Industrial Crops & Products 145 (2020) 112079

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Industrial Crops & Products

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Antioxidant capacity of the extracts from flowers of Erica australis L.: T

Comparison between microwave hydrodiffusion and gravity (MHG) and
distillation extraction techniques - Formulation of sunscreen creams
L. López-Hortasa, E. Condeb, E. Falquéc, H. Domíngueza, M.D. Torresa,*
a
Department of Chemical Engineering, Faculty of Sciences, University of Vigo, Edificio Politécnico, As Lagoas s/n, 32004 Ourense, Spain
b
GLECEX S.L., Edificio CEI, Parque Tecnológico de Galicia s/n, 32900 San Cibrao das Viñas, Ourense, Spain
c
Department of Analytical Chemistry, Faculty of Sciences, University of Vigo, Edificio Politécnico, As Lagoas s/n, 32004 Ourense, Spain

A R T I C LE I N FO A B S T R A C T

Keywords: Microwave hydrodiffusion and gravity (MHG) extraction of Erica australis flowers was optimized evaluating
Green extraction different microwave irradiation powers (25−200 W). Collected extracts were compared with the liquid phase
Personal care obtained by conventional distillation. Their total phenolic content, antioxidant capacity and color features were
Rheology evaluated. Microscopical properties of the flower tissues allowed assessing the distinct effects of the extraction
Wild flowers
processes. The cosmetic application of the collected bioactive extracts in the formulation of sunscreen creams
with waters from three different thermal spring waters and the corresponding characterization (e.g. chemical,
bioactive and rheological features) and sensory analysis were also made. For cosmetic comparative purposes,
extracts from Ulex europaeus flowers obtained by MHG procedure was also analyzed. The stability of these oil-in-
water model emulsions was tested during accelerated oxidation conditions. Results indicated that MHG at 50 W
for 130 min was the most adequate work conditions for the extraction of antioxidant compounds from these wild
flowers (around 0.27 mg Trolox eq/g flower dry weight and 0.01 mg ascorbic acid/g flower dry weight or
0.04 mg FeSO4 * 7H2O/g flower dry weight). This procedure also led a drop of energy consumption environ-
mental impact (about 8 times less) in comparison with distillation method. Small total color differences were
detected between the gathered extracts. The incorporation of flower extracts produced similar effects when
compared with added commercial antioxidants except for viscous behavior. Sensorially, E. australis extract in-
corporated with thermal waters displayed a positive effect on the skin cream application of the formulated
cosmetic, mainly with thermal water 3.

1. Introduction benefits against diseases (Embuscado, 2015). Green extraction pro-

The valorization of wild underused flowers is a scientific challenge
with a huge potential in the natural extracts market. Erica australis L.
could be a promising source of antioxidants, with potential healthy
features. Extracts from this plant have shown antibacterial and anti-
tumoral properties as well as increasing the metabolic activity in fi-
broblast proliferation responsible for tissue regeneration so the appli-
cation of extracts from this plant can be an improvement in their health
benefits. (Nunes et al., 2014). These protective effects promote the
exploitation of the treatment of diseases (e.g. tumoral process) using the
natural compounds derived of this source widespread in the forest
ecosystems of the Iberian Peninsula (Farzaneh and Carvalho, 2015).
An increasing demand of natural extracts was observed in the last
few decades due to their bioactive compounds with potential health
cesses are being developed in recent times to respond to this request
with efficient methodologies that favor a lower environmental impact
and energy consumption (Perino and Chemat, 2019). In contrast to
conventional extraction procedures as solid-liquid extraction, in-
novative microwave-assisted extraction methods allow saving time,
energy and resources as minimizing used solvents. This last case is that
of the novel microwave assisted hydrodiffusion combined with gravity
(MHG) extraction system employed to the removal of interesting
bioactive chemicals from botanic and marine resources as well as by-
products (Angoy et al., 2018; Flórez-Fernández et al., 2018; Ravi et al.,
2018).
Several cosmetic purposes were extensible studied for extracts from
other wild flowers as Calendula officinalis or Crocus sativus (Arya et al.,
2014; Chitrakar et al., 2019; Madan and Nanda, 2018). From this

⁎
Corresponding author.
E-mail address: matorres@uvigo.es (M.D. Torres).

https://doi.org/10.1016/j.indcrop.2019.112079
Received 13 October 2019; Received in revised form 30 November 2019; Accepted 28 December 2019
Available online 02 January 2020
0926-6690/ © 2019 Elsevier B.V. All rights reserved.
L. López-Hortas, et al.
reason, potential applications for personal care products as sunscreen
creams can be developed by E. australis flowers since this utilization
have not yet been studied.
The rheological testing, in terms of viscosity behavior of cosmetics
as creams, is dramatically relevant for some factors like to know the
required force to remove the cream from the bottle (yield stress), to
simulate the flow initial application of the skin (apparent viscosity at
low shear rates) or to simulate the application across large body surface
(apparent viscosity at high shear rate) (Houlden, 2018). These studies
are especially relevant when extracts are added to conventional for-
mulations, since the viscoelastic properties can be dramatically mod-
ified which involves a challenge the cosmetics processing and quality to
the end products.
The main goal of this work was the selection of the most adequate
MHG conditions to recover antioxidant compounds from E. australis
flowers. A parallel objective was the comparison with a traditional
extraction technique as steam distillation system. The yield and energy
consumption of these extraction methods were also examined. A mi-
croscope study of the samples after the extraction procedures was
realized in order to determine the structural changes in the flowers
tissues during the employed extraction systems. The corresponding
extracts were characterized by color features and antioxidant protocols.
Optimum extracts were used to formulate functional sun creams en-
riched with three different thermal waters. These creams were tested to
determinate some fundamental cosmetic features and to evaluate the
possible acceptance by potential consumers.
2. Materials and methods
2.1. Materials
Fresh flowers were collected in San Xoán de Río (Ourense, NW
Spain) and stored in hermetic bags at freezing temperature
(-18 ± 2 °C). Afterwards, the flowers were defrosted in a fridge
(4 ± 2 °C) for 24 h until further use in the tested extraction systems.
These flowers presented tubular-bell-shaped with reflexed petal lobes of
rose-purple to pink color during their full flowering stage. The ash,
extract and moisture content determined by using standard methods
was of 1.92 ± 0.02 %, 31.91 ± 0.26 % and 66.35 ± 0.54 % wet
basis, respectively. All used reagents were of analytical grade.
2.2. Bioactive compounds extraction procedures
Emerging microwave hydrodiffusion and gravity and conventional
steam distillation extractions were used to recover the bioactive frac-
tions of E. australis L. flowers. MHG extractions were conducted at least
in duplicate on a multimode microwave extractor (NEOS-GR, Milestone
Srl, Italy) as reported elsewhere (Binello et al., 2014). Briefly, about
100 g of defrosted flowers were placed on an open vessel (1.5 L). Then,
they were irradiated at different microwave powers (25, 50, 100, 150
and 200 W). These conditions were selected based on the results pre-
viously reported for other similar materials (López-Hortas et al., 2016).
Monitoring of the collected volume (each 5 mL), time and temperature
were made in all cases. It should be indicated that the MHG treatment
was ended when it was not possible to collect more liquid fractions. All
liquid extracts were drained by gravity on a condenser outside the
microwave device. Afterwards, the fractions were mixed at room tem-
perature and were stored in a fridge (4 ± 2 °C) in darkness until further
use. Note here that steam distillation extraction was made following the
traditional procedure reported elsewhere (López-Hortas et al., 2016;
López-Hortas et al., 2019).
2.3. Expected environmental impact
An estimation of the extraction procedures environmental influ-
ences was determined following the indications reported elsewhere
2
Industrial Crops & Products 145 (2020) 112079
(Benmoussa et al., 2018). Concisely, the required dioxide carbon re-
leased was calculated considering 800 g of CO2 by the consumed of
1 kW h from coal or fuel.
Estimated energy consumption of the studied extraction methods
could be determined by the following equation (Darvishi et al., 2013):
E = tP Eq. (1)
2.4. Scanning electron microscopy of flower tissues
Defrosted E. australis flowers, the solid phase obtained after MHG at
different irradiation powers and after steam distillation without coho-
bation system were freeze-dried. Then, tested samples were fixed onto
aluminium stubs and sputter coated with gold to perform the micro-
scopy measurements using an Emitech K550X (Quorum Technologies
Ltd, UK) equipment. Above samples were analyzed at least in duplicate
by means of a Field Emission Ion (FEI) (QUANTA 200, FEI Company,
The Netherlands) electron scanning microscope (SEM) under vacuum
conditions at an accelerating voltage of 15.0 kV.
2.5. Determination of the extracts features
2.5.1. Total phenolic content and antioxidant profile
Folin-Ciocalteu method was used to determine the total phenolic
content of the MHG and distillation collected liquid fractions (Singleton
and Rossi, 1965). The obtained content was expressed as milligrams of
gallic acid equivalents (GAE). Concisely, 0.50 mL of the collected liquid
extracts or the standard (gallic acid) were dispersed in 3.75 mL distilled
water. Folin-Ciocalteu reagent (1:1, v/v, 0.25 mL) and sodium carbo-
nate solution (10 %, w/v, 0.50 mL) were also added to the mixture.
After keeping the samples in darkness at room temperature for 1 h, the
absorbance was read (765 nm).
The method proposed by Re et al. (1999) was employed to obtain
the ABTS (2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) dia-
mmonium salt radical cation scavenging capacity of above samples. It
was expressed as Trolox equivalents antioxidant capacity (TEAC) value.
Briefly, 20 μL of samples or standard (Trolox) were added to 2.00 mL of
diluted ABTS·+ solution. Samples were stored at 30 ± 2 °C for 6 min
and subsequently the corresponding absorbance was measured
(734 nm).
The ferric reducing antioxidant power (FRAP) test (Benzie and
Strain, 1996) was used to determine the reduction of the ferric 2,4,6-
tripyridyl-s-triazine (TPTZ) complex for a set of liquid fractions col-
lected by MHG. Distillation liquors were also analyzed with compara-
tive purposes. As standard, ascorbic acid and iron (II) sulphate hepta-
hydrate were used. Liquors (100 μL) were dispersed in the FRAP
reagent (3.00 mL). Then, the absorbance was measured (593 nm) after
6 min at room temperature.
The DPPH (α,α-diphenyl-β-picrylhydrazyl) radical scavenging ac-
tivity of aforementioned samples was obtained according to the pro-
cedure of von Gadow et al. (1997). Briefly, liquors (50 μL) and DPPH
radical solution (2.00 mL) were mixed. Next, the absorbance drop from
0 to 16 min was read (515 nm) employing a blank sample (distilled
water). Note that the inhibition percentage was determined. All above
trials were made at least in triplicate.
2.5.2. Color features
The color properties of the collected fractions and set of fractions of
the aqueous phase of defrosted E. australis flowers treated by MHG and
distillation were conducted at least in quintupled on a CR-400 colori-
meter (Konica Minolta, Japan). CIEL*a*b* system was used to present
the parameters and magnitudes, being L* the lightness (whiteness,
L* = 0, or brightness, L* = 100), a* the red/green coordinate (redness,
a* > 0, or greenness, a* < 0) and b* the yellow/blue coordinate (yel-
lowness, b* > 0, or blueness, b* < 0). Concerning magnitudes, C* and
L. López-Hortas, et al.
S* are hue (h (º)), chroma (C*) and saturation (S*) were calculated as
indicated below.
b*
h (º) = arctan( ) pH values and color test were got following the above instructions.
a* (2)
C* = (a * + b*)
(3)
C Succinctly, 1 g of cream was mixed until 25 mL with 96 % (v/v) ethanol
S* =
L* (4)
The total color (ΔE*) and hue (ΔH*) differences were also calculated
as indicated below.
ΔE* = (ΔL*)2 + (Δa *)2 + (Δb*)2 (5)
ΔH* = (ΔE*)2 − (ΔL*)2 − (ΔC*)2 (6)
2.5.3. pH determinations
pH measurements of the flower extracts were done with pH-meter
counter GLP 21 (Hach Lange Spain, S.L.U., Barcelona, Spain) at room
temperature. Standard solutions were used to perform a prior electrode
calibration.
2.5.4. Total solid content
The total solid content of the collected extracts was analyzed
gravimetrically using an extract aliquot sample (1 mL) by oven drying
at 105 °C during 24 h. The results were expressed as g dry residue/L.
Then the total solid extraction yield (g extract/g raw material dry
weight) could be estimated considering the moisture content of the
defrosted flower.
2.5.5. Sun protection factor
Sun protection factor (SPF) value was determined using Kaur and
Saraf (2010) protocol. In short, samples (20 μL) were mixed with 40 %
(v/v) ethanol solution (1980 μL) and scanned between 290 and 320 nm
at 5 nm intervals. For the calculation of the SPF data was used the
equation proposed by Mansur et al. (1986) with reference to the nor-
malized product of the erythemal effect of the radiation with wave-
length and the solar intensity of the spectrum suggested by Sayre et al.
(1979).
2.6. Cosmetic applications
Sunscreen creams formulation was made at least in duplicate fol-
lowing the modified protocol previously reported (Balboa et al., 2014).
Briefly, components of oil cream basis (O/W) -18 g-, dimethicone 350 -6
g-, avocado oil -3 g-, sunscreen -8 g-, micronized titanium dioxide -18 g-
and fenonip XB -0.35 g-) and water (distilled or thermal water -80 g-,
carbomer 940 -1.5 g-, propyleneglycol -6 g- and triethanolamine -1.5 g-)
phases were tempered at 70 ± 2 °C and 40 ± 2 °C, respectively, in two
water baths. When oil phase blend was melted then it was transferred to
the water bath at 40 ± 2 °C and adjusted at this temperature. Then this
was added at water phase and homogenized until the formation of a gel-
like matrix. The selected flower extracts, butylhydroxytoluene (BHT)
and ( ± )-α-tocopherol commercial antioxidants or the different used
water as controls (750 μL or mass equivalent in weight), bergamot oil
(450 μL) and tetramer cyclometicone (3 mL) were added and mixed at
the O/W emulsion at room temperature before their store at re-
frigeration temperature in flasks and amber glass vials.
The employed thermal water were collected from each point of
emission in Ourense region with plastic bottles. pH, total solid content
and color features were measured in laboratory following the above
methods. Their conductivity was determined using a conductivity meter
HI 9033 (Hanna Instruments Ltd Eden Way, United Kingdom) at room
temperature.
The following fundamental characteristics were analyzed for all
3
Industrial Crops & Products 145 (2020) 112079
formulated creams.
2.6.1. pH, color, total solid content and SPF measurements
However, the total solid content of the sunscreen creams was realized
using 0.5 g of sample in the above conditions. Similarly, the cosmetic
SPF assays were realized following Dutra et al. (2004) procedure.
solution and centrifuged at 500 rpm during 5 min. The next step was
submitted the solution at ultrasonication for 5 min and filtered it. The
absorbance of the mixture was scanned between 290 and 320 nm
considering in the mathematical calculation of the SPF data that the
necessary correction factor was 20 since a standard sunscreen for-
mulation with 5.46 % solar filter presented a low SPF value of 3.18.
2.6.2. Sensory analysis
A descriptive sensory analysis was carried out by 17 volunteers
recruited from students and staff of the Faculty of Sciences (University
of Vigo, Campus of Ourense). The nine sunscreen creams (one control
without extract and distilled water, four creams with E. australis MHG-
extracts and distilled water or thermal waters, and four formulations
with U. europaeus MHG-extracts and distilled water or thermal waters)
coded with three-digit random numbers were evaluated in one session.
A total of 13 descriptors relative to the appearance attributes (gloss,
consistency/appearance, color preference, smell intensity and smell
preference) and to the skin parameters after application (spreadability,
penetration, softness, skin gloss, skin feel, texture preference, skin smell
intensity and skin smell persistence) were evaluated. The intensity le-
vels of each sensory attributes were ranged from 0 (represents ‘none’) to
10 (‘extremely strong’). Finally, the testers expressed their overall ac-
ceptance.
2.6.3. Determination of thiobarbituric acid reactive substances (TBARS)
The degree of lipid oxidation in emulsion samples was defined by an
adapted method from Scheffler et al. (2010) so that standard (mal-
onaldehyde solution (20 nmol/mL)) or samples (0.8 g) were added to a
thiobarbituric acid-butylated hydroxytoluene (TBA-BHT) solution
(1.6 mL) in test tubes. They were vortexed for 30 s and immersed in a
water bath at 95 ± 2 °C for 15 min. Then, tubes were cooled in an ice-
tap-water bath for 10 min and centrifuged at 5000 rpm for 10 min. The
absorbance of the gathered supernatant was determined at 532 nm. The
units of TBARS outcomes were nmol malonaldehyde/g sun cream dry
weight.
2.6.4. Accelerated oxidation test
An accelerated oxidation assay at 50 ± 2 °C for 15 days was rea-
lized for evaluate the physicochemical stability of the cosmetics ela-
borated from E. australis extracts. The produced changes on their total
solid content and color characteristic were determined at the end of this
study whereas pH and TBARS test were carried out periodically on 1
day intervals.
It should be indicated that all above analytical measurements were
performed on a spectrophotometer Hitachi U-2000 (Tokio, Japan) and
determined at least in triplicate.
2.6.5. Steady-state shear measurements
The apparent viscosity versus shear rate of representative creams
was monitored using a MCR 302 controlled-stress rheometer (Paar
Physica, Austria) equipped with a sand blasted plate-plate measuring
system (25 mm diameter, 1 mm gap) to prevent possible creams slip. In
all cases, the flow curves were determined at 25 °C, controlled by a
Peltier system ( ± 0.01). Light paraffin oil was used to seal the creams
placed on the measuring system to prevent water loss during viscosity
tests. Before rheological testing, creams were rested 10 min to favor
structural and temperature equilibration. Hysteresis phenomenon was
also analyzed by measuring the apparent viscosity with shear rate
L. López-Hortas, et al.
decreasing, following the increasing one experiment. All above trials
were made at least in triplicate.
2.7. Statistical study
Physico-chemical data were analyzed by means of one-factor ana-
lysis of variance, ANOVA, employing the software PASW Statistics v.22
(IBM SPSS Statistics, New York, USA). A post-hoc Scheffé analysis was
conducted to differentiate means with 95 % confidence (p < 0.05),
whenever the variance analysis showed means differences. Sensory data
were analyzed by a two-factor (extract, water) ANOVA and the sig-
nificant differences were also studied (p < 0.05). Formulations pre-
ference and descriptive data were evaluated by principal component
analysis (PCA) and Hierarchical Cluster Analysis (HCA) using the pro-
gram Statistica 8.0 (Statsoft Inc., 2004,Tulsa, OK, USA).
3. Results and discussion
3.1. Extraction conditions effects
The determination of the impact of the microwave irradiation
powers (25, 50, 100, 150 and 200 W) during microwave hydrodiffusion
and gravity extraction for E. australis flowers on the volume of the
collect liquid phases and the time and temperature extraction allow
selecting the most suitable extraction conditions. These parameters are
displayed in Fig. 1 jointly with the data corresponding to the examined
steam distillation technique for comparison. Typical microwave heating
profiles were registered in all MHG extractions. For example, different
phases were observed at the lowest microwave irradiation (25 W)
(Fig. 1a). In this case, the first drop of extract outside the microwave
oven occurred after 37 min at 42 °C. This latency period corresponded
Fig. 1. Collected volume (bars), vessel temperature (circles) and extraction time (triangles) during MHG treatment of defrosted E. australis flowers at different
microwave irradiation power (W): a) 25, b) 50, c) 100, d) 150, e) 200 and f) distillation. Note here that y -axes scales are different in each plot.
4
Industrial Crops & Products 145 (2020) 112079
with a heating outcome near to 0.60 °C/min. Then, a second step took
place during 70 min with a regular linear heating of 0.09 °C/min up to
52 °C collecting an appreciable amount of liquid extract (15 mL), that
represented about 34 % of the collected liquid phase. The following
period corresponded with a plateau region: this third step was extended
for 138 min with an increase of heating value of 0.7 °C/min up to 58 °C.
In this interval, the obtained liquid phase was the most abundant, about
57 % (25 mL) of the total yield. Finally, a descending temperature line
was defined for a negative heating range of 0.15 °C/min for 55 min,
reaching a final temperature of 50 °C. In this stage, the collected volume
was limited and represented around 8 % (∼ 3.6 mL). This behavior
agreed with that described by Zill-e-Huma et al. (2009) for fresh onions
submitted at MHG process. This phenomenon has been accentuated
when higher irradiation powers were employed (50−200 W)
(Fig. 1b–e). The maximum temperature value was higher (around
100 °C) and consequently the extraction time and extract volume were
notably reduced. The gathered volume was about 23 mL at 200 W
treatment (Fig. 1e) employing 40 min in this extraction process. This
method did not describe the last step of the heating outline, which
could respond to the loss of the free water within the flowers tissue and
their structural collapse underwent by the microwave process.
On the other hand, distillation technology (Fig. 1f) provided a
constant increase temperature up to 120 °C in the final point of the
extraction process (135 min), corresponding with a heating issue near
to 0.74 °C/min. This method offered a total volume of 236 mL of liquid
phase: this displayed a difference around of 79 % with respect to the
maximum extract volume derived by MHG procedure at 50 W (∼
49 mL). This trend was similar to the Ulex europaeus L. flowers pro-
cessed by this same extraction procedure (López-Hortas et al., 2016).
This difference is clearly observed in Figure S1 that compiles the
effect of the treatments by MHG and distillation techniques related to
L. López-Hortas, et al.
Fig. 2. Required energy consumption at examined microwave irradiation
powers of defrosted E. australis flowers during MHG technique. Value estimated
for the aqueous phase obtained by distillation was also summarized for com-
parative purposes.
the initial volume of removed water from the defrosted flowers. It is
necessary to take into account that the moisture content of this matrix
was 66.35 ± 0.54 % wet basis. As we can see on this figure, a notably
difference was clearly observed between MHG treatments and distilla-
tion process whereas similar percentages of obtained extracts were
compiled at 25−150 W (close to 66 % of total water of the flowers).
The percentage of the collected liquid phase at the highest microwave
power was noticeable inferior (about 30 % less) but the maximum
quantify of initial volume of reclaimed water was derived by MHG
treatment at 50 W (around 74 %).
3.2. Estimated energy consumption
Fig. 2 describes the estimated energy consumption necessary for the
extraction of the collected liquid phases by MHG method and distilla-
tion process. The results pointed out a similar pattern to the last figure:
distillation system required the highest energy requirements (about
3238 kJ -equivalent to 720 g CO2 rejected into the atmosphere-) with a
remarkable difference when compared with MHG assays. These high
energy requirements could be related with the energy consumption of
the used heat source (an electrical heating mantle XC-1000 (Raypa) at
400 W) and the necessary extraction time for this extraction system. It is
perceptible that this parameter was 165 min inferior to the time ne-
cessary to process this raw material at 25 W by MHG procedure. This
extraction method presented noteworthy inferior energy requirements
(roughly 7 times less). In general, energy consumptions of MHG ex-
tractions were around 500 kJ, highlighting the extraction process at
50 W where the lowest energy values (390 kJ) were required. In terms
of energy requirements, 50 W seems to be the most adequate irradiation
power to perform the assays. Overall, MHG values were lower than the
considered energy consumption for the extraction of bioactive com-
pounds by alternative extraction technologies as essential oils from
Cinnamomum camphora leaves by solvent-free microwave assisted ex-
traction (Liu et al., 2018) or antioxidant polyphenols from fresh chicory
grounds by ultrasound-assisted extraction (Pradal et al., 2016). The
environmental impact of pollution derived by MHG method was about
112 g CO2 rejected into the atmosphere according to the amount to
extract essential oil from Mentha leaves by MHG technology (Vian et al.,
2008).
3.3. Color features of the aqueous extracts
Visual appearance of the individual fractions collected by MHG was
pale yellow whereas fractions by distillation presented a colorless
5
Industrial Crops & Products 145 (2020) 112079
attribute. Color coordinates and magnitudes by the CIEL*a*b* method
of these samples is exhibited in Table 1. Slight differences in the mac-
roscopic shape were showed since the range of the different parameters
was limited, namely lightness, a* and b* by MHG fluctuated on the
range from 88.25–89.19, from 1.36 to 1.65 and from -3.27 to -2.50,
respectively; these values from liquid extracts by distillation varied in
from 88.36–89.22, from 1.65 to 1.74 and from -3.80 to -2.61, respec-
tively. In relation to the magnitudes, the highest difference between
these two extraction methodologies was described for the hue angle of
the fraction samples with around 4 units. Chroma and saturation were
similar with an average of 3.64 and 0.04, respectively.
Color measurements of the set of fractions of MHG extraction pro-
cess at 50 W is displayed in Table 2. This irradiation power was selected
as optimum extraction conditions since it provided the highest volume
of recovered water with the lowest energy consumption and environ-
mental impact of by microwave treatment. Their color data was com-
pared with the values derived by the set of fractions by distillation
method. MHG coordinates were slightly lower than distillation out-
comes: the highest difference was detected at b* with close to 1 unit.
The magnitudes presented a similar pattern to the individual fractions
above mentioned, with the same hue angle variation and chroma and
saturation issues close with each other. A small difference (ΔE* < 1.5)
were stablished between 50 W and distillation process according to the
classification of the total color difference of Adekunte et al. (2010). The
hue difference was also reduced (ΔH* = 0.20) therefore these two ex-
traction procedures offered similar color features.
3.4. Total phenolic content and antioxidant capacity
The effect of the MHG and distillation extraction technologies from
E. australis flowers on the bioactive profile of collected fractions is
presented in Fig. 3. In general, the concentration of bioactive com-
pounds showed an increase tendency at the same time that the ex-
traction processes occurred. This phenomenon could be associated with
the enhance of the bioaccessibility of phenolic and antioxidant com-
pounds by their thermal degradation in the end of the practice. A si-
milar increase was reported by Vodnar et al. (2017) with peels and pulp
fruit and vegetable samples processed at 80 °C during 10 min. Despite
this rise was noticeable, the used microwave irradiation power was
higher (e.g. total phenolic compound at 200 W provided an average of
0.07 ± 0.01 mg GAE/g flower dry weight), though it was necessary
took in consideration that the total volume of gathered aqueous extracts
was reduced considerately in these work conditions. This same trend
was observed for the ABTS diammonium salt radical cation scavenging
capacity. In this case, the fraction with highest antioxidant capacity was
the latest of the microwave treatment at 100 W (0.181 ± 0.000 mg
Trolox eq/g flower dry weight). Fractions from distillation method
supplied a comparable tendency especially in the total phenolic content
with a maximum value of 0.27 ± 0.00 mg GAE/g flower dry weight.
Chemical characterization comparison of the set of fractions of MHG
at 50 W and distillation techniques is given in Table 3. A significant
difference between the total solid extraction yield of these extraction
procedures was identified; concentration by conventional system was
around 2 times higher than the microwave process. The opposite rela-
tion was described by the total phenolic content since MHG extraction
method offered the highest concentration. These data were significantly
higher than the outcomes from dried aerial parts of Erica carnea L.
submitted to Soxhlet extraction, maceration, ultrasound assisted ex-
traction, microwave-assisted extraction and subcritical water extraction
(Veličković et al., 2017). Regarding to the antioxidant capacity, TEAC
and FRAP assays described slightly higher values contrasting with the
outcomes by distillation. Ascorbic acid and Fe(II) sulphate heptahy-
drate exhibited a stronger positive correlation with total phenolic
content (r = 0.939 and r = 0.943, respectively). The values of the ef-
fective concentration at which 50 % of DPPH radical was scavenged
(EC50) were close to each other with an overage around 0.720 g/L
L. López-Hortas, et al. Industrial Crops & Products 145 (2020) 112079

Table 1
Colorimetric features by CIEL*a*b* system from the collected fractions of the aqueous phase of defrosted E. australis flowers at different microwave irradiation power
by MHG technique. Values of the color coordinates and magnitudes of the aqueous phase obtained by distillation were also summarized for comparative purposes.
Coordinates Magnitudes

Extraction technique Irradiation power Fraction Lightness a* b* Hue angle Chroma Saturation
(L*) (hº) (C*) (S*)

MHG 25 W 1 89.19 ± 0.11a 1.58 ± 0.02a −3.00 ± 0.10a 117.77 ± 0.23d 3.39 ± 0.05b 0.04 ± 0.01a
2 89.14 ± 0.02a 1.59 ± 0.02a −3.01 ± 0.02a 117.82 ± 0.24d 3.41 ± 0.04b 0.04 ± 0.01a
3 88.96 ± 0.25a 1.57 ± 0.05a −2.98 ± 0.03a 117.78 ± 0.19d 3.37 ± 0.04b 0.04 ± 0.01a
4 88.95 ± 0.04a 1.64 ± 0.03a −3.09 ± 0.05a 117.91 ± 0.25d 3.50 ± 0.05a 0.04 ± 0.01a
5 88.97 ± 0.19a 1.62 ± 0.07a −2.98 ± 0.08a 118.53 ± 0.32c 3.39 ± 0.06b 0.04 ± 0.01a
6 88.86 ± 0.05a 1.64 ± 0.02a −3.27 ± 0.02a 116.68 ± 0.12e 3.66 ± 0.05a 0.04 ± 0.01a
7 89.13 ± 0.04a 1.59 ± 0.05a −3.10 ± 0.10a 117.20 ± 0.15d 3.49 ± 0.08a,b 0.04 ± 0.01a
8 88.95 ± 0.11a 1.65 ± 0.01a −3.24 ± 0.06a 116.99 ± 0.13e 3.64 ± 0.05a 0.04 ± 0.01a
9 89.08 ± 0.08a 1.64 ± 0.02a −3.21 ± 0.09a 117.06 ± 0.20d 3.60 ± 0.05a 0.04 ± 0.01a
50 W 1 88.25 ± 0.09b 1.45 ± 0.07b −2.68 ± 0.08b 118.44 ± .023c 3.05 ± 0.06d 0.03 ± 0.01a
2 88.73 ± 0.10b 1.44 ± 0.05b −2.63 ± 0.08b 118.76 ± 0.23c 3.00 ± 0.04d 0.03 ± 0.01a
3 88.25 ± 0.10b 1.36 ± 0.06b −2.69 ± 0.09b 116.76 ± 0.14e 3.01 ± 0.05d 0.03 ± 0.01a
4 88.63 ± 0.05b 1.41 ± 0.02b −2.71 ± 0.03b 117.49 ± 0.32d 3.05 ± 0.03d 0.03 ± 0.01a
5 88.65 ± 0.16b 1.38 ± 0.09b −2.67 ± 0.14b 117.30 ± 0.21d 3.00 ± 0.05d 0.03 ± 0.01a
6 88.56 ± 0.11b 1.43 ± 0.04b −2.64 ± 0.07b 118.42 ± 0.23c 3.00 ± 0.04d 0.03 ± 0.01a
7 88.33 ± 0.14b 1.38 ± 0.05b −2.62 ± 0.09b 117.75 ± 0.24d 2.96 ± 0.03d 0.03 ± 0.01a
8 88.83 ± 0.11b 1.43 ± 0.06b −2.75 ± 0.08b 117.49 ± 0.20d 3.09 ± 0.05c,d 0.03 ± 0.01a
9 88.81 ± 0.07b 1.46 ± 0.03a −2.77 ± 0.06b 117.83 ± 0.19d 3.13 ± 0.06c,d 0.04 ± 0.01a
10 88.92 ± 0.13b 1.56 ± 0.04a −2.74 ± 0.03b 119.63 ± 0.21b 3.15 ± 0.05c,d 0.04 ± 0.01a
100 W 1 88.77 ± 0.07b 1.55 ± 0.03a −2.84 ± 0.03b 118.56 ± 0.22c 3.24 ± 0.05c 0.04 ± 0.01a
2 88.58 ± 0.06b 1.51 ± 0.04a −2.69 ± 0.03b 119.33 ± 0.24b 3.08 ± 0.05d 0.03 ± 0.01a
3 88.78 ± 0.13b 1.57 ± 0.05a −2.86 ± 0.04b 118.65 ± 0.23c 3.26 ± 0.06c 0.04 ± 0.01a
4 88.47 ± 0.09b 1.56 ± 0.01a −2.87 ± 0.06b 118.50 ± 0.15c 3.27 ± 0.05c 0.04 ± 0.01a
5 88.86 ± 0.02b 1.52 ± 0.05a −2.83 ± 0.07b 118.29 ± 0.17c 3.21 ± 0.05c 0.04 ± 0.01a
6 88.47 ± 0.12b 1.53 ± 0.05a −2.83 ± 0.05b 118.39 ± 0.15c 3.21 ± 0.05c 0.04 ± 0.01a
7 88.80 ± 0.22b 1.52 ± 0.06a −2.83 ± 0.07b 118.24 ± 0.19c 3.21 ± 0.04c 0.04 ± 0.01a
8 88.79 ± 0.06b 1.58 ± 0.02a −2.73 ± 0.07b 120.07 ± 0.13a 3.15 ± 0.05c,d 0.04 ± 0.01a
9 88.99 ± 0.16b 1.55 ± 0.05a −2.98 ± 0.01a 117.48 ± 0.19d 3.36 ± 0.03c 0.04 ± 0.01a

Coordinates Magnitudes

Extraction technique Irradiation power Fraction Lightness a* b* Hue angle Chroma Saturation
(L*) (hº) (C*) (S*)

MHG 150 W 1 88.53 ± 0.04b 1.47 ± 0.02b −2.63 ± 0.05c 119.16 ± 0.13c 3.01 ± 0.03b 0.03 ± 0.01a
2 88.61 ± 0.16b 1.46 ± 0.03b −2.66 ± 0.04c 118.71 ± 0.16c 3.03 ± 0.04b 0.03 ± 0.01a
3 88.69 ± 0.07b 1.51 ± 0.04b −2.65 ± 0.06c 119.74 ± 0.21c 3.05 ± 0.02b 0.03 ± 0.01a
4 88.87 ± 0.18a,b 1.49 ± 0.03b −2.67 ± 0.06c 119.21 ± 0.18c 3.05 ± 0.03b 0.03 ± 0.01a
5 88.86 ± 0.06a,b 1.49 ± 0.05b −2.68 ± 0.04c 119.01 ± 0.19c 3.06 ± 0.04b 0.03 ± 0.01a
6 88.53 ± 0.10b 1.49 ± 0.05b −2.66 ± 0.06c 119.29 ± 0.23c 3.05 ± 0.04b 0.03 ± 0.01a
7 88.61 ± 0.08b 1.51 ± 0.03b −2.57 ± 0.07c 120.49 ± 0.22b 2.98 ± 0.03b 0.03 ± 0.01a
8 88.66 ± 0.10b 1.50 ± 0.03b −2.63 ± 0.06c 119.73 ± 0.25c 3.03 ± 0.02b 0.03 ± 0.01a
200 W 1 88.75 ± 0.22a,b 1.53 ± 0.03b −2.50 ± 0.07c 121.41 ± 0.23a 2.93 ± 0.04b 0.03 ± 0.01a
2 88.87 ± 0.15a,b 1.53 ± 0.02b −2.50 ± 0.05c 121.52 ± 0.25a 2.93 ± 0.04b 0.03 ± 0.01a
3 88.46 ± 0.06a,b 1.53 ± 0.03b −2.55 ± 0.07c 120.96 ± 0.20a 2.97 ± 0.03b 0.03 ± 0.01a
4 88.76 ± 0.08a 1.55 ± 0.05b −2.63 ± 0.02c 120.43 ± 0.22b 3.05 ± 0.02b 0.03 ± 0.01a
5 88.82 ± 0.06a 1.58 ± 0.02b −2.97 ± 0.03b 118.06 ± 0.20d 3.37 ± 0.05b 0.04 ± 0.01a
Distillation 1 88.98 ± 0.11a 1.72 ± 0.06a −3.69 ± 0.06a 114.99 ± 0.32e 4.07 ± 0.03a 0.05 ± 0.01a
2 89.22 ± 0.00a 1.74 ± 0.04a −3.74 ± 0.08a 114.95 ± 0.23e 4.12 ± 0.04a 0.05 ± 0.01a
3 88.61 ± 0.01b 1.72 ± 0.07a −3.77 ± 0.04a 114.59 ± 0.22e 4.14 ± 0.04a 0.05 ± 0.01a
4 89.13 ± 0.06a 1.71 ± 0.02a −3.67 ± 0.02a 114.98 ± 0.25e 4.05 ± 0.03a 0.05 ± 0.01a
5 89.21 ± 0.11a 1.72 ± 0.03a −3.74 ± 0.05a 114.74 ± 0.24e 4.12 ± 0.03a 0.05 ± 0.01a
6 89.16 ± 0.17a 1.73 ± 0.03a −3.80 ± 0.05a 114.50 ± 0.21e 4.17 ± 0.03a 0.05 ± 0.01a
7 88.60 ± 0.05b 1.74 ± 0.04a −3.73 ± 0.02a 115.00 ± 0.20e 4.11 ± 0.05a 0.05 ± 0.01a
8 88.36 ± 0.14b 1.65 ± 0.08a −3.61 ± 0.08a 114.50 ± 015e 3.97 ± 0.04a 0.04 ± 0.01a

Data are given as mean ± standard deviation. Data values in a column with different superscript letters are statically different (p ≤ 0.05).

(equivalent to 0.19 g BHA/L).
To sum up, MHG technology at 50 W during 130 min provided the
highest volume of liquid extract with a noticeable total phenolic con-
tent and antioxidant capacity in combination with the lowest energy
consumption and environmental impact.
3.5. Microstructural flower tissues changes
Different extraction procedures have a different effect on the cell
walls of the flower tissues (Fig. 4). Microscopic observations permitted
compare the undamaged E. australis samples (Fig. 4a) with the solid
phase obtained at 25 and 200 W by MHG method (Fig. 4b and c). Mi-
crowave heating caused a shrinking effect on the flower tissue which
was accentuated when higher irradiation powers were employed. This
could occur as consequence of the rapid removal of the phyto-
compounds from within the flower tissue. MHG treatment originated
some more pronounced injuries on the cells that distillation system
since the samples derived of this extraction methodology experimented
a slightly increase in their volume as we can see in the Fig. 4d. It could
derive by the steam generated in this traditional process. Similar cell

6
L. López-Hortas, et al.
Table 2
Comparison of the colorimetric features by CIEL*a*b* system from the set of fractions from the aqueous phase of defrosted E. australis flowers obtained at 50 W by
MHG procedure in comparison with the aqueous phase obtained by distillation.
Flowers Coordinates
Lightness a*
(L*)
MHG at 50 W 88.30 ± 0.04a 1.30 ± 0.02b
Distillation 88.94 ± 0.08a 1.56 ± 0.02a
50 W Total color difference (ΔE*)
Distillation
Data are given as mean ± standard deviation. Data values in a column with different superscript letters are statically different (p ≤ 0.05).
transformations were detected in the tissues of flower buds of Lonicera
japonica Thunb. subjected at heat-reflux extraction and ultrahigh
pressure technology (Hu et al., 2015).
3.6. Cosmetic application of E. australis extracts
Based on the antioxidant potential results obtained for the aqueous
extracts from E. australis flowers by MHG and distillation extraction
procedures, MHG was disclosed as the extraction method more suitable.
The selected flower MHG-extract (at 50 W) was used as antioxidant in
the development of a sunscreen cream. For comparative purposes,
aqueous extract from wild U. europaeus flowers by MHG at 100 W for
70 min was also employed in the prepared emulsions (López-Hortas
et al., 2016). Both flower extracts showed an acid pH issue (about 3.4)
and a negligible SPF value (an average of 0.18). The elaborated
sunscreen creams presented a SPF data approximately of 5.8.
Distilled water and three thermal waters from different spring wa-
ters were used in these cosmetic formulations. Their pH values varied
around 5.5 to the distilled water whereas the thermal waters changed
Industrial Crops & Products 145 (2020) 112079
Magnitudes
b* Hue angle Chroma Saturation
(hº) (C*) (S*)
−2.27 ± 0.04a 119.79 ± 0.56b 2.61 ± 0.05b 0.03 ± 0.01a
−3.20 ± 0.04a 116.04 ± 0.68a 3.56 ± 0.08a 0.04 ± 0.01a
Hue difference (ΔH*)
1.16 Distillation 0.20
over the range 7.4 - 7.6. These thermal waters exhibited an electrical
conductivity ranges between 1260–3200 μS/cm in contrast with the
reduced outcomes presented for the applied distilled water (round
about 12 μS/cm). These differences were not significant in relation to
their total solid content that it was about 0.10 - 0.15 mg dry residue/mL
water: the thermal water number 1 was the only thermal water that
exceed this parameter roughly 4 times (approximately 0.45 mg dry
residue/mL water). On the other hand, the color characterization of the
distinct employed waters was found to be the same in all cases: the
color coordinates values were L* = 89.56, a* = -4.24 and b * = 3.64.
The sunscreen creams presented a creamy oily aspect with visual
white color and any visible skin irritation or erythema were observed.
To know the acceptance by consumers, a Principal Component Analysis
was applied to the intensities of all sensory attributes. The main var-
iance was explained by the first two factors which accounted for 84.06
% of the variability (72.61 % and 11.45 %, respectively). MHG-extracts
of E. australis presented a floral, bee pollen and ripe fruity aromas, and
U. europaeus smelled like yellow flowers and with myrtle aromatic
nuances, but probably citric aroma of bergamot oil added to the O/W
Fig. 3. Total phenolic content (a) and TEAC
value (b) from the collected fractions of de-
frosted E. australis flowers obtained by MHG
procedure in different working conditions in
comparison with the collected fractions ob-
tained by distillation. Note here that the
numbers from 1 to 10 in x-axes represent the
individual collected fractions. nd: no detected.
7
L. López-Hortas, et al. Industrial Crops & Products 145 (2020) 112079

Table 3 feeling is clear and located in the positive part of Factor 1 and in the
Characterization of the aqueous phase collected from defrosted E. australis negative part of Factor 2. All volunteers considered that the thermal
flowers obtained at 50 W by MHG procedure in comparison with the aqueous water used in the elaboration of the formulations had a significance
phase obtained by distillation. prominence and they were preferred in comparison with the distilled
Chemical properties Extraction technique water, confirmed by Hierarchical Cluster analysis (Figure S3). The sun
cream formulated with E. australis and thermal water number 3 re-
MHG at 50 W Distillation ceived the maximum score, more than 0.7 and 0.3 points of difference
Total solid extraction yield 0.799 ± 0.070 b
1.480 ± 0.000a
with respect to the control sample (without any added extracts and with
(mg extract /g flower dry weight) distilled water) or the creams with U. europeaus, respectively; this last
Total phenolic content 0.090 ± 0.000a 0.047 ± 0.010b formulation presented similar scores with the three thermal waters, but
(mg GAE /g flower dry weight) higher than with distilled water. This preference was also observed in
TEAC (mg Trolox eq /g flower dry weight) 0.267 ± 0.000a 0.244 ± 0.010b
other studies (del Castillo et al., 2016; Balboa et al., 2017).
FRAP (mg ascorbic acid/g flower dry 0.005 ± 0.000a 0.001 ± 0.000b
weight) The total solid content of the made sunscreen creams is displayed in
(mg FeSO4 * 7 H2O/g flower dry 0.039 ± 0.000a 0.017 ± 0.000b Fig. 5. As we can see, the values hardly changed. The minimum and
weight) maximum data were about 0.30–0.35 g dry residue/g sun cream, re-
DPPH EC50 (g/L) 0.686 ± 0.030b 0.748 ± 0.050a
spectively. Thermal water 3 displayed outcomes with significant dif-
ference between the two flower MHG extracts. The total solid content of
Data are given as mean ± standard deviation. Data values in a raw with dif-
ferent superscript letters are statically different (p ≤ 0.05). the studied sun creams experimented a minor reduction (around 0.05
TEAC: Trolox Equivalent Antioxidant Capacity. units) after the accelerated oxidation test during 15 days (data not
FRAP: Ferric Reducing Antioxidant Power. shown). This circumstance was also validated with the color measure-
DPPH: α,α-diphenyl-β-picrylhydrazyl. ments at 0 and 15 days. In this case, U. europaeus sunscreen creams
EC50: Effective concentration at which 50 % of DPPH radical was scavenged. carried out the maximum total color difference (ΔE* = 3.80) at 0 days,
classified as very distinct (ΔE* > 3.0), according with the classification
emulsions has been able to mask these aromas because, according to the reported by Adekunte et al. (2010), in relation to the control cosmetic
loading plot (Figure S2), the first factor separated the variables related formulation elaborated with the thermal water 2 and without added
with the smell of the creams or after application to the skin (intensity antioxidant extracts. The remaining samples offered small differences
and preference) which do not appear play an important role for con- (ΔE* < 1.5) when compared to the corresponding control cosmetics.
sumer preference. The interrelationships among the overall preference The total color difference of the creams after accelerated oxidation
of the sun creams and the scores of texture (visual and applied to the assay at 15 days disclosed that U. europaeus extract kept the maximum
skin), spreadability, softness, good skin penetration ability and skin value of total color difference (ΔE* = 1.99), in this case with the

Fig. 4. Microscopic structure of E. australis flowers for defrosted samples (a), the solid phase obtained during MHG at the limits of the range of the different
irradiation powers employed [25 W (b) and 200 W (c)] and after steam distillation without cohobation (d).

8
L. López-Hortas, et al.
cosmetic formulated with the thermal water 3. A very distinct differ-
ence was also presented by the samples elaborated with the thermal
water 2 in combination with the commercial antioxidant BHT and
( ± )-α-tocopherol (an average of ΔE* = 1.72).
The effect of the accelerated oxidation work conditions under
50 ± 2 °C during 15 days in the pH values of the samples of the
sunscreens creams is compiled in the Figure S4. In all cases, the pH of
formulated creams varied in a restricted range between 5.7 and 6.2.
These data were in accordance with the pH results of stability de-
terminations of sunscreen cream containing starch sponges (Bhuptani
and Patravale, 2019). However, distilled water creams showed slightly
lower pH data (an average of 5.6). These data are in well agreement
with the normal skin pH (Dong et al., 2019). Overall, pH measurements
were constant over time despite these small differences so the emulsion
stability was continuous on accelerated testing. The formation of the
final chemical compounds of representative lipid oxidation values from
TBARS profiles during the accelerated oxidation to which the different
creams were subjected appears in Fig. 6. The malonaldehyde values
oscillated around 14.7 units: U. europaeus creams displayed the lowest
TBARS outcomes. This same trend was recorded in the thermal water
products, since their TBARS parameter oscillated between roughly 12.3
and 23.8 nmol malonaldehyde/g sun cream dry weight. The range
provided by the distilled water O/W emulsions was slightly larger
9
Industrial Crops & Products 145 (2020) 112079
Fig. 5. Total solid content of the sun cream
formulated with selected MHG extracts from E.
australis flowers (bars with vertical lines) and
U. europaeus (grey bars) and flowers with dif-
ferent thermal waters. For comparative pur-
pose, data of sun cream formulated with BHT
(bars with horizontal lines), ( ± )-α-tocopherol
(dotted bars) and water control (squared bars)
are also shown.
(approximately between 12.0 and 26.7 nmol malonaldehyde/g sun
cream dry weight). The detected lipid peroxidation was practically in-
variant with time, likewise this behavior was indicated for the oxidative
damage on lipids of sunflower oil with essential oil from Coriandrum
sativum (Wang et al., 2018).
Fig. 7 shows the impact of used waters in the flow properties of
enriched sunscreen creams at 25 °C. In all cases, the apparent viscosity
decreased (about 4 decades) with increasing shear rate, displaying
shear-thinning behavior. The observed pseudoplastic behavior is con-
sistent with the tendencies previously found for synthetic sunscreen
creams, with values in the range of several commercial cream products
(Houlden, 2017). For creams formulated with U. europaeus extracts
(Fig. 7a), no notably differences were observed between the flow curves
independently of the used water. In contrast, for those prepared with E.
australis extracts (Fig. 7b), lower apparent viscosity values at the same
shear rate were identified over the range of tested shear rates for the
thermal water 3. This behavior indicates that the water of this thermal
spring lead to creams easier to extend across large body surface areas
(Houlden, 2018), corroborated by the sensory panel, because this cream
achieved the highest scores in spreadability, penetration, softness, skin
feel and texture preference. No relevant differences were observed for
the other systems. Comparing creams formulated with both extracts,
those made with E. australis extracts featured slighted lower apparent
Fig. 6. Evolution of thiobarbituric acid re-
active substances (TBARS) during accelerated
oxidation determination of the sun cream for-
mulated with selected MHG extracts from E.
australis (grey bars) and U. europaeus (bars with
vertical lines) flowers with a) distilled water,
b) thermal water 1, c) thermal water 2 and d)
thermal water 3. For comparative purpose,
data of sun cream formulated with BHT (bars
with horizontal lines), ( ± )-α-tocopherol
(dotted bars) and water control (squared bars)
are also shown.
L. López-Hortas, et al.
Fig. 7. Viscous behavior of the sun cream formulated with selected MHG extracts from a) U. europaeus and b) E. australis flowers and c) BHT, d) ( ± )-α-tocopherol
and e) water control with distilled water (blue), thermal water 1 (red), thermal water 2 (green) and thermal water 3 (purple).
viscosity values (mainly at the lowest shear rates). This suggests that
the creams formulated E. australis extracts will have an initial easier
application to the skin (Houlden, 2018). Note here that those creams
prepared using BHT and ( ± )-α-tocopherol (Fig. 7c and d) exhibited
similar profiles and magnitudes, whereas those prepared with the water
control featured slightly higher values which is consistent with the
absence of bioactive fractions (Nooeaid et al., 2017). It should be
highlighted that no hysteresis phenomenon was identified in tested
sunscreen creams, with the consequent advantage from the industrial
point of view.
4. Conclusions
To conclude, MHG technology allowed obtaining adequate amount
of bioactive extracts from E. australis, selecting 50 W as the most sui-
table operation conditions to recover bioactives, save time and energy,
with the consequent reduction of the generated environmental impact,
when compared with conventional distillation. Both extraction proce-
dures did not notably affect the color of the extracted liquors. The in-
corporation of E. australis or U. europaeus MHG extract in sunscreen
cream models with different thermal waters led to cosmetics with si-
milar properties and with comparable features to their counterparts
made with commercial antioxidants. Furthermore, the use of waters
from thermal springs favours the acceptance by consumers. The best
sun cream formulations in terms of mechanical properties were
achieved with thermal water 3 which favored skin cream application,
and sensorially was significantly selected as preferred cream. Further
studies on the identification of the phytochemical extract compounds as
well as the action mechanism of the antioxidants compounds on the
skin after their topical application should be relevant. Overall, the use
of underused flowers could be an attractive alternative to prepare
natural cosmetics with improve properties to the synthetic ones.
Author contributions
E.F. and H.D. conceived and planned the experiments. L.L.H, E.C.
and M.D.T. participated in samples preparation and analysis. L.L.H. and
M.D.T. performed the data analysis, interpretation of the results, and
10
Industrial Crops & Products 145 (2020) 112079
wrote the paper draft. E.F., H.D. and M.D.T. supervised the research
work, contributed to the discussion of the data and revised the manu-
script.
Declaration of Competing Interest
The authors declare that they have no conflict of interest.
Acknowledgements
The authors are grateful to the Ministry of Economy and
Competitiveness of Spain (CTM2015-68503-R) and FEDER for the fi-
nancial support. L. López-Hortas thanks the Xunta de Galicia for her
pre-doctoral grant (2014/2020 European Social Fund). M.D. Torres
acknowledges the Ministry of Economy, Industry and Competitiveness
for her post-doctoral grant (IJCI-2016-27535).
Appendix A. Supplementary data
Supplementary material related to this article can be found, in the
online version, at doi:https://doi.org/10.1016/j.indcrop.2019.112079.
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