 mL
toluene)
Baby foods (14 PAEs) MeCN 4 g MgSO4, 1 g NaCl d-SPE (1200 mg MgSO4, 200 mg PSA) GC-MS/MS 72e120 0.33e1.11 mg/ [150]
kg
Bovine milk (5-Nitroimidazoles) MeCN 8 g MgSO4, 3 g NaCl d-SPE (25 mg PSA) HPLC-PDA 45e93 23e47 ng/mL [151]
Breast milk (Bisphenols S and A) MeCN with 1% FA 8 g MgSO4, 3 g NaCl d-SPE (45 mg Z-Sep, 5 mg Z-Sep Plus) LC-QqQ-MS 70e92 0.20e1.35 ng/ [152]
mL
Coffee (Acrylamide) MeCN:HEX (67:33 4 g MgSO4, 1 g NaCl d-SPE (0.15 mg PSA, 0.30 mg SAX, GC-MS 52e95 8 mg/kg [55]
v/v) 900 mg MgSO4)
Chicken muscle (16 b-lactams) MeCN with 0.1% FA 6 g MgSO4, 1.5 g NaOAc d-SPE (900 mg MgSO4, 300 mg PSA, UHPLC-Q-Orbitrap-MS 83e112 0.13e1.16 mg/ [153]
150 mg C18) kg
7
8
Dog food (Pentobarbital) MeCN 5 g NaCl d-SPE (2 mg MgSO4, 300 mg Bondesil, GC-MS/MS 75e136 2 ppb [154]
300 mg C18)
Drinking water (9 Parabens) MeCN with 1% FA 4 g MgSO4, 1 g NaCl d-SPE (150 mg MgSO4, 50 mg chitin) LC-MS/MS 70e115 0.04e4 mg/L [48]
Edible tissues (22 Sulfonamides) H2O:MeCN (1:2 v/v) 4 g MgSO4, 1 g NaCl, 1 g d-SPE (150 mg PSA, 900 mg MgSO4) LC-QqQ-MS e e [155]
with 1% HAc SCTD, 0.5 g SCDS
Edible tissues (Mebendazole and its MeCN 800 mg MgSO4, 500 mg d-SPE (50 mg Al-N, 50 mg C18) LC-MS/MS 80e114 <1 mg/kg [156]
metabolites, albendazole and its NaCl
metabolites)
Fish, meat, infant food (12 PAHs) MeCN 4 g MgSO4, 1 g NaCl, 1 g d-SPE (900 mg MgSO4, 150 mg PSA, GC-MS/MS 75e108 0.1e1 mg/kg [157]
SCTD, 0.5 g SCDS 150 mg C18)
Fish feed (Albendazole and 3 MeCN 2 g MgSO4, 0.5 g NaCl d-SPE (450 mg MgSO4, 25 mg PSA) LCeMS/MS 99e101 <145 ng/g [158]
metabolites)
Fish muscle (5 Tetracyclines) MeCN 1.25 g (NH4)2SO4 d-SPE (500 mg C18) UHPLC-MS/MS 80e105 1.7e4.4 mg/kg [159]
Fish tissue (137 veterinary drugs and MeCN:H2O (84:16 1 g MgSO4, 300 mg NaOAc d-SPE (22 mg PSA, 240 mg MgSO4, UHPLC-MS/MS 81e111 0.01e4.73 mg/ [102]
metabolites) v/v) with 0.1 M 43 mg Z-Sepþ) kg
EDTA, 1% HAC
Fish tissues (Eugenol) MeCN 2 g MgSO4 d-SPE (150 mg ODS, 900 mg MgSO4) GC-MS/MS 91e100 10 mg/kg [160]

Foodstuffs (23 b-lactams) MeCN 4 g Na2SO4, 1 g NaCl d-SPE (900 mg Na2SO4, 200 mg C18) LC-MS/MS 74e104 e [45]
Fruits, soil, vegetables (Triticonazole MeCN 6 g MgSO4, 1.5 g NaOAc d-SPE (50 mg PSA, 50 mg GCB, 150 mg LC-MS/MS 84e103 3.6e9.1 mg/kg [161]
enantiomers) MgSO4)
Fruits, vegetables (10 PFAAs) MeCN with 1.5% FA 4 g MgSO4, 1 g NaCl d-SPE (150 mg ENV SPE Bulk, 900 mg UHPLC-MS/MS 85e97 6e27 mg/g [162]
MgSO4)
Fruit juice (Forchlorfenuron) MeCN with 1% HAc 400 mg MgSO4, 100 mg d-SPE (50 mg PSA, 150 mg MgSO4) IMS 80e115 22e79 mg/L [163]
NaOAc
Grain Sorghum (14 Phthalate esters) MeCN 700 mg MgSO4, 320 mg d-SPE (150 mg MgSO4, 50 mg PSA, GC-MS 82e120 0.5e20 mg/kg [164]
NaCl 50 mg C18)
Honey (4 Antibiotics residues and their MeCN with 5% citric 4 g MgSO4, 2 g NaCl d-SPE (150 mg MgSO4, 50 mg PSA, LC-MS/MS 52e102 e [165]
metabolites) acid 50 mg C18)
Human milk (14 Parabens) MeCN 150 mg MgSO4, 150 mg d-SPE (25 mg MgSO4, 250 mg PSA, UHPLC-MS/MS 87e112 0.3e0.6 ng/mL [166]
NaCl 50 mg C18)
Infant milk-based products (5- MeCN 500 mg MgSO4, 100 mg d-SPE (150 mg MgSO4, 100 mg PSA) UHPLC-MS/MS 63e94 0.08e0.65 mg/L [167]
Nitroimidazole) NaCl
Maize, soil (Rimsulfuron, mesotrione, MeCN with 0.1% 2 g MgSO4, 1 g NaCl, d-SPE (200 mg MgSO4, 25 mg C18) LC-MS/MS 80e110 2.4e6 ng/g [168]
fluroxypyr-meptyl, fluroxypyr) HAc
Meat (13 Steroids and 1 metabolite) MeCN 800 mg MgSO4, 200 mg d-SPE (50 mg Al2O3/50 mg florisil) UHPLC-Orbitrap-MS 70e103 1.0 - 2 mg/kg [169]
NaCl
Milk (10 Non-steroidal anti- MeCN with 5% HAc 5 g Na2SO4, 1 g NH4CH3CO2 d-SPE (1000 mg MgSO4, 150 mg C18) LC-QqQ-MS/MS 78e97 0.4e42.3 mg/kg [60]
inflammatory drugs)
Milk (9 Bisphenols) MeCN with 1% FA 1 g MgSO4, 2 g NaCl d-SPE (250 mg MgSO4, 100 mg PSA, HPLC-FLR 76e94 3.5e9.8 mg/kg [170]
100 mg C18)
Raw milk (13 Steroid hormones) MeCN 4 g MgSO4, 1 g NaCl, 1 g d-SPE (900 mg MgSO4, 150 mg PSA, UHPLC-QTOF-MS 74e100 0.23e1.7 mg/kg [171]
SCTD, 0.5 g SCDS 200 mg Al2O3).
Roasted coffee, barley, potato crisps MeCN with 0.2% FA 10 g MgSO4, 1 g NaCl d-SPE (150 mg Al2O3) LC-MS/MS 80e84 0.5 mg/L [172]
(Acrylamide)
Salmon (34 Sulfonamides and their MeCN:H2O (84:16 1 g MgSO4, 100 mg NaOAc d-SPE (45 mg Z-Sepþ, 32 mg PSA, 0.25 g UHPLC-Orbitrap-MS e e [98]
metabolites) v/v) with 1% HAc Na2SO4)
Seafood (23 Antibiotics and MeCN:MeOH 6 g MgSO4, 1.5 g NaOAc d-SPE (150 mg PSA, 150 mg C18, 900 mg UHPLC-MS/MS 30e70 0.02e1.03 ng/g [53]
metabolites) (75:25 v/v) MgSO4)
Smoke meat (16 PAHs) H2O:MeCN (1:1 v/v) 3 g MgSO4, 0.5 g NaCl d-SPE (100 mg Z-Sep, 500 mg MgSO4) GC-MS 74e117 0.41e20.01 ng/ [173]
g
Soy sauce (7 Biogenic amines) MeCN 2x (2 g NaCl) d-SPE (100 mg PSA, 100 mg C18) UHPLC-MS/MS 84e115 15e30 mg/kg [174]
Tea (Bisphenol A, Tetrabromobisphenol MeCN with 0.7% 2 g MgSO4, 4 g NaCl d-SPE (10 mg MWCNTs, 200 mg SCX, LC-MS/MS 77e109 1e20 mg/kg [175]
A) HAc 100 mg C18)
Teas (Benz[a]anthracene, chrysene, EtAc 4 g Mg, 1 g NaCl, d-SPE (300 mg MgSO4, 100 mg PSA, HPLC-FLD 54e99 0.1e0.5 mg/kg [176]
benzo[b]fluoranthene, benzo[a] 300 mg Si gel)
pyrene]
Types of milk (13 Veterinary drugs) MeCN with 1% HAc 4 g MgSO4 d-SPE (50 mg chitosan, 150 mg MgSO4) LC-MS/MS 62e125 1e50 mg/kg [91]
Vegetables (16 PAHs) MeCN 4 g MgSO4, 1 g NaCl d-SPE (150 mg MgSO4, 25 mg PSA) GC-MS 76e106 0.04e0.1 ng/g [177]
Vegetables, rice (2-Nitrofluorene, 1- MeCN 4 g MgSO4, 1 g NaCl d-SPE (30 mg PSA, 150 mg MgSO4) HPLC-FLD 78e113 0.16e0.43 mg/ [178]
nitropyrene, benzo[a]pyrene) kg
Pharmaceutical and clinic analysis
Animal livers (Chlordecone, chlordecol) MeCN 4 g MgSO4, 1 g NaCl, 1 g d-SPE (50 mg PSA, 50 mg C18, 50 mg HPLC-MS/MS 70e120 1.36e2.50 mg/ [179]
SCTD, 0.5 g SCDS Envi-Carb, 150 mg MgSO4) kg
Body fluids, tissues (Zolpidem, MeCN Captiva ND Lipids d-SPE (25 mg C18EC, 150 mg MgSO4) LC-MS/MS 82e110 [180]
zolpidem phenyl-4-carboxylic acid) cartridges
Bovine muscle tissue (Avermectins, MeCN with 2% HAc 2 g NaCl, 4 g Na2SO4 d-SPE (250 mg C18, 250 mg MgSO4) UHPLC-MS/MS 85e119 0.011 [181]
benzimidazoles and nitroimidazoles e113.674 mg/kg
residues)
Fish tissues, feed, blood (7 PBDEs, 8 MeCN:Toluene (4:1 1 g MgSO4, 0.25 g NaCl d-SPE (200 mg EMR-lipid, 20 mg GC-MS/MS 70e120 <265 pg/g [182]
MeO-PBDEs) v/v) MgSO4, 30 mg Z-Sepþ)
Human hair (28 Pesticides) MeCN:H2O (1:1 v/v) 1 g MgSO4, 250 mg NaOAc d-SPE (500 mg Z-Sep) UHPLC-MS/MS, GC-MS 40e150 0.6e288.5 pg/ [183]
mg
Human plasma (31 Pesticides) EtAc with 2% HAc 400 mg MgSO4 d-SPE (50 mg PSA) GC-MS/MS 74e107 0.13e13.53 ng/ [184]
mL
Human blood plasma (5 Antiretroviral MeCN with 0.1% 2.16 g salts d-SPE (25 mg PSA, 25 mg C18, 150 mg HPLC-MS 60e83 29.0e112.5 ng/ [185]
drugs) HAc MgSO4) mL
Human urine (Fluoxetine, EtAc 200 mg SCTD, 100 mg SCDS, d-SPE (25 mg PSA, 25 mg C18, 150 mg UHPLC-PDA 86e109 0.10 mg/mL [186]

clomipramine and their active 200 mg NaCl, 800 mg MgSO4)
metabolites) MgSO4
Human urine (Bisphenol A) MeCN with 1% HAc 6 g MgSO4, 1.5 g NaOAc d-SPE (25 mg C18, 150 mg MgSO4) GC-MS 74e120 0.43 mg/L [16]
Human tissue (Zearalenone and its 4 EtAc 6 g MgSO4, 1.5 g NaOAc d-SPE (1200 mg MgSO4, 400 mg PSA, HPLC-FLD, UHPLC- QTOF 50e83 232 ng/g [187]
metabolites) 400 mg C18)
Muscle, viscera (7 b-agonists) MeCN with 1% EtAc 6 g MgSO4, 1.5 g NaOAc d-SPE (900 mg MgSO4, 150 mg PSA, LC-MS 70e12 1 ng/g [188]
150 mg C18EC)
Pig heart, liver, spleen and muscle (9 MeCN:H2O (1:1 v/v) 2 g MgSO4, 500 mg NaCl, d-SPE (50 mg C18, 100 mg MgSO4) LC-MS/MS 70e110 1e2 ng/g [189]
Zearalenone-like mycotoxins) with 0.1% FA
Pig kidney, liver and lungs MeCN 4 g MgSO4, 1 g NaCl, 1 g d-SPE (900 mg MgSO4, 150 mg PSA, LC-MS/MS 92e127 6.27e7.21 mg/ [190]
(Ractopamine and its metabolites) SCTD, 0.5 g SCDS 150 mg C18EC) kg
Porcine muscle (Naloxone, yohimbine, MeCN with 0.1% 4 g MgSO4, 1 g NaCl, 1 g d-SPE (150 mg C18, 900 mg MgSO4) LC-MS/MS 61e83 0.5e5 ng/g [191]
thiophanate, altrenogest) TFA SCTD, 0.5 g SCDS
Post-mortem blood, serum (15 MeCN 5 mg K2CO3, 150 mg MgSO4 d-SPE (150 mg MgSO4, 25 mg PSA) LC-MS/MS 85e113 1e50 ng/mL [94]
Psychotropic drugs)
Swine manure (26 Veterinary drugs) MeOH, MeCN, 4 g MgSO4, 1 g NaCl d-SPE (40 mg PSA, 20 mg C18) LC-MS/MS 61e106 0.05e5.91 mg/ [192]
0.1 M EDTA- kg
McIlvaine buffer
(12.5:37.5:50 v/v/v)
Sturgeon organs (Emerging organic MeCN 2 g MgSO4, 500 mg NaCl d-SPE (150 mg MgSO4, 50 mg PSA, GC-MS 60e107 e [193]
contaminants) 50 mg C18)
Urine, feces (Chlordecone, chlordecol) MeCN 4 g MgSO4, 1 g NaCl, 1 g d-SPE (150 mg MgSO4, 50 mg PSA, HPLC-MS/MS 70e120 0.1e2.4 mg/L, [194]
SCTD, 0.5 g SCDS 50 mg C18, 50 mg Envi-Carb) 3.2e5.8 mg/kg
Whole blood (Valproate) MeCN 400 mg MgSO4, 100 mg d-SPE (150 mg MgSO4, 50 mg C18) GC-MS/MS 71e104 10 ng/mL [195]
NaCl
9
Whole blood (D -tetrahydrocannabinol MeCN 80 mg NaCl, 150 mg MgSO4 d-SPE (12.5 mg C18) GC-MS/MS 94e102 0.03e0.43 ng/g [196]
and its 2 metabolites)
Environmental analysis
Sediments (18 Pesticides) MeCN with 0.1% 6 g MgSO4, 1.5 g NaOAc d-SPE (150 mg MgSO4, 50 mg PSA, UHPLC-MS/MS 71e106 0.8e13 ng/g [197]
HAc 50 mg C18)
Sediments (31 Pesticides) EtAc 4 g MgSO4, 1 g NaCl d-SPE (150 mg MgSO4, 25 mg florisil, GC-MS/MS 71e116 0.01e0.08 ng/ [198]
25 mg PSA) mL
Soil by radish (Chlortetracycline, MeCN with 1% HAc 1 g SCTD, 500 mg SCDS, d-SPE (30 mg PSA, 30 mg C18) LC-MS/MS 77e114 2e20 mg/kg [199]
enrofloxacin, sulphathiazole) 100 mg EDTA-Na2
Soil (26 Acid herbicides) MeCN with 1% HAc 4 g MgSO4, 1 g NaCl, 1 g d-SPE (200 mg Al2O3) LC-MS/MS 70e120 10 mg/kg [20]
SCTD, 0.5 g SCDS
Soil (6 Amine herbicides) MeCN:H2O (1:1 v/v) 4 g NaCl d-SPE (50 mg PSA, 10 mg GCB, 50 mg GC-MS 92e108 5e20 mg/kg [21]
C18, 100 mg MgSO4)
9
10
Soils (Imazethapyr, imazapic) MeCN 4 g MgSO4, 3 g NaCl d-SPE (250 mg MgSO4) LC-MS/MS 85e117 6.1e6.6 mg/kg [200]
Soils (16 PAHs) DCM 3 g Na2SO4 d-SPE (50 mg C18, 150 mg PSA, 900 mg GC-MS/MS e e [201]
Na2SO4)
Soil (10 Emerging organic MeCN with 0.1% 1.5 g NaOAc d-SPE (500 mg C18) LC-MS/MS 60e120 0.05e10 mg/kg [42]
contaminants) HAc
Soil, tomato (Cyazofamid) MeCN 4 g MgSO4, 1 g NaCl d-SPE (200 mg C18, 40 mg PSA, 500 mg LC-MS/MS 76e109 0.33e3.8 mg/kg [202]
MgSO4)
Soil (15 OCPs) HEX:acetone (9:1 v/ 1 g NaCl d-SPE (40 mg florisil, 150 mg MgSO4) APGC-QTOF-MS 70e119 0.86e9.99 mg/L [203]
v)
Soil, water, fruits (Indaziflam and its MeCN with 1% 3 g MgSO4, 2 g NaCl d-SPE (50 mg C18, 150 mg MgSO4) UHPLC-MS/MS 81e112 0.01e1.01 mg/ [204]
five metabolites) NH4OH kg
Multiclass analysis
Animal livers (53 Pesticides, 9 MeCN 500 mg NaOAc d-SPE (50 mg PSA, 50 mg C18, 150 mg LC-MS/MS 83e118 5e50 mg/kg [205]
mycotoxins) MgSO4)
Avocado, kale, pork, and salmon (65 MeCN 7.5 g NH4HCO2 d-SPE (180 mg Verde, 30 mg PSA, 30 mg GC-MS/MS 62e107 e [73]
Pesticides and 52 environmental C18, 90 mg MgSO4)
contaminants)

Carbohydrate-rich foods (Acrylamide, H2O:MeCN (1: 2 v/ 4 g MgSO4, 1 g NaCl d-SPE (900 mg MgSO4, 150 mg PSA, GC-MS 79e82 9 mg/kg [206]
free and bound 3-MCPD, glycidyl v) 300 mg C18)
esters)
Egg, milk (65 Antibiotics residues, 39 MeCN with 3.35% 4 g Na2SO4, 1.2 g NaCl, d-SPE (1500 mg Na2SO4, 140 mg PSA, LC-MS/MS 40e105 0.01 - 31 mg/kg [39]
mycotoxins and metabolites) FA 500 mg NaOAc 300 mg C18)
Honey (90 Pesticides, 16 PAHs, 22 PCBs) MeCN 4 g MgSO4, 1 g NaCl, 1 g d-SPE (1.2 g MgSO4, 400 mg PSA, LC-MS/MS, GC-MS/MS 22e99 0.16e55.87 ng/ [207]
Honey (16 PAHs, 22 PCBs) MeCN 4 g MgSO4, 1 g NaCl, 1 g d-SPE (1.2 g MgSO4, 400 mg PSA, GC-MS/MS 60e104 0.23e55.87 ng/ [208]
Human serum (6 NBFRs, 8 PBDEs) Acetone:HEX (1:1 4 g MgSO4, 1 g NaCl d-SPE (100 mg MgSO4, 200 mg C18) GC-MS 78e129 e [209]
v/v)
Lettuce, grapes, milk, chicken, pork, MeCN 400 mg MgSO4, 100 mg d-SPE (75 mg, MgSO4:PSA:C18:GCB GC-MS, LC-MS/MS 68e126 0.03e2.2 mg/L [210]
beef (17 Pesticides, 16 alkaloids, 18 NaCl 3:1:1:1 (w/w/w/w))
drugs)
Milk (9 Anabolic steroids, 16 b-agonists) MeCN with 5% HAc 1 g ZnO d-SPE (50 mg PSA) UHPLCeMS/MS 63e126 0.02e0.4 mg/kg [211]
Milk (26 Veterinary drugs, 187 MeCN with 0.1% 2 g MgSO4, 1 g NaOAc d-SPE (50 mg PSA, 200 mg MgSO4) LC-MS/MS 75e120 8e12 mg/kg [212]
pesticides) HAc
Seed, nuts (3 Tocopherols, 4 sitosterols) MeOH 4 g MgSO4, 1 g NaCl d-SPE (450 mg MgSO4, 75 mg PSA) HPLC-PDA 71e116 0.26e2.75 mg/L [213]
Whole blood (16 PAHs, 12 PCBs, 17 MeCN:H2O (3:1, v/ 1 g MgSO4, 200 mg NaCl, d-SPE (150 mg MgSO4, 50 mg PSA, GC-MS/MS 71e149 0.1e1.0 ng/mL [214]
OCPs, 7 PBDEs) v) 50 mg C18)
a
Target compounds are described until four analytes.
The optimization step included performance assays with MeCN acetate buffers) [71e73]. Ammonium ions promotes the formation
acidified with HAc or FA, and the best extraction efficiency for most of ammonium adducts rather than the less desirable sodium ad-
of the target analytes was achieved using MeCN containing 1% HAc ducts is enhanced [71]. In this sense, Nanita and Padivitage [74]
as an extraction solvent. On the other hand, Kaczyn ski et al. [10] evaluated the efficiency on partitioning and clean-up steps of
reported for the first time a one-step QuEChERS-based approach for different ammonium salts for pesticide residue analysis in food and
the extraction and clean-up of 23 sulfonylurea herbicides in cereals biological matrices. Similar results among certain ammonium salts
using acidified (1% FA) MeCN as extracting solvent. Desmarchelier were obtained, but they selected NH4Cl based on minor practical
et al. [56] used an acidic QuEChERS-like extraction (MeCN with 0.1% considerations. Moreover, Gonza lez-Curbelo et al. [61] evaluated
FA) to screen 105 antibiotic, anti-inflammatory, antiparasitic agents three new different versions of the QuEChERS method using NH4Cl,
and tranquilizers in raw materials of animal origin by LC-MS/MS. In NH4HCO2 and acetate buffers to induce phase separation and
studies involving biological fluids, Correia-Sa et al. [16] employed extraction of 43 representative pesticides from food matrices. The
acidified MeCN for the fast determination of bisphenol A in human performance of the three methods compared positively with the
urine. Ruiz-García et al. [12] to achieve the highest extraction effi- QuEChERS AOAC Official Method 2007.01, being NH4O2CH buffering
ciency of the health-promoting phytoalexin, trans-resveratrol, from the most promising for wide applicability to monitor gas chroma-
grapes, tested different solvent combinations such as MeOH:EtAc tography (GC-) and liquid chromatography (LC-) amenable pesti-
(50:50, v/v), MeOH:MeCN (50:50, 20:80 v/v) and MeCN:EtAc cides. Rúbies et al. [60] substituted NaCl by NH4CH3CO2 in the
(50:50, v/v). The optimum extraction/partitioning solvent combi- extraction of ten non-steroidal anti-inflammatory drugs in milk
nation for the target compound was MeCN:EtAc (50:50, v/v), since samples and obtained lower baseline noise, which enabled low
it provided a very selective and specific chromatographic response detection limits (LODs) and high recovery percentages (78e96%).
for trans-resveratrol. Additionally, Abdel-Ghany [54] extracted five Moreover, the same procedure was performed by Kachhawaha
neonicotinoids from soil samples using MeCN:DCM (1: 2 v/v). In et al. [40] for the multiresidue analysis of pharmaceuticals and
this case, the results showed that the method developed was personal care products (PPCPs) in sewage and surface water. It was
suitable for determining the residues, the rate of disappearance of observed that buffering with HAc plus NH4CH3CO2 resulted in good
the five neonicotinoids from soil, and the half-lives of the recoveries (73e125%) for all target analytes.
neonicotinoids. The temperature during the QuEChERS procedure may also
Regarding the promotion of phase separation and the salting- affect the extraction efficiency of thermally-labile analytes. Some
out effect, a wide range of different salts, such as MgSO4, sodium pesticides for example can be degraded upon the addition of
sulfate (Na2SO4), ammonium acetate (NH4CH3CO2), NaCl, NaOAc, anhydrous MgSO4 due to its exothermic hydration reaction. To
SCTD, SCDS, and combinations of these have been assayed reduce this problem, freezing the sample prior to extraction or
[12,39,57e60] to induce MeCN/water phase separation during the adding cold water (<4 C) have been proposed as alternatives. In
analytes extraction step [61]. Overall, the combination of MgSO4 the case of using frozen samples, the temperatures achieved after
and NaCl is the most widely used in QuEChERS extraction extraction have been shown to be moderate. Modification in the
[7,9,14,25,28,54,62e68], since MgSO4 allows best salting-out of purity of MgSO4 on the other hand has been shown to achieve a
MeCN and co-extracting some undesirable polar compounds from remarkable temperature difference with no significant differences
sample matrix like sugars, whereas NaCl controls the polarity of the in recoveries [75,76]. In this context, cold-induced aqueous MeCN
extraction solvents and thus increases selectivity of extraction [69]. phase separation (CIPS) represents the main change introduced in
Although Na2SO4 is quite popular in the applications involving the QuEChERS procedure. Shao et al. [77] replaced the initial
drugs and their metabolites [39,70]. In this context, it is important (salting-out) step of a representative QuEChERS procedure with
to refer the work of Zhou et al. [39], evaluated the extraction effi- CIPS, applying this modified procedure (“CIPS-QuEChERS”) to a
ciency of six groups of salt combinations (Na2SO4, NaCl, NaOAc, homogenate of salmon.
MgSO4, sodium citrate (C6H5Na3O7), SCDS) in order to define the Another important improvement on the QuEChERS approach
most favourable combination for the simultaneous extraction of involves the development and multi-laboratory validation of a
mycotoxins and veterinary drugs in egg and milk. The most single method, the so-called quick polar pesticides (QuPPE)
favourable extraction efficiency was obtained using combinations method, being proposed by the EU Reference Laboratories [24].
of either NaCl or NaAc with Na2SO4 (recoveries > 60%). Possibly, QuPPe method allows the extraction of highly polar analytes from a
interactions between the target veterinary drugs and Mg2þ (from wide range of sources with acidified MeOH followed by filtration.
MgSO4 used in the original protocol) occurred that may have hin- Then, the extracts are directly analysed by liquid chromatography-
dered the extraction procedure. Therefore, better results were ob- tandem mass spectrometry (LCeMS/MS) and a clean-up step (d-
tained using Mg2þ-free salt combinations. Desmarchelier et al. [56] SPE) is not required [78]. The QuPPE method makes use of different
adopted a similar strategy, using a partitioning salt mixture chromatographic separation mechanisms, including hydrophilic
composed of Na2SO4 and NaCl instead of MgSO4 for the determi- interaction chromatography, to identify highly polar pesticides in
nation of different antibiotic, anti-inflammatory, antiparasitic foods of plant origin [79].
agents and tranquilizers. The fact that MgSO4 is known to induce
the chelation of quinolones certainly contributed to Desmarchelier 2.1.1. Sorbents for clean-up QuEChERS extracts
et al. [56] opting to use other salts, namely Na2SO4 and NaCl. Concerning, the second step in the QuEChERS procedure (d-SPE
Moreover, MgSO4 as well as Na2SO4, are low vapour pressure salts step), different sorbents have been evaluated. The most popular
that tend to deposit as solids on surfaces in the MS source and sorbents reported in the literature, used in combination or sepa-
potentially within the analyser, thus leading to a loss in instrument rately, include primary secondary amine (PSA), octadecyl silica (C18)
performance. In GC, salts also pose problems as they tend to deposit and graphitized carbon black (GCB) [80]. PSA is typically used to
in the inlet liner, thereby leading to a greater frequency of liner remove fatty acids, sugars, organic acids, lipids and some pigments,
replacement [71]. Thus, in order to overcome these drawbacks and while C18 is particularly effective for the removal of high lipid
to improve the compatibility with MS detection, these salts have contents and GCB for co-extracted pigments, namely carotenoids
been replaced by salts with highest volatility, that can easily be and chlorophyll, typical from highly pigmented matrices (e.g. green
evaporated and/or decomposed in the ionization chamber (e.g. leaf vegetables), but should be used with caution since it might
ammonium chloride (NH4Cl), ammonium formate (NH4HCO2) and remove pesticides with planar structures [80]. So, there is a risk of
losing planar pesticides when GCB is part of the d-SPE sorbent wide range of unwanted analytes, Waters updated their Oasis
design. Furthermore, alternative sorbents are continuously being product to Oasis Prime and Supelco devised zirconia-based Z-Sep
proposed to improve and broaden even more the range of appli- and Z-Sepþ [73]. Hamed et al. [29] proposed an innovative
cations in which the QuEChERS approach can be used. Several approach based on the QuEChERS protocol using a zirconium-based
companies have commercialized novel sorbents and materials for sorbent (Supel™ QuE Z-Sepþ) as a new material for clean-up. This
extraction compounds from food, environmental and clinical sorbent, composed of C18 and zirconia bound to the same silica
samples. Over the past few years, Agilent, United Science and particles, was used in the original d-SPE step and was reported to
United Chemical, introduced Enhanced Matrix Removal-Lipid remove fats and pigments more efficiently than traditional PSA, C18
(EMR-lipid), CarbonX and ChloroFiltr, respectively to selectively and GCB sorbents [29]. In addition, a novel carbon/zirconia-based
remove major interfering compounds from sample matrix. In EMR- material, Supel™ QuE Verde, was evaluated in a filter-vial disper-
lipid, the sorbent will pull interfering lipids from samples while sive solid-phase extraction clean-up of pork, salmon, kale, and
leaving analytes behind, improving method reliability and avocado extracts, for the residual analysis of 65 pesticides and 52
ruggedness. The structure of EMR-lipid does not act as a solid environmental contaminants [73]. Overall good recoveries were
adsorbent in d-SPE and its mechanism involves a combination of attained (70e120%). Łozowicka et al. [88] tested the efficiency of
hydrophobic interactions and size exclusion between the long eight commercial sorbents (florisil, neutral alumina, GCB, PSA, C18,
aliphatic chain of lipids and the sorbent. The EMR-lipid d-SPE diatomaceous earth, Verde and ChloroFiltr) and one organic sor-
instead of the traditional d-SPE sorbents, requires additional water bent (chitosan) to estimate the fate of spirotetramat and dissipation
to activate the material, increasing the efficiency of lipid removal metabolites in the leaf-root and soil systems of Apiaceae and
from the matrix. The supernatant resulting from EMR-lipid is Brassicaceae grown under greenhouse conditions. The results
transferred to the EMR-lipid polish salts in order to separate the showed that florisil (200 mg) provided the most effective clean-up,
MeCN/water [81e83]. Although, the potential of EMR-lipid for removing the greatest amount of interfering substances and
lipids removal, this issue continues to be a concern. To overcome simultaneously ensuring analyte recoveries greater than 70% for
the drawbacks, Ultra Clean Technology (UCT) has developed a novel most compounds with a RSD lower than 20% [88]. In the same
sorbent, LipiFiltr®, for the clean-up of fatty samples. The easy-to- context Lo pez-Blanco et al. [89] evaluated the efficiency of different
use LipiFiltr® push-through purification cartridge was developed sorbents, such as C18þPSA, Z-Sepþ (zirconium oxide and C18 dual
to remove lipids from MeCN extracts. The samples are extracted bonded to silica), Z-Sep (zirconium oxide bonded to silica) and the
using a standard QuEChERS procedure and an aliquot of the su- novel EMR-lipid sorbent, for the clean-up step of pesticide analysis
pernatant is pushed through the LipiFiltr® purification cartridge in olive oil, olives and avocado. The best extraction efficiency in
using a disposable syringe. The purified extract is collected into an olive oil were obtained using the EMR-lipid sorbent, while for olives
autosampler vial and analysed by a high resolution chromato- and avocado the results were quite similar amongst the different
graphic technique. The capacity to obtain cleaner extracts, ease of sorbents used. Soares et al. [90] reported a good analytical perfor-
use, time and cost investments, make the new LipiFiltr® push- mance in the use of chitin as a d-SPE sorbent in the extraction of
through cartridges a potential clean-up option for laboratories organic contaminants in drinking water from treatment sludge,
conducting pesticide residue analysis in complex fatty samples whereas Cabrera et al. [80] evaluated the efficiency of alumina,
[84]. Moreover, the d-SPE step can also be combined with a freeze- florisil®, chitosan and diatomaceous earth as clean-up sorbents for
out step, which consists of precipitation of lipid at low temperature. pesticide residues in rice upon a QuEChERS extraction using acetate
Norli et al. [85] designed the combination of disposable syringes buffer. The obtained results showed that chitosan can be an eco-
with freezing polystyrene block. The freezing block keeps the nomic alternative to the C18 sorbent, maintaining the efficiency of
temperature in the extract at 20.5 C. the clean-up procedure in the extraction of pesticide residues [80]
The ChloroFiltr® sorbent was used for selective removal of and veterinary drugs [91] in milk. Overall, such improvements can
chlorophyll from organic extracts without loss of pesticides with be verified in the different application fields described in Fig. 1 and
planar structures. It is used instead of GCB in UCT dispersive Table 1.
extraction centrifuge tubes. ChloroFiltr® has been experienced
against hundreds of pesticides and herbicides, and the results ob- 2.1.2. QuEChERS miniaturization
tained shown a reduction of chlorophyll higher than 82%, without Since the first work developed in QuEChERS, different ap-
loss of target analytes. However, ChloroFiltr® should not be used for proaches for the miniaturization of the method have been proposed
mycotoxin and hexachlorobenzene analysis [69]. CarbonX sorbent [16,92e96]. In 2018, Dong et al. [92] developed a modified
works similarly to GCB without the large losses of planar pesticides QuEChERS method involving ultrahigh performance liquid
that occurs with GCB. In addition, the CarbonX removes more chromatography-tandem mass spectrometry (UHPLC-MS/MS) for
efficiently potential contaminants than GCB leading to decreased the simultaneous analysis of perchlorate (ClO 4 ) and bromate
fouling of the column and liner [86]. (BrO 3 ) in fruits and vegetables. Using a small amount of sample
Cleanert® NANO sorbent was designed based on functionalized (100 g), as well as 140 mg of C18 in combination with 40 mg of GCB
carbon nanotubes, and showed better efficiency to remove chlo- as the extraction salt, the authors obtained lower LODs, high re-
rophyll, pigments and fatty acids. In addition, the surface deacti- coveries (82e100%), and good sensitivity and selectivity. In turn,
vation process could control the over adsorption within limited Muhammad et al. [93] proposed a m-QuEChERS method for the
area, and ensure the recovery of aromatic pesticide. Cleanert® determination of the non-fluorescent antibiotic, chloramphenicol,
NANO could be broadly used in the multiresidue pesticide analysis in human urine and serum. To achieve this, 300 mL of sample,
in fruit, vegetable and other agro-food products. Small amount of 900 mL of MeCN, 60 mg tin (IV) oxide (SnO2), 140 mg MgSO4, and
the nanomaterial (10e15 mg) is enough for most of the samples, 70 mg NaCl were used and allowed for good selectivity, linearity,
making it could be packed as a filter format cartridge. Fast analysis LODs and recoveries (78e100%). Casado et al. [97] also proposed an
and small amount of sample are the most important advantages improved m-QuEChERS protocol for the determination of 12
using this approach [87]. phenolic compounds in baby foods. In this procedure, 300 mg of
Phenomenex commercialises Phree for removal of proteins and sample, 200 mg of the QuEChERS mixture (keeping the proportion
phospholipids from plasma samples, Millipore Sigma supplies 4:1:1:0.5 of MgSO4:NaCl:SCTD:SCDS) and 700 mL of MeCN were
molecularly imprinted polymer (MIP) for selective extraction of a used enabling excellent recovery rates (71e100%). On the other
hand, Pouliopoulos et al. [94] proposed a modified single step analytical protocols and methodologies have been used in the
QuEChERS method based on the addition of 600 mL of MeCN, 5 mg analysis of food composition. In this regard, the QuEChERS method
of potassium carbonate (K2CO3) and 150 mg MgSO4 in 100 mL of has become very popular as an extraction procedure for a wide
post-mortem blood and serum to identify 15 psychotropic drugs. range of analytes from food matrices. This has been made possible
The results obtained showed that the K2CO3 salt provided higher due to the significant modifications to the original QuEChERS
peak areas of analytes suggesting higher extraction recovery under procedure, particularly in terms of the use of buffers, described
basic conditions. A screening method for the simultaneous analysis above. As can be seen in Table 1, MeCN is the most often used
of 379 pesticides in human serum was developed by Shin et al. [95]. solvent in the partitioning step [13,28,97], in some reports acidified
The sample preparation was based on scaled-down QuEChERS, or alkalinized. Moreover, mixtures of MeCN with other solvents
where serum (100 mL) was extracted with MeCN (400 mL) and have been also used, namely MeCN:H2O [104] and MeCN:EtAc [12].
partitioned with MgSO4 (40 mg) and NaCl (10 mg), while the upper The partitioning salts are used according to the chemical nature
layer was used for analysis without further clean-up steps. Jesús of the analytes, solvents and to the version of the QuEChERS pro-
et al. [96] also used a miniaturized QuEChERS for the determination cedure selected. Kim et al. [104] used only NaCl in the partitioning
of a range of pesticides in odonate nymphs, while Correia-Sa et al. step to determine arbutin in pear peels. Similarly, some authors
[16] proposed a modified m-QuEChERS/GC-MS method to deter- chose not to add salt in the first step of QuEChERS, however the
mine bisphenol A in human urine samples. The optimized method clean-up step was regularly performed using d-SPE with C18, PSA
presented good linearity, accuracy (74% recovery), reproducibility and MgSO4 [105]. Fontana and Bottini added calcium chloride
(RSD < 11%) and sensitivity for bisphenol A determination (CaCl2) in clean-up step for the analysis of pyrazines [14] and ethyl
(LOD ¼ 0.13 mg/L). In comparison to the original extraction method, phenols [6] in wines. In turn, Dusek et al. [28] and Waterstraat et al.
these miniaturization protocols have the advantage of producing [65] used only MgSO4 in the d-SPE step for the isolation of eight
minimal waste amounts, since they involve considerably less phenolic compounds in hops and fifteen phenolic compounds in
sample, partitioning salts, solvents and sorbent amounts, and are milk samples, respectively. In order to minimize the analysis time
thus more environmentally friendly. and avoid extra sample manipulation, some authors [13,104]
At a different level, other modifications of the QuEChERS pro- skipping the clean-up step prior to instrumental determination of
tocol have been reported involving the reduction of analysis time, the extracted analytes (Table 1).
and the eventual introducing of some automation [98,99]. In this ACFs e based activated carbon fibres, Al-N e aluminium-N,
regard, in their work involving the analysis of organochlorine Al2O3 e aluminium oxide, C18 e octadecyl silica, CaCl2 e calcium
pesticides (OCPs) in fish tissues, Stremel et al. [99] proposed the chloride, CCl4 e carbon tetrachloride, C6H5Na3O7 e sodium citrate,
utilization of ultrasounds (US) as a strategy to reduce sample COPs e Cholesterol-oxidation products, DCM e dichloromethane,
amount and analysis time, since it provides a more efficient contact DLLME e dispersive liquid-liquid microextraction, d-SPE e
between the sample and the solvent. On the other hand, consid- dispersive solid-phase extraction, d-mSPE e dispersive microsolid-
ering the fact that laboratories nowadays are encountering a huge phase extraction, EDTA e ethylenediaminetetraacetic acid, EDTA-
numbers of samples and that the QuEChERS method is still a Na2 e ethylene diamine tetraacetic acid disodium, EMR-lipid e
labour-intensive procedure involving shaking and sample manip- enhanced matrix removal-lipid, EtAc e ethyl acetate, FA e formic
ulation steps, automation appears as a future perspective. In this acid, Fe3O4-PSA e iron oxide - primary secondary amine, FM-6-1 e
sense, some companies are working with DPX Labs and other N0 -[4-chloro-2-(trifluoromethyl)phenyl]-2-
companies to automate the QuEChERS method [100]. The typically propoxyethanimidamide, FS e fluorinated sorbent, GCB e graphi-
used d-SPE can be changed by the application of disposable pipette tized carbon black, GC-ECD e gas chromatography electron capture
extraction (DPX), which is a fully automated d-SPE method. Mas- detector, GC-mECD e gas chromatography micro-electron capture
trianni et al. [101] reported the use of automated DPX tips to extract detector, GC-MS e gas chromatography mass spectrometry, GC-
ten b-adrenergic agonists in pork meat, in an extraction time less MS/MS e gas chromatography tandem mass spectrometer, H2O e
than 20 min. A full automation of the QuEChERS method based on water, HAc e acetic acid, HMF e hydroxymethylfurfural, HPLC-PDA
the DPX tips clean-up step combined with the Gerstel MPS XL was e high performance liquid chromatography tandem photodiode
used by Jian et al. [98,102] for the untargeted screening of sulfon- array detector, HPLC-UV e high-performance liquid chromatog-
amides and other metabolites in salmon, as well as in veterinary raphy with ultraviolet detection, K2CO3 e potassium carbonate, LC-
drug residues in Tilapia muscle tissue using UHPLC-MS/MS. By this HRMS e liquid chromatography-high resolution mass spectrom-
approach the authors obtained lower LODs and LOQs, high recovery etry, LC-MS/MS e liquid chromatography tandem mass spectrom-
rates (>80%) and good reproducibility (RSD < 11%). The perfor- eter, LDS-DLLME e low-density solvent dispersive liquideliquid
mance of the analytical methodology are within the requests of the microextraction, LOQ e limit of quantification, MeCN e acetonitrile,
guidelines specified in European Commission Decision 2002/657/ Meo-PBDEs e methoxylated polybrominated diphenyl ethers,
EC. The results showed that this automated strategy may constitute MeOH e methanol, MgSO4 e magnesium sulfate, MCPD e 3-
a promising analytical tool for screening studies, since the extrac- monochloropropane-1,2-diol, MWCNTs e multi-walled carbon
tion parameters can be optimized according to the target analytes nanotubes, NaOAc e sodium acetate, NAC e nitrogen-enriched
[98]. activated carbon, NaCl e sodium chloride, NaHCO3 e sodium bi-
carbonate, NaOH e sodium hydroxide, Na2SO4 e sodium sulfate,
3. QuEChERS applications NBFRs e novel brominated flame retardants, NH4CH3CO2 e
ammonium acetate, OCPs e organochlorine pesticides, OPPs e
3.1. Food analysis organophosphorus pesticides, PAEs e phthalates, PAHs e polycyclic
aromatic hydrocarbons, PBDEs e polybrominated diphenyl ethers,
Besides food composition evaluation has been carried out for PCBs e polychlorinated biphenyls, PFAAs e perfluorinated alkyl
many decades. Currently, since food analysis is far more relevant acids, PPCPs e pharmaceutical and personal care products, PSA e
because consumers are more informed, and requires better and primary secondary amine, QuEChERS e Quick, Easy, Cheap, Effec-
more functional foods, the needed for higher traceability to guar- tive, Rugged and Safe, Rec (%) e recovery, Ref e references,SAX e
antee the origin, quality and safety of food products used by the strong anion exchange, SCDS e sodium citrate dibasic sesquihy-
human population has increased [103]. A huge number of different drate, C6H6Na2O7∙1.5H2O, SCTD e sodium citrate tribasic dihydrate,
C6H5Na3O7$2H2O, SCX e strong cation exchange, Si e silica, SnO2 e residues from different vegetables. The same combination was used
tin(IV) oxide, SMCs e Synthetic musk compounds, TFA e tri- by Xie et al. [129] to remove interferents from tomato extracts for
fluoroacetic acid, tri-BuA-rGO e tributylamine-functional reduced quantification of metribuzin and its metabolites, with satisfactory
graphene oxide, UHPLC-MS/MS e ultrahigh performance liquid recoveries (ranging from 72 to 96% with a RSD lower than 9%).
chromatography tandem mass spectrometer, ZnO e zinc oxide, Z- Cabrera et al. [80] selected chitosan (with MgSO4) as d-SPE sorbent
Sep e zirconium dioxide based sorbents. for the extract clean-up in the determination of pesticides and
metabolites from rice. The comparison of the performance of chi-
3.2. Food safety tosan with other sorbents, namely PSA, C18, GCB, florisil®, alumina
(Al2O3) and diatomaceous earth, was performed. Although the C18
3.2.1. Pesticides sorbent showed the best results, chitosan presented similar results
Pesticides are usually used to increase yields by protecting or and was shown to have the best performance among the uncon-
controlling crops from weeds, diseases, and pests [122]. However, ventional sorbents evaluated. In turn, Martins et al. [130] demon-
its use in agriculture and crops has become an important issue in strated the higher efficiency of a fluorinated sorbent (FS) in
recent years because they often occur in foods as residues, causing a comparison with the PSA, C18 and GCB for the clean-up of tomato
variety of adverse health effects, including neurological disorders, and sweet pepper extracts. The results showed that FS are an
nervous system, mimicking hormones causing reproductive prob- effective alternative with lower costs and greater efficiency. Liu
lems and its potential carcinogenicity, in addition to environmental et al. [122] proposed sorbent-based magnetite nanoparticles
contamination concerns arising from its use [122,215]. The control (MNPs) modified with PSA (Fe3O4-PSA). Significant improvements,
is based on food tolerances defined as the maximum residue limits in the removal of interferents for the simultaneous determination
(MRLs), established by the European Union (EU), Codex Ali- of pesticides in rice, wheat and soybean, were reported relative to
mentarius (CA) and other organizations Regulatory organizations the conventional d-SPE approach. Fernandes et al. [124] proposed a
such as Environmental Protection Agency (EPA, USA), European magnetic dispersive micro solid-phase extraction-based MNPs for
Food Safety Authority (EFSA, European Union), among others [126]. the purification of strawberries extracts regarding organophos-
Several analytical methods, including solid-phase extraction (SPE) phorus pesticides (OPPs) quantification. The use of MNPs showed a
[216], solid-phase microextraction (SPME) [216], and dispersive better performance regarding sugars, organic acid and pigments
liquid-liquid microextraction (DLLME) [217] combined with high removal from extracts, in addition to less solvent and sorbent
resolution chromatographic techniques, have been developed to amount as well less time-consuming. The high sorbent capacity of
accurately determine and monitor the residual levels of pesticides. MNPs used in clean-up step, allows the minimization of the GC
Most of these methods present some drawbacks and limitations inlet/column contamination and chromatographic interferences
that include complicated and time-consuming procedures, high [124]. synthetized by Also, Ma et al. [126] synthetized a new sor-
costs and require large amounts of toxic organic solvents [22]. The bent, tributylamine-functional reduced graphene oxide (tri-BuA-
versatility, effectiveness and simplicity of the QuEChERS prepara- rGO), for pesticides residue analysis in green tea. A cleaner extract,
tion technique [2] makes it the preferred tool for MRLs monitoring. than PSA, C18 and GCB sorbents, was obtained. Qin et al. [215] re-
QuEChERS allows for the selective extraction of multiresidue pes- ported an automated multi-filtration clean-up (auto m-FC)
ticides with a significant reduction of sample interferents and approach for the QuEChERS extraction of pesticides from apples,
achieve high extraction efficiencies of pesticides from different oranges, peanuts, wheat, spinach and green tea. The authors used a
chemical groups. The chemical structures of some pesticides nitrogen-enriched activated carbon (NAC) material with PSA and
commonly extracted by the QuEChERS are presented in Fig. S2. MgSO4 as a high-throughput approach to significantly reduce the
The original QuEChERS method [2], the AOAC Official Method manual operation workload in the clean-up step while obtaining an
[218] and the CEN Standard Method [219], are the most used pro- excellent clean-up efficiency. Recently, zirconia-coated silica (Z-
cedures in multiresidue pesticide analysis. In the recent years, Sep) particles were proposed for the development of new d-SPE
several modifications have been introduced into these procedures, sorbents. Rejczak et al. [9] used Z-Sep and Z-Sep Plus zirconium
mainly in the partitioning salts and in the d-SPE sorbents (Table 1). dioxide-based sorbents and PSA in the d-SPE clean-up of milk ex-
In different works involving pesticides extraction from food sam- tracts for pesticides analysis, while Guo et al. [64] used poly-
ples, NaCl was the only salt used in the partitioning step vinylpolypyrrolidone (PVPP) combined with PSA and GCB in the d-
[38,54,59,110,111,121,126,129,215] with recoveries (70e120%). More SPE clean-up of polyphenol-rich agricultural products for purifi-
extensive modifications were introduced by Bordin et al. [220] for cation of the extract for the determination of multiple pesticide
the quantification of pesticides in whole wheat flour. In this case, residues. The results obtained showed that PVPP as a sorbent in
the authors reported an acetate/citrate simplified QuEChERS pro- combination with a dilution method is as a promising QuEChERS
cedure without a clean-up step and using MgSO4, NaOAc and SCDS method for multiple pesticide residues analysis in complex
as the partition salts. Another interesting QuEChERS-based matrices [64]. For the first time, phenolic resin based activated
approach was proposed by Kaczyn ski and Łozowicka [10] to carbon fibres (ACFs) were applied as a reversed-dispersive solid-
extract and clean-up sulfonylurea herbicides in cereals (e.g. barley, phase extraction (r-DSPE) sorbent in the clean-up step by Singh
oats, rye, triticale and wheat), in a single step, using natural chitin et al. [221]. The results obtained demonstrated that ACFs were
to remove unwanted interferents, avoiding the d-SPE step. more efficient, cheaper, and more robust in the determination of
Although simplified QuEChERS procedures without a clean-up step pesticides in food commodities (e.g. vegetables, grains, fruits), and
have been proposed, the complexity of the samples will dictate its that they could be used as a cost-effective alternative to the PSA
use. A wide variety of new sorbents, alternative to the most tradi- sorbent. Trevisan et al. [112] proposed a QuEChERS variation for the
tional PSA and C18 sorbents, have been proposed. Among these, GCB extraction of pesticides from coffee leaf extracts. In Trevisan's study
has been widely reported in different multiresidue assays conventional d-SPE using PSA, C18 and MgSO4 was followed by a
[7,25,32,46,64,116,118,129,131,133]. Shabeer et al. [7] reported the second SPE step involving Supel QuE Z-Sep and a final DLLME with
use of PSA, C18 and GCB as clean-up sorbents to remove interferents carbon tetrachloride (CCl4) and MeCN. Similarly, Li et al. [127] also
arising from the simultaneous isolation of pesticide residues from applied a two-step clean-up procedure involving d-SPE using
cardamom. In turn, Zoccali et al. [131] and Konatu et al. [32] used multiwalled carbon nanotubes (MWCNTs) and PSA followed by
GCB, PSA and MgSO4 for the extract purification of pesticide DLLME (CCl4 and H2O) to remove interferents from tea extracts for
pesticide residue analysis. A more sophisticated clean-up proced- fruits from China.
ure based on d-SPE with the PSA sorbent followed by a DLLME Nevertheless, the major modifications in the QuEChERS pro-
based on the solidification of a floating organic droplet (DLLME- cedures used in mycotoxins extraction occurs in the clean-up step.
SFO) was introduced by Wang et al. [114] to remove interfering The most popular approach continues to be d-SPE, although in
substances from extracts of fish samples for the organochlorine some works, this step has not been used [37,47,135,223,227,229].
pesticides analysis. The proposed method showed high recovery Interestingly, d-SPE is usually performed with the C18 sorbent and
rates (88e121%) with RSD lower than 15%, and lower LODs and MgSO4 without use of PSA, since some classes of mycotoxins have a
LOQs. Finally, it is worthwhile to refer to the innovative QuEChERS high affinity to PSA leading to loss of target analytes. Alternative d-
approach proposed by Hong et al. [222] in which a membrane SPE sorbents for mycotoxins extraction were reported by Qian et al.
filtration (polytetrafluoethylene, 0.1 mm pore size) was used [135] and Zhao et al. [144]. The first authors used magnetic sorbents
instead of d-SPE to clean-up spinach extracts for the analysis of based on ferrocene (Fe(C5H5)2) and zirconium chloride (ZrCl4) to
pesticides. Overall, the described and reported applications extract mycotoxins from feed. Several magnetic materials including
demonstrated the great versatility and the wide range of applica- MDN@Fe3O4, PSA@Fe3O4, and ZrO2@Fe3O4 were tested as adsor-
bility of the QuEChERS approach in the multiresidue analysis of bent materials, with MDN@Fe3O4 being the most efficient adsor-
pesticides. New modifications and improvements are expected to bent for the purpose. In turn, Zhao et al. [144] used a carbon-based
continuously be developed in the next years. SPE sorbent with C18 and MgSO4 in the clean-up step for the
determination of Fusarium mycotoxins in pepper, potato, tomato
3.2.2. Mycotoxins and cucumber. Huang et al. [139] used a combination of adsorbents
Mycotoxins, secondary toxic metabolites produced through the - PSA, silica gel (Si), C18 and MgSO4, in the clean-up step for the
contamination of food products by some Fungi genera (e.g. Asper- simultaneous determination of mycotoxins in liquorice. The classic
gillus, Penicillium and Fusarium), may occur during the growing, SPE version for the clean-up step has also been reported in some
harvesting, storage, transport and processing of food and/or food- studies involving the analysis of target mycotoxins. This is the case
related products. Its toxicity depends on several factors, namely of the analysis of ochratoxin A in red wine performed by Marin ~ o-
the chemical nature of the mycotoxin, the fungi species, the time of Repizo et al. [141] using the Isolute® Myco cartridge. On the other
colonization, food proprieties, and climatological conditions hand, Arroyo-Manzanares et al. [228] used a simple salting-out
[139,223]. Mycotoxins are associated with several liver and kidney liquid-liquid extraction (SO-LLE) to obtain a most efficient extrac-
diseases, as well as hematopoietic, immune, fetal and reproductive tion of the aforementioned mycotoxin classes from wheat and
system problems. In addition, some mycotoxins exert potential maize in a short time.
carcinogenic and mutagenic effects on humans and animals. This
led the EU, through the European Commission's Scientific Com- 3.2.3. Other food contaminants
mittee for Food (ESCF) under the council of the EFSA, to establish There is a growing concern about food safety, largely due to the
the mycotoxins maximum levels (MMLs) for some mycotoxins in cases of food contamination and adulteration that are becoming
foods and food-related products [224,225]. Usually, the analytical more frequent and that are contributing considerably to health
methods used for MMLs determination involve two main steps. An problems. Thus, the development of analytical methods that allow
initial step corresponding to sample preparation where the myco- for the determination of potential contaminants in foods and food-
toxins are extracted from samples, followed by a screening analysis related products assumes particular importance in the current
to identify the extracted analytes. The determination of the MMLs context. Although a wide range of analytical methods for food
can be carried out through chromatographic (LC and GC), electro- safety monitoring exist, in recent years the QuEChERS procedure
phoretic (CE), spectrometric (MS), spectroscopic (UV) or immuno- combined with chromatographic and spectrometric techniques has
logical (ELISA) methods. As mycotoxins are typically present in been used as a reliable and simple alternative to analyse different
complex food matrices at low levels, its extraction is challenging. types food contaminants including natural or synthetic additives,
Methods such as LLE and SPE are commonly used for its extraction, packaging migration and process-induced contaminants. The most
however the QuEChERS method has now become a preparative recent QuEChERS applications to food contaminants are described
technique with wide application range in the analysis of these in Table 1. Again, the most QuEChERS procedures were based on the
metabolites [225]. Its easy and fast procedure to simultaneously original citrate- and acetate-buffered versions with slight varia-
isolate multiple mycotoxins belonging to a wide range of classes, tions. MeCN (or acidified MeCN) is usually the preferred parti-
including aflatoxins, fumonisins, ochratoxins, enniatins, beauver- tioning solvent, although 1-propanol [230], EtAc [176], mixtures of
icins, trichothecenes, estrogenic toxins, and xanthones, constitute MeCN with HEX [55], MeOH [53] and H2O [53,98], as well as
important outcomes for its acceptability and wide application. in acetone with HEX [147], have also been used. Adam et al. [230]
different food matrices, including cereals [134], feed [135], food- proposed a modified QuEChERS method using 2-propanol as
stuffs [223], fruits [142,226], pasta [227], wines [141], dried fruits extraction solvent and without the clean-up step for analysis of
[50], vegetables [144], and wheat and maize [52,228]. The chemical synthetic food dyes in jellies and smarties, whereas Toufi et al. [176]
structures of some common mycotoxins extracted by QuEChERS are used EtAc as extraction solvent to extract polycyclic aromatic hy-
illustrated in Fig. S3. drocarbons (PAHs) from tea. The combination of acetone with HEX
The QuEChERS procedures for mycotoxins extraction derived (1:1 v/v) as extraction solvent was proposed by Babalola et al. [147]
from the three previously described versions (e.g. original, citrate to analyse antibiotics in seafood. For the analysis of quaternary
and acetate) with some modifications, as shown in Table 1. Im- ammonium compounds (QACs) in milk, and ClO
4 and BrO3 in fruits
provements have been introduced mainly in the d-SPE step, and vegetables, respectively, Xian et al. [231] and Dong et al. [92]
although few modifications in the liquid-liquid partitioning step did not incorporate any salt in the partitioning step. In turn, Dong
was also performed. MeCN (or MeCN acidified with FA et al. [174] performed the partitioning steps twice, using only NaCl,
[47,139,143e145,228] and HAc [137,142,223]) remains the most in the determination of biogenic amines in soy sauce. For the
commonly used solvent, mixtures with other solvents, namely analysis of non-steroidal anti-inflammatory drugs in milk, Rúbies
MeOH [37], H2O [135,140], and different acids (e.g. citric acid) [50], et al. [60] developed a highly modified QuEChERS procedure, where
have also been employed. Wang et al. [50] used MeCN with citric NH4CH3CO2, 0.02 M ascorbic acid in 0.24 M HCl and Na2SO4 were
acid in the QuEChERS extraction of mycotoxins from nuts and dried used in the partitioning step. On the other hand, Adam et al. [230]
used MgSO4, NaCl and HCl in the partitioning step regarding the well-known that pharmaceuticals, after administration, are absor-
analysis of synthetic food additives in jellies and smarties. In some bed and undergo metabolic reactions to produce metabolites that
works, the clean-up step was not performed, whereas alternative can be even more harmful than the original compounds, or can
sorbents were used in other applications. Surma et al. [55] used the even be transformed back to the original active drugs. In this sense,
strong ion exchange (SAX) and PSA sorbent in the determination of Licata et al. [233] proposed a QuEChERS method that skipped the
acrylamide levels in coffee and coffee substitutes. Marta-Sanchez partitioning step and only used MgSO4 in the clean-up to extract
et al. [48] used chitin combined with MgSO4 in the clean-up pro- psychoactive drugs (e.g. triptans, benzodiazepines and metabolites,
cedure to evaluate the occurrence of parabens (including isomers) analgesics, antiepileptics, antidepressants, non-benzodiazepine
in mineral and drinking waters, whereas Arias et al. [91] used hypnotics, antipsychotics and its metabolites) from human hair
chitosan from shrimp shell waste combined with MgSO4 for the by the LC-MS/MS method. The procedure was applied to 234 real
determination of multiresidues from veterinary drugs in different hair samples obtained from patients with headache and was used
types of milk. On the other hand, Xu et al. [156] evaluated the ef- as a tool to monitor the intake of these drugs. Additionally, Pou-
ficiency of different sorbents, such as C18, PSA, NH2 and alumina-N liopoulos et al. [94] used a modified single step mini-QuEChERS
(Al-N) for the extract purification with respect to quantification of protocol (with addition of MeCN, K2CO3 and MgSO4 in 100 mL of
mebendazole, albendazole levamisole and its metabolites in edible sample) to extract prescribed antipsychotic drugs from post-
tissues of aquatic animals. The best efficiency was achieved using a mortem blood and serum samples. This method proved to be
combination of C18 and Al-N. Gao et al. [175] used C18, MWCNTs and suitable for the analysis of clinical samples for therapeutic drug
strong cation exchange (SCX) as the adsorbent mixture to eliminate monitoring, as well as ante-mortem or post-mortem whole blood
tea co-extracts, whereas Xin-Tong et al. [171] used a combination of analysis in forensic. Alves et al. [186] developed a modified
MgSO4, PSA and Al2O3 sorbent in the clean-up step to determine QuEChERS method, combined with UHPLC-PDA, as a new and
steroid hormones in raw milk. Finally, Petrarca [149] proposed a powerful strategy for the simultaneous and efficient isolation of
method to determine PAHs in baby food using QuEChERS combined two different antidepressants (fluoxetine and clomipramine) and
with low-density solvent dispersive liquideliquid microextraction their active metabolites in human urine samples. Wurita et al. [19]
(LDS-DLLME) using toluene as extracting solvent and a combina- applied a modified QuEChERS-based approach to verify the fatal
tion of PSA, C18 and MgSO4 for extract clean-up. Other ambitious poisonings of an abuser by multiple new psychoactive substances,
applications are reported involving the extensive multiresidue including AB-CHMINACA, 5-fluoro-AMB and diphenidine. AB-
analysis of veterinary drugs in food matrices using QuEChERS as CHMINACA metabolites were extracted from the urine of the
extraction technique [70,91,98,148,156,232]. In this context, Konak abuser by a modified QuEChERS method and analysed by LC-MS/
et al. [148] develop a highly sensitive and reliable multiresidue MS before and after hydrolysis with b-glucuronidase to achieve
method to determine sulfonamides and acetylated metabolites in an accurate quantification of the metabolites. In addition, Santos
baby foods by using UHPLC-Orbitrap-MS, using the original et al. [234] developed a modified QuEChERS method followed by
QuEChERS method combined with ASE to achieve the best recovery capillary electrophoresis-tandem mass spectrometry (CE-MS/MS)
ntara-Dura
for all analytes. Alca n et al. [70] carried out a sensitive to determine amphetamine and its derivatives in natural weight
multiresidue analysis based on nanoflow liquid chromatography loss pills and dietary supplements. In this modified QuEChERS
high-resolution mass spectrometry (LC-HRMS) to quantify veteri- method MeCN, alkanized with sodium hydroxide (NaOH), was used
nary drugs residues in honey, veal muscle, egg and milk using a as solvent for extraction and the d-SPE clean-up step was not
modified QuEChERS procedure. Additionally, a recent study pub- considered. Guo et al. [192] proposed a modified QuEChERS
lished by Arias et al. [91] used chitosan from shrimp shell waste method followed by LC-MS/MS to determine the veterinary drug
(renewable and non-toxic biopolymer) as a sorbent for the clean- content namely tetracyclines, sulfonamides, macrolides, fluo-
up step in QuEChERS towards the determination of veterinary roquinolones, lincosamides and pleuromutilins, in swine manure.
drug residues in milk samples. In this protocol, NaCl was eliminated This QuEChERS method involved a sample extraction with a
and the reagent consumption was reduced, making this protocol an MeOH:MeCN:0.1 M EDTA-McIlvaine buffer, followed by phase
innovative and environmental-friendly approach. separation with MgSO4:NaCl, and a clean-up step with PSA and C18.
As previously indicated, the presence of antibiotics in food Hasegawa et al. [180] proposed a modified QuEChERS method to
matrices used for human consumption may lead to risks for con- determine zolpidem and its predominant metabolite zolpidem
sumers [53], eventually triggering bacterial multidrug resistance. phenyl-4-carboxylic acid in body fluids and solid tissues from au-
Therefore, the analysis of antibiotic residues in foodstuffs is very topsies. The sample was passed through a Captiva ND Lipids car-
relevant and constitutes another very popular application field of tridge and cleaned with C18 and MgSO4 sorbents.
QuEChERS. Several validated methods are reported to analyse Furthermore, modified QuEChERS approaches, combined with
drugs, such as sulfonamides and its metabolites, in different foods GC-MS and LC-MS/MS, has been extensively used in the analysis of
from animal origin [98] and in baby foods [148]. Buchweitz et al. pesticides and environmental contaminants in biological tissues.
[154] proposed a combined food emergency response network This is attributable to the greater sensitivity and versatility of the
(FERN) and QuEChERS approach to pentobarbital extraction to- method for the detection of a broad number of target analytes, even
wards its quantification in dog food. In this method the partition at trace amounts. Regarding pesticides determination, a very rele-
process was performed only with NaCl and the clean-up included vant study was carried out by Srivastava et al. [184] to assess the
MgSO4, C18 and bondesil sorbents. Despite its versatility and wide presence of pesticide residues in the top of the food chain, in hu-
application, QuEChERS is still not very convenient for the recovery man plasma. Accordingly, the authors developed and validated a
of polar veterinary drugs, such as penicillin, tetracycline and qui- simple, cost-effective and rapid mini-QuEChERS approach com-
nolone, among others, and improvements are still necessary in this bined with GC-MS/MS for the simultaneous analysis of 31 multi-
regard. class pesticide residues (organophosphates, organochlorines, and
synthetic pyrethroids) in human plasma. The mini-QuEChERS
3.3. Pharmaceutical and clinical analysis approach was optimized and the best results were achieved
when using EtAc with 2% HAc and 400 mg MgSO4, followed by d-
Pharmaceutical products play an important role in the treat- SPE for extract clean-up with 50 mg of PSA per 1 mL of human
ment and prevention of diseases in both humans and animals. It is plasma. In turn, a very interesting work using QuEChERS was
proposed by Pajewska et al. [187] to quantify ZEA and one of its approach represents an innovative application for the estimation of
metabolites, a-zearalenol in human endometrial cancer tissues. The PPCPs and may be used both for routine monitoring and regulatory
relevance of this work lies in the fact that the authors optimized purposes [40].
several steps of the QuEChERS extraction process, namely the The importance of the control of pesticide presence in the
MeOH/EtAc extraction and several d-SPE sorbents, as well as the context of food safety composition has already been highlighted. In
subsequent HPLC-FLD or UHPLC-QTOF/MS analysis of ZEA. Due to this context, Mondal et al. [198] proposed a modified QuEChERS
its structural similarity with estrogen, ZEA is classified as a xen- method combined with GC-MS/MS for the determination of pes-
oestrogen, acting as an endocrine disruptor in the human body. For ticides in sediments. Pesticide extraction was performed using EtAc
this reason, the role of ZEA in endometrial cancer, one of the most as the extraction solvent, while PSA, florisil and MgSO4 sorbents
commonly diagnosed cancers in women, is being exhaustively were used in the clean-up step. The performance characteristics for
studied and its presence in the food composition is being tightly the selected pesticides were acceptable according to the European
monitored. A recent study performed by Lehman et al. [183] used Commission (EC) guidelines for method validation (recovery from
the QuEChERS procedure for the simultaneous extraction of 37 70 to 120%, RSD lower than 20%). On the other hand, Nannou et al.
multiclass pesticides in human hair. In this study, the d-SPE step [197] proposed a QuEChERS method to extract pesticides from
was performed using the Z-Sepþ sorbent, which allowed for the sediments using MeCN acidified with HAc as an extraction solvent
recovery of pesticides with high sensitivity, precision, and accuracy. and MgSO4 and NaOAc as salts in partitioning step used. These
Persistent organic pollutants (POPs) represent a huge class of authors also obtained good recoveries (71e106%) and satisfactory
heterogeneous organic compounds that have been released into precision (RSD < 21%). Cheng et al. [203] proposed a modified
the environment, through human activities and they are consid- QuEChERS method combined with atmospheric pressure gas
ered to be priority pollutants by governmental and regulatory chromatography quadrupole-time-of-flight mass spectrometry
agencies [235]. Cruz et al. [182] developed a QuEChERS method (APGC-QTOF-MS) for the simultaneous determination of OCPs in
combined with the d-SPE method to quantify PBDEs and soils using a combination of HEX with acetone (9:1 v/v) as extrac-
methoxylated PBDEs (MeO-PBDEs) in distinct seafood matrices tion solvent, NaCl as partition salt, and florisil and MgSO4 as sor-
(muscle, liver). In this study several solvents (e.g. MeCN, EtAc, HEX, bents in the clean-up step. Regarding herbicides, Kaczyn ski et al.
isopropanol and a mixture of MeCN:toluene (4:1, v/v)) were tested, [20] developed a QuEChERS protocol to analyse acid herbicides,
with the highest extraction efficiency being achieved using a including phenoxy, pyridine, aliphatic and aromatic acids, from soil
MeCN:toluene (4:1 (v/v)) solution. using acidic Al2O3 as a sorbent in the clean-up step. In turn, Mei
et al. [21] in the determination of amine herbicides in soil used NaCl
3.4. Environmental contaminants salt in the partitioning step, MeCN:H2O (1:1 v/v) as the extraction
solvent and performed the clean-up with PSA, GCB, C18 and MgSO4.
Particularly since the end of the 20th century, the prevalence of Finally, Xu et al. [202] developed a fast and simple QuEChERS
environmental contaminants in air, soil, sediments and water has method coupled with the LC-MS/MS method for the simultaneous
generated increasing public concerns. Even at trace levels, many of analysis of cyazofamid (a fungicide of the novel cyanoimidazole
these compounds are known to promote mutagenic and carcino- class) and its primary metabolite, 4-chloro-5-p-tolylimidazole-2-
genic effects. For this reason, the release of contaminants into the carbonitrile (CCIM), in soil and tomato samples.
environment should be controlled and its presence monitored us-
ing high-through analytical methods. In this regards, and as 3.5. Multiclass analysis
described in Table 1, the QuEChERS protocol has been extensively
applied in the analysis of a wide variety of environmental con- Multiclass analysis is a modern analytical approach that relies
taminants including PAHs, pesticides (e.g. OCPs, amine herbicides), on carrying out several targeted analyses with the purpose of
PPCPs, among others. These compounds constitute the most sig- covering a broad range of contamination sources and quantifying as
nificant environmental contaminants and have been assayed in many contaminants as possible. Ideally, a multiclass method should
soils [11,20,200e202,236], sediments [197,198] and sewage sludge be simple, cost-effective, easy to perform, able to cover a wide
[237]. It is well known that PAHs constitute an extensive class of range of analytes, and require a low amount of solvent and reagents
organic pollutants with potential risk for human health, being compared with the single analysis approach. Recently different
classified as priority pollutants to be monitored by the EU and the studies have used multiclass methods to analyse different chemical
US EPA. PAHs are composed of two or more aromatic rings and are groups in single analysis [30,184]. For example, Reichert et al. [4]
produced by incomplete combustion processes [238]. Several developed a QuEChERS procedure for the simultaneous analysis of
studies have been performed regarding this family of contaminants pesticides and mycotoxins in raw coffee beans using MgSO4 in the
with the main goal of reducing their harmful effects in the envi- partitioning step and skipping the subsequent extract clean-up
ronment and, consequently, to human health. This has required the step. These conditions were selected after QuEChERS optimiza-
development of accurate methods to assess its presence, such as tion in terms of MeCN being acidified with either HAc or FA, with or
the QuEChERS/GC-MS/MS approach proposed by Wang et al. [201]. without buffer, and with or without clean-up of the extracts before
Here, the determination of PAHs in top layer (0e10 cm), middle the LC-MS/MS analysis. Imamoglu et al. [230] developed a fast and
layer (10e30 cm), and bottom layer (30e50 cm) soils was per- simple EtAc multiclass method based on LC-MS/MS to determine
formed using DCM as the extraction solvent, Na2SO4 as partitioning 26 veterinary drugs and 187 pesticide residues in milk. This method
salt and PSA, C18 and Na2SO4 as sorbent in clean-up step. On the was validated according to the criteria set in the Commission De-
other hand, the presence of PPCPs in aquatic environments has cision 2002/657/EC and SANTE/11945/2015. Han et al. [73] evalu-
raised concerns due to their potential harmful effect, even at trace ated a new carbon/zirconia-based sorbent, Supel™ QuE Verde, for
concentrations [40]. In this context, a modified QuEChERS method the clean-up of food extracts for in the multiclass analysis of pes-
was proposed by Kachhawaha et al. [40]. for the analysis of mul- ticides and environmental contaminants. In addition, Al-Alam et al.
ticlass PPCPs in surface and sewage water. The proposed method [207] purposed a QuEChERSeSPME method for the simultaneous
using MeCN acidified with HAc as extraction solvent and MgSO4 analysis of 90 pesticides, 16 PAHs and 22 polychlorinated biphenyls
and NH4CH3CO2 in the partitioning step, while sample clean-up (PCBs) in honey. Regarding biological samples, Sell et al. [205] re-
step was skipped. According to the authors, this modified ported a new analytical multiclass method based on QuEChERS
method, that has proven to be effective in diagnosing fatal analytical performance without disadvantages of the referred
poisoning cases in animals. The reported method has been devel- methods, like the need for specific devices, as microwaves or ul-
oped for the determination of analytes in animal livers comprising trasounds (Fig. 2). The analysis of pesticides in food matrices is
rodenticides, carbamate, organophosphorus pesticides, coccidio- another application in which QuEChERS is widely used. Overall, in
stats and mycotoxins. Cloutier et al. [221] proposed a fast and the studies presented in Table 2 [163,239e244], QuEChERS is again
rugged method for the analysis of PCBs, PAHs, polybrominated the extraction protocol that performs better and so, to avoid an
diphenyl ethers (PBDEs), polychlorinated dibenzodioxins and di- excessive repetition, we will focus primarily on the examples that
benzofurans (PCDD/Fs) in biological tissues using QuEChERS did not confirm this trend and possible reasons contributing to that
extraction and a clean-up by gel permeation chromatography (GPC) result. Chen et al. [240], for instance, reported that ME-IL-VALLME
and silica SPE. Gao et al. [209] proposed two simple and efficient provides a higher enrichment factor and consequently a better
pretreatment procedures for the simultaneous extraction and analytical performance than conventional QuEChERS in the anal-
clean-up of six novel brominated flame retardants (NBFRs) and ysis of difenoconazole in cowpea. In turn, Di et al. [243] analysed
eight common PBDEs in human serum. Vijayasarathy et al. [214] OCPs in soils, and reported that MAE and QuEChERS extraction
described a multiclass method for the simultaneous quantification methods generally yielded higher results compared to the USE and
of PCBs, PBDES, OCPs and PAHs in green turtle blood. In the envi- ASE, while the lowest recovery (57%) for 2,40 -Dichlorodiphenyl)
ronmental context, Ramos et al. [232] proposed a QuEChERS/ dichloroethane (o,p0 -DDD) was obtained using the QuEChERS
GCeMS/MS methodology to extract synthetic musk compounds method. Thus, MAE proved to be the most efficient method to
(SMCs) and ultraviolet-filters (UVFs) from sewage sludge. Accord- analyse these target analytes in soil. In another report, Orellana-
ing to these authors, the best conditions achieved to extract the Silla et al. [163] reported the advantages of using smart materials
target compounds simultaneously were 500 mg freeze dried such as immunosorbents in the analysis of forchlorfenuron in fruit
sludge, 2.5 min of vortex, 15 min ultrasound and a partitioning salt juices by ion mobility spectrometry (IMS). The analytical perfor-
mixture composed by 500 mg MgSO4, 410 mg C18 and 315 mg PSA. mance of the proposed immunosorbent when compared with
Then, the supernatant was transferred to an amber vial, evaporated QuEChERS and C18-based SPE, gave the cleanest extracts for accu-
to dryness under a gentle N2 stream and reconstituted in 500 mL of rate determinations of forchlorfenuron by IMS. On the other hand,
HEX. the QuEChERS method showed better performance than SPE and
LLE for the determination of pesticides in roots and rhizomes of
4. Comparison of QuEChERS with other extraction methods Chinese herbal medicines [241] and in honey and honey bees [245].
In turn, Dong et al. [246] compared the extraction efficiency of
As described in Table 1, the range of QuEChERS applications is SPE and QuEChERS clean-up for the analysis of mycotoxins in fruits
very broad. The relevance of QuEChERS has allowed for its com- and vegetables, and SPE showed more selectivity, accuracy and
parison with reference methods in different applications. These precision in mycotoxins determination.
methods include different forms of LLE, solid liquid extraction Regarding the analysis of different pharmaceutical compounds,
(SLE), SPE, ASE, MAE, UAE, among others, depending essentially in Sichilongo et al. [185] looked at six sample extraction techniques,
the nature of the analytes to extract and the complexity of the i.e. QuEChERS (Q), liquid extraction (LE), protein precipitation
matrix. In the analysis of soil contaminants, for instance, the (PPT), Q-PPT, Q-LE and LE-PPT, for the extraction of antiretroviral
laborious, time-consuming and not environmental-friendly Soxhlet drugs emtricitabine, tenofovir, efavirenz, lopinavir and rotinavir in
extraction has been progressively replaced by more efficient human blood plasma. The results obtained demonstrated that the
methods, as ASE, MAE or UAE. However, nowadays QuEChERS is a mixed modes presented slightly lower recoveries, but Q-LE
high-throughput valid alternative, able to deliver similar or better compared well with the single modes at slightly higher spike levels.
Fig. 2. Overview of QuEChERS features and advantages over other extraction methods. Abbreviation: ASE - accelerated solvent extraction, d-SPE - dispersive solid-phase extraction,
GC - gas chromatography, LC - liquid chromatography, LLE - liquid-liquid extraction, LLME - liquid-liquid microextraction, MAE - microwave-assisted extraction, MeCN e aceto-
nitrile, MEPS e microextraction in packed sorbent, SBSE - stir bar sorptive extraction, SDME, SLE - solid-liquid extraction, SPE - solid-phase extraction, Soxhlet e soxhlet extraction,
SPME - solid-phase microextraction, USE - ultrasonic solvent extraction.
Table 2
Comparison of the efficiency of different extraction approaches for selected applications.
Analytes Matrix Extraction procedures Best extraction procedure Analytical method Observation Ref
Pesticides
10 OCPs Soils ASE, MAE, UAE, QuEChERS MAE GC-ECD, GC-MS/MS MAE and QuEChERS yielded higher recoveries, but lowest [243]
recovery for one of the analytes was obtained using
QuEChERS
Difenoconazole Cowpea ME-IL-VALLME, QuEChERS ME-IL-VALLME LC,LC-MS/MS ME-IL-VALLME method provides higher enrichment factor [240]
compared with conventional QuEChERS
Forchlorfenuron Fruit juices SPE, QuEChERS, IMS IMS IMS IMS provides the cleanest extracts for accurate [163]

determination of forchlorfenuron.
10 Pyrethroids (insecticides) Fruit juices DLLME, QuEChERS-DLLME, QuEChERS QuEChERS-DLLME GC-ECD, GC-MS The two methods provided acceptable recoveries and [242]
repeatability, but QuEChERS-DLLME has a broader
application to more complex matrices
12 Pesticides Soil SLE, QuEChERS, Soxhlet extraction QuEChERS GC-MS Lower LODs (<12 mg/kg) and higher recoveries (54e103%) [239]
were achieved by QuEChERS
52 Pesticides Honey, honey bees SPE, LLE, QuEChERS QuEChERS LC-MS/MS The results proved that the QuEChERS protocol was the [245]
most efficient method for the extraction of the selected
pesticides in both matrices.
135 Pesticides Roots and rhizomes of SPE, QuEChERS QuEChERS LC-MS/MS Optimized QuEChERS had obvious advantages of time [241]
Chinese herbal medicines saving, high sample throughput, less labour and wide
analytical scope
6 Fungicides Wine QuEChERS-SPE, QuEChERS-d-SPE e LC-MS/MS Both approaches showed satisfactory feasibility for [244]
fungicide residue analysis in wine samples
Contaminants
9 Parabens Drinking water SPE, QuEChERS e LC-MS/MS Both methods proved to be selective and sensitive, and [48]
showed higher recoveries, 70e155% for SPE and 62e119%
for QuEChERS.
Mycotoxins
7 Mycotoxins Fruits, vegetables SPE, QuEChERS SPE UHPLC-MS/MS SPE showed more selectivity, accuracy and precision in [246]
mycotoxins determination.
Pharmaceuticals
11 Pharmaceuticals Celery, lettuce ASE, QuEChERS QuEChERS LC-MS/MS QuEChERS was comparable to or better than ASE [247]
Forchlorfenuron (plant Apples, kiwis, grapes SPE, QuEChERS QuEChERS LC-UV, QuEChERS was cheaper, safer, and less time-consuming [248]
growth regulator) LC-MS/MS than SPE
5 Phytoestrogens Soy-based products UAE, SPE, QuEChERS UAE, QuEChERS HPLC-MS/MS UAE and QuEChERS were more efficient (good recoveries, [249]
sensitivity and precision for the selected compounds.
5 Antiretroviral drugs Human blood plasma LLE, LLE-PPT, PPT, QuEChERS-LLE, e LC-MS/MS All techniques can be employed for routine therapeutic drug [185]
QuEChERS-PPT, QuEChERS monitoring studies
19
The LODs for all the six sample extraction techniques fell below the ammonium adducts by atmospheric pressure ionization rather
clinically relevant therapeutic range (from 3 to 8 ppm). Therefore, it than less desirable sodium adducts [71]. Finally, the clean-up step,
was shown that all methods can be employed for routine thera- which sometimes can be skipped to simplify the QuEChERS pro-
peutic drug monitoring studies. In another report, Chuang et al. cedure without compromising the analytical performance
[247] demonstrated that QuEChERS was more effective than ASE in [4,37,47,104,220,223], is usually very important to improve recov-
the extraction of target pharmaceuticals in celery and lettuce (high ery and minimize the matrix effect [251]. Eventually, the use of two
recoveries 70e119% with RSD lower than20%). Furthermore, sequential clean-up steps in the QuEChERS method can further
QuEChERS when compared to the ASE method, offers the advan- improve the obtained results [127,149]. PSA is often the selected
tages of reduced time and costs in sample preparation, and a need sorbent for clean-up, but this should not be a selection by default.
for less amount of organic solvents. Thus, according to these au- Instead, PSA should be carefully considered and evaluated accord-
thors, the established QuEChERS method could be used to deter- ing to the target analytes, because in certain applications PSA can
mine the accumulation of multiclass of pharmaceutical residues in remove polar components of the matrix. This is a critical choice to
vegetables and other plants, which is needed to evaluate the quality design a QuEChERS method for mycotoxin extraction, as PSA may
and safety of agricultural produce consumed by humans. cause a significant loss of fumonisins B [250]. A promising alter-
The selected reports challenged QuEChERS efficiency against native for the clean-up of pesticide residues, m-PFC, was proposed
other extraction approaches often used for the same analytes and by Qin et al. [232]. This syringe-type architecture allows an
matrices. Legend: ASE - accelerated solvent extraction (or equiva- increased contact time and area between the extracts and the
lent pressurized solvent extraction, PSE, or pressurized liquid compressed sorbents, is rapid, convenient and suitable for high-
extraction, PLE), dSPE - dispersive solid-phase extraction, DLLME - throughput methods. Other alternatives involving magnetic sor-
dispersive liquid-liquid microextraction, GC-MS/MS e gas chro- bents, MIPs and carbon-based nanomaterials are being continu-
matography tandem mass spectrometry, GC-ECD - gas chroma- ously developed and their application should extend even further
tography using electron capture detector, IMS e ion mobility the QuEChERS performance, particularly in the extraction of vet-
spectrometry, LC-MS/MS - liquid chromatography tandem mass erinary drugs in different matrices [23]. QuEChERS is a generic
spectrometry, LLE - liquid-liquid extraction, MAE - microwave- sample extraction procedure particularly robust for the analysis of
assisted extraction, ME-IL-VALLME - micellar extraction combined multiclass compounds. In this context, QuEChERS automation and
with ionic liquid based vortex-assisted liquid-liquid micro- miniaturization are certainly the most requested improvements
extraction, OCPs - organochlorine pesticides, PPT e protein pre- among the analyst chemists. The QuEChERS process generally im-
cipitation, SLE - solid-liquid extraction, SPE - solid-phase plies manual centrifugation, which promotes the risk of contami-
extraction, UHPLCMS/MS e ultra performance liquid chromatog- nation during solvent collection and transfer. This problem can be
raphy tandem mass spectrometry, UAE - ultrasonic assisted avoided using centrifugation automation, where the stable emul-
extraction. sions are generally avoided because their advantages are likely
outweighed by the prolonged phase separation and susceptible
5. Recommendations and future outlooks automation (e.g., formation of stable emulsions). On the other
hand, the QuEChERS automation can be reached through the
The pretreatment of the sample, prior to the QuEChERS development of an autosampler systems that allow the treatment
extraction, is a crucial step, particularly for solid samples (e.g. soil, of several samples in simultaneous. Nevertheless, it is necessary to
food matrices), and it must be simplified as much as possible to include some manual steps namely the replacement of vials. In
allow an efficient precipitation of the target analytes. For this addition, the QuEChERS automation will allow improvements in
reason, the inclusion of mechanical procedures to help in sample reproducibility, sample throughput and compatibility with modern
homogenization, such as grinding, microwave or ultrasounds, may analytical equipment's. Online approaches, that perform clean-up
be particularly useful (Fig. 2). In the case of dried samples (e.g. soil simultaneously as the partitioning step promote the reduction of
samples) it is recommended to implement strategies like a sample analyte degradation possible in batch operations when several
rehydration step before extraction or an excess of solvent in order hours can pass before final extracts are analysed in long sequences
to increase the recovery yields [250]. MeCN is the default solvent [252]. Morris and Schriner [253] reported an automated mini-
used in QuEChERS, since it separates easily from water in the sec- column solid-phase extraction (c-SPE) clean-up QuEChERS
ond salting-out step, allowing a more efficient removal of residual approach, using a robotic X-Y-Z instrument autosampler, for anal-
water with MgSO4 when compared to other solvents. Furthermore, ysis of 263 pesticides in fruits and vegetables by LC-MS/MS. The
MeCN co-extracts less lipophilic compounds that could be present results showed that c-SPE provides better clean-up than d-SPE. In
in many samples, such as waxes, fats, and pigments. However, manual batch applications, d-SPE is easier, cheaper and faster
when extracting very volatile compounds, a non-miscible water compared to the traditional c-SPE [254]. Lehottay et al. [252]
solvent, like as DCM is preferable [201]. Regarding the salts used in applied an automated high-throughput mini-cartridge solid-phase
the salting-out step, MgSO4 is usually the first choice due to its extraction (mini-SPE) clean-up for the rapid low-pressure gas
higher capacity for water removal. Nevertheless, MgSO4, and also chromatography tandem mass spectrometry (LPGC-MS/MS) anal-
Na2SO4, are low vapour pressure salts that tend to deposit as solids ysis of pesticides and environmental contaminants in QuEChERS
on surfaces in the MS source, and potentially within the analyser, extracts of foods. The QuEChERS miniaturization is crucial partic-
which can cause a decline in the instrument performance and an ularly in cases where there is a small available sample amount, and
increased need for maintenance. In GC, the salts and matrix com- is very popular in the field of analytical chemistry due to its ad-
ponents can cause problems when depositing in the inlet liner, vantages like reduced solvent costs, salts and sorbents amount,
leading to an increased frequency of liner replacement [71]. For this easier handling, processing, and minimal amount of waste disposal
fact, the salts have been replaced by more volatile salts, as in comparison to the classical extraction procedure. These features
ammonium chloride (NH4Cl), NH4HCO2 and acetate buffers in order allow a higher throughput analysis with consequent improvement
to reduce the GC inlet replacement and to improve the compati- of accuracy and a great reduction in time and costs. The m-
bility with MS detection, since these salts can be easily evaporated QuEChERS-USAE method was developed with lower sample, par-
and/or decomposed in the ionization chamber [71,72]. Moreover, titioning salts and organic solvent requirements, while conserving
the presence of ammonium ions can enhance the formation of the analytical performance of the original QuEChERS [255]. This
improved method should foster the challenge of miniaturization Methods 10 (2017) 147e160, https://doi.org/10.1007/s12161-016-0564-9.
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Declaration of interest Ecotoxicol. Environ. Saf. 142 (2017) 181e188.
[12] Y. Ruiz-García, C.L. Silva, E. Go mez-Plaza, J.S. Ca ^mara, A powerful analytical
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All authors declare having no conflict of interest. with ultrahigh pressure liquid chromatography for evaluating the effect of
elicitors on biosynthesis of trans-Resveratrol in grapes, Food Analytical
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This work was supported by FCT-Fundaça ~o para a Cie
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with UPLC-MS/MS analysis, J. Agric. Food Chem. 65 (2017) 5049e5055,
Tecnologia (project PEst-OE/QUI/UI0674/2019, CQM, Portuguese
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Desenvolvimento da Investigaça ~o Tecnologia e Inovaça
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Rosa Perestrelois a Postdoctoral Researcher at Madeira
[238] B. Socas-Rodríguez, J. Gonz alez-Salamo, A.V. Herrera-Herrera, J. Herna ndez-
Rodríguez-Delgado, Recent advances and developments in the University and is member of the CQM (Madeira Chemistry
Borges, M.A.
Research Center) research unit. She studied Chemistry in
QuEChERS method, Compr. Anal. Chem. 76 (2017) 319e374.
Madeira University, completed a master degree in Green
[239] R.D. Ðurovi c-Pejcev, V.P. Bursi c, T.M. Zeremski, Comparison of QuEChERS
Chemistry (Faculty of Sciences of Lisbon University) and
with traditional sample preparation methods in the determination of mul-
finished her PhD in 2013, where she evaluated the po-
ticlass pesticides in soil, J. AOAC Int. (2018), https://doi.org/10.5740/jaoa-
tential of Vitis vinifera L. grapes used to produce Madeira
cint.18-0296.
wine.She published 38 SCI papers, 5 book chapters, and
[240] X. Chen, Y. Bian, F. Liu, P. Teng, P. Sun, Comparison of micellar extraction
more than 70 poster presentations in International and
combined with ionic liquid based vortex-assisted liquid-liquid micro-
National conferences and about 19 Oral communications.
extraction and modified quick, easy, cheap, effective, rugged, and safe
H-index: 22; Number of citations: 1296; ORCID nº: 0000-
method for the determination of difenoconazole in cowpea, J. Chromatogr. A
0002-7223-1022.key subject areas: Analytical Chemistry -
1518 (2017) 1e7, https://doi.org/10.1016/j.chroma.2017.08.042.
Food Chemistry - Medicinal Chemistry - Metabolomics
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extraction methods for the determination of 135 pesticides in Corydalis
Rhizoma, Chuanxiong Rhizoma and Angelicae Sinensis Radix by liquid
chromatography-triple quadrupole-mass spectrometry. Application to the Pedro Silva is a PhD student at Madeira University and is
roots and rhizomes of Chine, Journal of Chromatography. B, Analytical member of the CQM (Madeira Chemistry Research Center)
Technologies in the Biomedical and Life Sciences 1017e1018 (2016) research unit, graduated in Biochemistry in 2008 (Madeira
233e240, https://doi.org/10.1016/j.jchromb.2016.03.003. University) and MSc in Applied Biochemistry (Madeira
[242] Y. Zhang, X. Zhang, B. Jiao, Determination of ten pyrethroids in various fruit University) in 2011. Actually, he develops studies in food
juices: comparison of dispersive liquid-liquid microextraction sample analysis, analytical chemistry and metabolomics
preparation and QuEChERS method combined with dispersive liquid-liquid domains.He published 12 SCI papers, 1 book chapters, and
microextraction, Food Chem. 159 (2014) 367e373, https://doi.org/10.1016/ more than 30 poster presentations in International and
j.foodchem.2014.03.028. National conferences. H-index: 5; Number of citations: 73;
[243] S. Di, S. Shi, P. Xu, J. Diao, Z. Zhou, Comparison of different extraction ORCID nº 0000-0003-1487-9346.Key subject areas: Food
methods for analysis of 10 organochlorine pesticides: application of MAE- Chemistry - Analytical Chemistry - Metabolomics
SPE method in soil from Beijing, Bull. Environ. Contam. Toxicol. 95 (2015)
67e72, https://doi.org/10.1007/s00128-015-1538-0.
Priscilla Porto-Figueira (ORCID 0000-0001-7773e182X) Dr Sonia Medina received her PhD in Agro-Food Resources
has a master's degree in applied Biochemistry by the and Technologies in 2012. Her current research interests
Madeira University in 2016. She won the award for Best focus on the development of comprehensive data analysis
Student 1st Cycle in Biochemistry in 2014 and the Best strategies for volatile and non-volatile bioactive com-
Student 2nd Cycle in Applied Biochemistry in 2017, both in pounds by metabolomics approaches. She worked from
Madeira University. Currently, Priscilla is PhD Student with 2012 to 2016 as scientific researcher at Spanish National
a fellowship by FCT (SFRH/BD/129630/2017) and with her Research Council and held a postdoctoral stay in Lasallian
work she contributes to increase knowledge in different University in Medellin, Colombia. Since 2017, she is a post-
areas of analytical chemistry, particularly in the charac- doctoral researcher in Madeira Chemistry Research Center
terization of putative biomarkers for high prevalence dis- (CQM) at the University of Madeira, Portugal. She (co-)
eases, such as cancer. She is also highly involved in other authored more than 50 scientific papers and nine book
activities of a multilateral projects aiming to evaluate the chapters.
performance of different analytical strategies based on
microextraction techniques and the characterization of
different natural products. Since 2013, she published 12
papers in international peer reviewed journals and 1 book Jose S. Ca
^mara received his M.Sc. degree in Quality Control in Chemistry in 1997 at the
chapter. She has attended several international and na- University of Coimbra. In 2004 he obtained his Ph.D. in Chemistry (Analytical Chem-
tional conferences in the Extraction techniques and istry) at University of Madeira Between 1993 and 2004 he worked in University of
Analytical Chemistry fields. Overall, she presented and Madeira as a Lecturer and as researcher with Professor Jose Carlos Marques on the
coauthored more the 30 oral communications and over 30 Analytical Characterization of Madeira wines. In 2004 he joined the University of
poster communications in these conferences. Madeira as Assistant Professor where he started his independent research on Food
Chemistry and after on Medicinal Chemistry. Since 2004 is senior member at CQM
where he is currently developing his research. From 2016 is member of the Executive
Jorge Augusto Machado Pereira (ORCID 0000-0003-0316- committee of CQM and he is responsible of the Natural Products Research group of
5348, Scopus 55613752500, publons.com/a/257264/) has a CQM. Is supervisor of Ph.D. and M.Sc. thesis and Director of the Course of Chemistry
PhD in Biochemistry (2008, ITQB/Universidade Nova de and CET on Hygiene and Food Security. He is coordinator of ERA-Net projects.Jose S.
Lisboa) and his current research in Madeira Chemistry Ca^mara is coauthor of more than 100 papers (h ¼ 38: i10 ¼ 65. Google Scholar)
Research Center (CQM, Madeira University) has contrib- including several reviews, encyclopedia and book chapters, in addition to more than
uted to span the use of more efficient microextraction 350 communications in International and National conferences. He is Associate Editor
techniques in different fields of research, particularly in the of JIOMICS and member of Editorial Board of some journals. His research interests
characterization of putative biomarkers for highly preva- include: Development of methodologies for extraction and analysis of volatile com-
lent diseases, as cancer and cardiovascular diseases. He has pounds and several secondary bioactive metabolites from different food or food-
published 25 papers, 9 books and book chapters and 34 related matrices (SPME, SPE; MEPS, GCO, GC-MS; LC-MS; UHPLC); Medicinal Chemis-
abstracts in international peer review journals and he has try and Metabolomics: validation of analytical approaches that may provide the
attended 27 international conferences, in which he pre- biochemical basis to study pathologies or can be implemented as a diagnostic tool
sented and coauthored 39 oral communications and over based on urine, saliva and exhaled breath matrices as non-invasive sampling strategies.
80 poster communications. He is Editor of an International Volatomics and urinomics studies related with breast, lung, and colorectal cancers.
peer reviewed Journal and a frequent reviewer of different Biomarkers of Oxidative Stress correlated with cardiovascular and cancer diseases.
journals and project funding calls. Food bioactive metabolites; Food antioxidants; Volatile metabolites as biomarkers of
several diseases including asthma and cancer; Metabolomics; Development and imple-
mentation of microextraction methodologies ORCID ID: 0000-0003-1965-3151
Catarina Luís Silva is a PhD student at Madeira University Researcher ID: G-3003-2013 Scopus Author ID: 10140393000 Publons: publons.com/
and is member of the CQM (Madeira Chemistry Research a/1206082/.
Center) research unit.After her graduation in Biochemistry
in 2004 (University of Porto e UP), Catarina got an MSc in
Applied Biochemistry (Madeira University) in 2009, where
she established the volatile metabolic profile of potential
biomarkers in individuals with oncologic pathologies.She
published 27 SCI papers, 3 book chapters, and more than
40 poster presentations in International and National
conferences. H-index: 14; Number of citations: 668; ORCID
nº: 0000-0002-3018-3165.Key subject areas: Analytical
Chemistry - Food Chemistry - Medicinal Chemistry
Metabolomics

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Analytica Chimica Acta xxx (xxxx) xxx

Contents lists available at ScienceDirect

Analytica Chimica Acta

QuEChERS - Fundamentals, relevant improvements, applications and

Modiﬁcation and miniaturization of

Abbreviations HPLC-UV High performance liquid chromatography with

OCPs Organochlorine pesticides ESCF European Commission's Scientiﬁc Committee for

1. Introduction of extract and sorbent, and allows the reduction or elimination of

Application ﬁelds of QuEChERS.

Matrices (target analytes)a QuEChERS Analytical method Validation parameters Ref

Extraction Solvents Partition salts/Buffers Clean-up Rec. (%) LOQ

R. Perestrelo et al. / Analytica Chimica Acta xxx (xxxx) xxx

Matrices (target analytes)a QuEChERS Analytical method Validation parameters Ref

Extraction Solvents Partition salts/Buffers Clean-up Rec. (%) LOQ

R. Perestrelo et al. / Analytica Chimica Acta xxx (xxxx) xxx

R. Perestrelo et al. / Analytica Chimica Acta xxx (xxxx) xxx

Matrices (target analytes)a QuEChERS Analytical method Validation parameters Ref

Extraction Solvents Partition salts/Buffers Clean-up Rec. (%) LOQ

R. Perestrelo et al. / Analytica Chimica Acta xxx (xxxx) xxx

R. Perestrelo et al. / Analytica Chimica Acta xxx (xxxx) xxx

Matrices (target analytes)a QuEChERS Analytical method Validation parameters Ref

Extraction Solvents Partition salts/Buffers Clean-up Rec. (%) LOQ

R. Perestrelo et al. / Analytica Chimica Acta xxx (xxxx) xxx

R. Perestrelo et al. / Analytica Chimica Acta xxx (xxxx) xxx

Environ. Sci. Pollut. Control Ser. 25 (2018) 27594e27605, https://doi.org/ 2016.06.019.

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