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4 1 Colombian mango processing by-product (Mangifera indica L.): Proximate
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7 2 composition, green extraction of carotenoids, and their application as an antioxidant
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9 3 additive for edible oils
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15 5 Andrea del Pilar Sánchez-Camargo1,2*, Luis-Felipe Gutierrez2, Sandra Milena Vargas1,
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6 Hugo A. Martinez-Correa3, Fabián Parada-Alfonso1, Carlos-Eduardo Narváez-Cuenca1
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8 Food Chemistry research group, Departamento de Química, Facultad de Ciencias
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26 9 Universidad Nacional de Colombia, Bogotá, Colombia, Carrera 30 No. 45-03, Bogotá D.C.,
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28 10 111321, Colombia
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11 Instituto de Ciencia y Tecnología de Alimentos, Universidad Nacional de Colombia Sede
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34 12 Bogotá, Carrera 30 # 45-03, Edificio 500A, Bogotá, DC, Colombia, 111321., Colombia.
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37 13 Department of Engineering, Universidad Nacional de Colombia, Carrera 32 No. 12-00,
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39 14 Palmira, Colombia
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42 15
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45 16 *Corresponding author:
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48 17 Dr. Andrea del Pilar Sánchez-Camargo, Food Science research group, Departamento de
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18 Química, Facultad de Ciencias Universidad Nacional de Colombia, Carrera 30 #45-03,
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53 19 Bogotá D.C., 111321, Colombia, e-mail: adsanchezc@unal.edu.co, Tel.: +57 1 3165000.
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55 20 Ext. 14480; fax: + 57 1 3165220
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58 21 Submitted to: Food Research International
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4 22 1. INTRODUCTION
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7 23 Nowadays, sustainable development is becoming an important issue in the government
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10 24 entities agenda due to effects on social, environmental, and economic progress (Otles and
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12 25 Kartal, 2018). The current worldwide linear economic model of ‘Take-Make-Consume-
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26 Dispose’ has promote massive amounts of waste to be disposed. In this sense, the concept of
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17 27 sustainability is now based on a circular economy model, which is focused on resource
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19 28 efficiency, waste reduction, recycling, and valorisation (Imbert, 2017). Bio-economy, a fast-
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22 29 growing sector, is one of the most strongly segment linked to the circular economy, which
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24 30 includes a variety of production activities such as agriculture, forestry, food, pulp and paper
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27 31 production, biotechnological and energy industries, among many others (Imbert, 2017).
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29 32 According to the European commission, food waste is ‘a key area in the circular economy’
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32 33 (European Comission, 2017), therefore its valorisation is considered a great alternative to
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34 34 converting waste into valuable bio-based products or bio-based industries (Otles and Kartal,
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35 2018). Some valorisation strategies for a sustainable and efficient waste management
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39 36 approach for the food industry includes a) animal feed and fertilizer supply, b) composting,
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41 37 c) thermal and electric energy (e.g. through anaerobic digestion), d) fermentation, e)
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44 38 chemical conversion (e.g. biofuel production), and more recently f) extraction of high-value
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46 39 functional compounds (Otles and Kartal, 2018).
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49 40 Fruit process industry produce large amounts of waste (mainly peels, seeds,
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51 41 pomace, and kernels) that can be good sources of potentially valuable bioactive compounds
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42 (Trigo et al., 2019). Mango (Mangifera indica L.) is one of the most important tropical
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56 43 fruits in the world in terms of production and consumer acceptance (Ruales et al., 2018).
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58 44 Colombia produced about 262,000 metric tons of mango in 2016 (AGRONET, 2019).
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4 45 Mango var. Sugar, one of the main cultivars, is highly demanded for local pulp and juice-
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7 46 manufacturing industries, due to its sugar content, flavour, and texture characteristics
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9 47 (Salgado Buelvas et al., 2017). During the industrial processing of mango, the peel
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12 48 represents about 15-20% of the fresh fruit, becoming a source of pollution without any
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14 49 sustainable disposal (Serna-Cock et al., 2016). Studies have reported the phytochemical
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50 profile of mango peel, which includes pectin, phenolic compounds, carotenoids (mainly all
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19 51 trans--carotene), and vitamins with different health benefits and techno-functional
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52 properties (Adilah et al., 2018; Baddi et al., 2015; Gourgue et al., 1992; Larrauri et al., 1996;
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24 53 Rojas et al., 2018). Recently, the extraction of compounds of the carotenoids family from
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26 54 agro industrial by-products, have received great attention due to their provitamin A activity
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29 55 and antioxidant properties (Meléndez-Martínez et al., 2017). For instance, all trans--
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56 carotene, -tocopherol, and lycopene have demostrated be able to protect edible oils from
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34 57 lipid oxidation, becomig therefore an alternative to the harmful synthetic antioxidants
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36 58 TBHQ, BHA, and BHT (Henry et al., 1998; Kaur et al., 2015; Kiokias and Gordon, 2004;
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39 59 Zeb, 2011). According to De Andrade Lima, Kestekoglou, Charalampopoulos, &
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41 60 Chatzifragkou (2019), in 2014, 24% of the global carotenoid production derived from agro
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44 61 industrial sources.
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46 62 When considering agro-industrial by-products as source of bioactive compounds,
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49 63 green extraction techniques are of interest. Among green extraction technologies,
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51 64 supercritical fluid extraction (SFE) has been recognized due to the numerous successful
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65 applications on the extraction of carotenoids from a wide range of fruit pulp and by-products
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56 66 matrices including persimmon (Zaghdoudi et al., 2016), passion fruit (Viganó et al., 2016),
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58 67 peach (Espinosa-Pardo et al., 2014), watermelon (Vaughn Katherine et al., 2008), apricot
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 1
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4 68 pomace (Şanal et al., 2005), and banana (Comim et al., 2010), as well as fruits from the
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7 69 Amazon rainforest, such as pitanga and buriti (Ferreira de França et al., 2002; Filho et al.,
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9 70 2008). Garcia-Mendoza, Paula, Paviani, Cabral, & Martinez-Correa (2015) explored the
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12 71 extraction of bioactive compounds from mango peel by two sequential extraction steps:
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14 72 supercritical CO2 extraction (ScCO2), followed by pressurized ethanol (PE) from the residue
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73 of the first stage. Results demonstrated that total carotenoids content is dependent on the
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19 74 extraction startegy, being higher for ScCO2 (5.60 ± 0.51 mg -carotene equivalent g-1
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75 extract) in contrast to PE (0.35 ± 0.035 mg β-carotene equivalent g-1 extract). To the best of
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24 76 our knowlegde, however, there have not been studies on the proximate and bioactive
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26 77 compounds composition, the optimization of extraction of carotenoids from mango peel var.
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29 78 Sugar by using ScCO2, and the use of such extracts to protect edible oils from lipid
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31 79 oxidation.For the fist time, therefore, the present study propossed: a) to determine the
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34 80 proximate composition, fatty acids profile, and total phenolic content of mango peel var.
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36 81 Sugar, b) to assess the effect of drying method towards the carotenoids profile c) to study
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82 the influence of the pressure, temperature, and co-solvent content on the extraction yield,
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41 83 carotenoid extraction yield, and total carotenoids content in the extracts using SFE, d) to
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43 84 evaluate the carotenoids profile in the SFE optimal extract, and e) to evaluate the effects of
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46 85 an optimal SFE mango peel carotenoids extract towards the oxidative stability of a bulk
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48 86 sunflower oil and rank it against pure all trans-β-carotene.
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51 87
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54 88 2. Materials and methods
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56 89 2.1. Materials
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4 90 Mango (Mangifera indica L.) peel var. Sugar samples were obtained as by-product from a
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7 91 local processing industry (Fast Fruit Ltda., Bogotá, Colombia). Carbon dioxide, 99.5 (g/100
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9 92 g) (Linde S.A., Bogotá, Colombia), absolute ethanol, and acetone (Merck, Colombia) were
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12 93 employed as solvents. A kit of enzymes (-Amylase, protease, and amyloglucosidase) used
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14 94 for the assay of dietary fiber, all trans--carotene (Type I ≥93%), and fatty acid methyl
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17 95 esters (Mix C4-C24) were purchased from Sigma Aldrich (St. Louis; MO, USA). For the
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19 96 determination of total fat and protein assays, analytical grade reagents (Merck, Germany)
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22 97 were used. Refined, bleached, and deodorized (RBD) sunflower oil, without antioxidants,
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24 98 was supplied by Team Foods (Bogotá, Colombia). Ultrapure water was produced by using
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99 a Milli-Q system (Millipore, USA). Solvents used for reversed phase (RP)-ultrahigh
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29 100 performance liquid chromatography (UHPLC) analysis were of HPLC grade.
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32 101 2.2. Chemical characterization of mango peel
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35 102 Chemical caracterization was performed in an air dried sample, except for moisture that
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37 103 was evaluated in a fresh sample as well. This characterization consisted on a proximate
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40 104 analysis according to the AOAC (2006) methods and on a evaluation of the total soluble
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42 105 phenols content (TPC). Moisture in both raw and dry by-product was quantified by oven-
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45 106 drying at 105 °C (AOAC 950.46), total fat by the Soxhlet method with n-hexane (AOAC
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47 107 991.36), crude protein using the microKjeldahl procedure (AOAC 960.52), crude ash by
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108 incineration in a muffle furnace at 550 °C (AOAC 942.05), and total dietary fiber by the
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52 109 enzymatic-gravimetric method (AOAC 985.29). In addition, fatty acids composition of the
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54 110 Soxhlet extract was determined by gas chromatrography with a flame ionization detector
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57 111 (FID), following the alkaline methylation method as described by Gutiérrez, Quiñones-
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59 112 Segura, Sanchez-Reinoso, Díaz, & Abril (2017). The derivatized fatty acids were identified
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4 113 by comparing their retention times with those of authentic fatty acid methyl esters standards
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7 114 under the same conditions and quantified by calculating the relative area. For TPC, the
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9 115 extraction method described by Blancas-Benitez et al., (2015) was carried out. Briefly, a
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12 116 sequential extraction using an acidified methanol (0.8% HCl 2 N)-water solution (50:50%,
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14 117 v/v), followed by a acetone-water solution (80:20%, v/v) was performed. After
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118 centrifugation (3,500 rpm; 10 min; and 15 ºC), both supernatant extracts were combined
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19 119 together. TPC content was determined in the combined extract, following the Folin-
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21 120 Ciocalteu method as defined by Singleton, Orthofer, & Lamuela-Raventós (1999) with
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24 121 some modifications. The result was expressed as mg gallic acid equivalents (GAE) g-1 of
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26 122 sample dry weight. Proximate analysis, fatty acid composition, and TPC were performed in
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29 123 triplicate.
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32 124 2.3. Effect of drying method towards carotenoids content
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35 125 To study the effect of the drying method on the extraction process, the mango peel sample
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37 126 was dryed not only by convective air flow (CMP), but also by freeze-drying (FMP). In the
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127 CMP strategy the sample was dried by convective air flow at 50 ºC for 24 h in a
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42 128 dehydrating oven. In FMP, sample was frozen at -80 °C during 24 h and freeze dried at -35
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44 129 °C and 4.00 Pa during 48 h (Labconco Freezone, Kansas, MO, USA). The dried samples
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47 130 (CMP and FMP) were ground in an electric knife mill and then separated according to
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49 131 particle size, using vibrating sieves from 30 to 200 mesh (0.6 mm < di < 0.075 mm) of the
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52 132 standard Tyler series. A mean diameter dmg of 0.28 mm was calculated by the ASAE
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54 133 S319.3 method (ASAE Standards, 1995). Both types of dried material were stored at -18 °C
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134 in plastic bags sealed in vacuum until the assesment of total carotenoids content (Section
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59 135 2.4.) and the evaluation of the chromatographic profile of individual carotenoids (Section
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4 136 2.5) was completed. Furthermore, CMP sample was used to performing SFE optimization
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7 137 (Section 2.6).
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10 138 2.4. Total carotenoids content by UV-Vis
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13 139 Total carotenoids content was evaluated following the method described by Biswas, Sahoo,
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15 140 & Chatli (2011). CMP and FMP samples were extracted with acetone at 5 °C by vortexing
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141 during 20 min. This procedure was repetead in total four times. After the fourth extraction,
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20 142 the pellet was colorless. Combinated acetone extracts were filtered by Whatmann paper No.
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22 143 42 and the absorbance was read at 450 nm (maximum observed) against a blank (acetone)
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25 144 using an UV-Vis spectrophotometer (Thermo Scientific Genesys 20®, USA). Total
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27 145 carotenoids content was calculated using a calibration curve of all-trans-β-carotene (0.5-
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30 146 50.0 g mL-1). Results were expressed as mg all-trans--carotene equivalent g-1 extract
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32 147 (carotenoid content in the extract) and as mg all- trans--carotene equivalent g-1 dried
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35 148 mango peel (carotenoid extraction yield). All determinations were made in triplicate.
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38 149 2.5. Carotenoids profiling and quantification of -carotene by RP-UHPLC-DAD
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41 150 The profile of carotenoids and the concentration of -carotene were determined by RP-
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43 151 UHPLC using a diode-array detector (DAD), according to a method previously described
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46 152 by Cuéllar-Cepeda et al. (2019). Briefly, carotenoids were extracted with a polar
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48 153 (acetone:methanol 2:1, v/v) and non-polar (n-hexane) mixture from 250 mg of CMP sample
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51 154 and FMP sample. Then, compounds were tentatively identified and quantified by RP-
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53 155 UHPLC-DAD. An AQUITY UPLC C18 column (150 mm × 2.1 mm, 1.7 µm) was used.
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56 156 More details on the chromatographic conditions are despicted in the cited reference.
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58 157 Tentative identification of compounds was based on elution order, UV-Vis spectra, and
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4 158 injection of authentic all-trans-beta-carotene. Cis isomers of β-carotene have been reported
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7 159 in mango peel samples (de Ancos et al., 2018; Yahia et al., 2006). To help identification of
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9 160 such cis isomers, the intensity of the cis peak was calculated as the ratio between the height
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12 161 of the cis peak (AB) near to 340 nm and the height of the middle maximum absorption peak
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14 162 (AII) multiplied by 100 (%AB/AII) as described by Rodriguez-Amaya (2001). Quantification
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163 was based on a calibration curve, with seven different concentrations of all trans--
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19 164 carotene prepared in acetone, ranging from 5 to 100 g mL-1. Such standard solutions were
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22 165 analysed under identical condition in which extracts were run.
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25 166 2.4. Supercritical fluid extraction (SFE) optimization
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28 167 The extractions were carried out using a lab scale SFE homemade instrument as previously
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30 168 described by Gallo-Molina et al. (2019). The extraction unit was eqquiped with a 10 cm3
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169 extraction cell with independient temperature control. A back pressure regulator was used
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35 170 to control the flow and pressure in the extraction unit. For each extraction the scCO2 flow
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37 171 (6.7 g min-1), extraction time (180 min, based on a previous kinetic curve), and CMP
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40 172 sample amount (5.00 g), were kept constant according to preliminary tests (data not
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42 173 shown). Ethanol, as co-solvent, was supplied by a high pressure liquid pump and it was
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45 174 mixed with a CO2 flow before to getting into the extraction cell. The extract was collected
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47 175 in a previously weighed collection bottle, which was wrapped in aluminum foil during and
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176 after extraction to avoid oxidation of the extract components. After extraction was
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52 177 performed, the remanent ethanol was evaporated under vacuum (35 °C, 100 mBar) and the
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54 178 dried extracts were stored at -20 °C until analysis.
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57 179 The effects of temperature (40-60 °C), pressure (25.0-35.0 MPa), and co-solvent
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60 180 concentration (5-15%, w/w) on global extraction yield and total carotenoid content in the
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4 181 extract obtained using scCO2 from CMP sample. For this aim, a Box-Behnken design, with
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7 182 three factors and three central points were developed. The global extraction yield was
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9 183 determined gravimetrically and expressed as g extract 100 g-1 sample. The total carotenoid
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12 184 content was expressed as mg all trans--carotene equivalent g-1 extract (carotenoid content
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14 185 in the extract) and as all trans--carotene equivalent g-1 dried mango peel (carotenoid
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17 186 extraction yield) as described in section 2.4. Table 1 shows the levels of the variables in
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19 187 coded and real units. The experimental design and data analysis were carried out using the
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22 188 response surface methodology with the software STATGRAPHICS® Centurion XV
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24 189 (Version 15.2.06). The effects of the independent variables on the response variables in the
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190 extraction process were evaluated using the pure error, considering a level of confidence of
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29 191 95% for all the response variables. Using this methodology, 2nd order polynomial models
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31 192 were obtained for all the response variables. The adecuacy of the model was evaluated by
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34 193 calculating the percent variation explained by the correlation coefficient (R2) and the F-test
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36 194 from the analysis of variance (ANOVA, including the test of lack-of-fit). The response
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39 195 surfaces of the respective mathematical models (Eq. (1)) were obtained and the
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41 196 significances were accepted at p ≤ 0.05.
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44 197
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47 198
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49 199 Eq. 1
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52 200 where Y is the response, 0 is the constant coefficient, 1, 2, and 3 are the linear
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55 201 coefficients, 11, 22, and 33 are the quadratic coefficients, and 12, 13, and 23 are the
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57 202 linear-by-linear interaction coefficients for the independent variables X1 (Pressure), X2
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60 203 (Temperature), and X3 (Ethanol concentration).
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4 204 Because the obtained optimal conditions of pressure, temperatue, and co-solvent
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7 205 concentration after mathematical modelling did not coincide with any of the experimental
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9 206 assays, such conditions were validated by performing SFE under those optimal parameters.
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12 207 Besides the global extraction yield, the extract of CMP sample was characterized on its
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14 208 total carotenoids content (Section 2.4.) and individual carotenoids by RP-UHPLC-DAD
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209 (Section 2.5.).
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210 2.6. Oxidative estability of a bulk sunflower oil by the Rancimat method
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22 211 Accelerated oxidation test for a bulk RBD sunflower oil was performed by the Rancimat
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25 212 Method, following the method described by Ospina, Montaña-Oviedo, Díaz-Duque,
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27 213 Toloza-Daza, & Narváez-Cuenca (2019). Brielfly, 4.00 g of a bulk RBD sunflower oil (free
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30 214 of added antioxidants or preservatives) were added with either the optimal SFE extract
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32 215 (200, 500, and 1000 mg extract Kg-1 oil, equivalent to 6, 14, and 28 mg β-carotene Kg-1 oil
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35 216 ) or pure all-trans--carotene (6, 14, and 28 mg β-carotene Kg-1 oil). The test was carried
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37 217 out at an airflow of 20 L h-1 and 100 °C. The induction time (ti) of the extracts or pure β-
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40 218 carotene was compared to that oil without antioxidants. The results were expressed as
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42 219 protection factor (tiextract/ticontrol, . tipure β-carotene/ticontrol).
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45 220
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48 221 3. RESULTS AND DISCUSSION
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50 222 3.1. Chemical characterization of mango peel var. Sugar
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53 223 There are several studies about the proximal composition of the mango epicarp exploring
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56 224 varieties such as Keitt, Tommy Atkins, and Hilacha (Serna-Cock et al., 2016), as well as
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58 225 other varieties from countries such as India and Brazil (Ajila, Aalami, Leelavathi, & Rao,
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4 226 2010; Larrauri et al., 1996; Ribeiro, Barbosa, Queiroz, Knödler, & Schieber, 2008).
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7 227 However, there is scarce information about the Sugar variety, which is the most used by the
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9 228 juice-pulp processing industry in Colombia. Results show that mango peel is a good source
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12 229 of dietary nutrients, incluiding dietary fiber, protein, and TPC (Table 2). It is worth noting
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14 230 that total dietary fiber content represents more than one third of the total dry sample weight
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231 (35.62  0.54%). Likewise, there is a ratio of 1:2 between the content of soluble fiber
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19 232 (12.09  0.31%) and insoluble fiber (23.53  0.44%), whose intake is highly recommended
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22 233 for the prevention of cardiovascular and chronic diseases such as obesity, colon cancer,
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24 234 diabetes, and hypercholesterolemia (Ajila et al., 2010; Gourgue et al., 1992). Furthermore,
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27 235 the analysed material showed higher content of crude protein (6.33  0.12%) as compared
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29 236 to the eddible epicarp of other fruits such as apple (2.80 ± 0.17%) (Dibanda Romelle, Rani,
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32 237 & Manohar, 2016), but similar to that of peach (7.51  0.71%) (Yangılar, 2016). The ash
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34 238 content reached a value near to 4%. Despite the composition of ashes was not analyzed,
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37 239 according to other studies, the predominant macro-elements in mango peel are calcium,
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39 240 sodium, magnesium, iron, and zinc (Dibanda Romelle et al., 2016; García-Chacón,
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241 Castaño, & Osorio, 2016; Onuh, Momoh, Egwujeh, & Onuh, 2017). The content of total
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44 242 lipids was low (1.56  0.05%) when compared to the other components. Other studies for
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243 different varieties of mango peel have reported values of fat content around 4-5% (Dibanda
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49 244 Romelle et al., 2016; Mejía Giraldo, Martínez Correa, Betancourt Gutiérrez, & Castrillón
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51 245 Castaño, 2007). The fatty acid profile of the lipid fraction revealed the presence of palmitic
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54 246 (C16:0, 29.8%, mol/mol), palmitoleic (C16:1, 5.9%, mol/mol), stearic (C18:0, 21.4%,
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56 247 mol/mol), oleic (C18:1, 27.5%, mol/mol), and linoleic (C18:2, 15.4%, mol/mol) acids.
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59 248 About the TPC, Serna-Cock et al. reported data for several varietes of mango peel around
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4 249 the world, which vary between 32 and 100 mg GAE g-1 sample. In our case, mango peel
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7 250 var. Sugar showed a TPC of 64.79  0.59 mg GAE g-1 sample, being superior to other
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9 251 Colombian fruit wastes such as papaya (0.57 mg GAE g-1), orange (2.2 mg GAE g-1) and
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12 252 passion fruit (0.69 mg GAE g-1) (Alzate et al., 2017).
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15 253 3.2. Effect of drying method towards carotenoids content
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18 254 The drying method of the mango peel var. Sugar influenced not only the total carotenoids
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20 255 content (Table 3), but also the content of all-trans-β-carotene and its relative abundance
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256 (Figure 1).
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257 When assesing the chromatographic profile of carotenoids in CMP and FMP
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28 258 (Figure 1B and 1C) a different relative abundance of all-trans-b-carotene was observed.
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30 259 Chromatographic peaks with a percentage of area higher than 5% of total area (Peaks 1-3)
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33 260 were tentatively annotated. Peak 1 was annotated as all-trans--carotene (Rt 13.857 min),
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35 261 which was the most abundant compound in the analysed samples. The visible absorption
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38 262 spectra for peaks 2 (Rt 14.127 min) and 3 (Rt 14.630 min) (Supplementary Figure S-1)
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40 263 exhibited a high proportion of %AB/AII. This value was 10% for peak 2 and 48% for peak
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43 264 3. Elution order, together with %AB/AII, and UV-Vis maxima were indicative of peaks 2
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45 265 and 3 being 9-cis--carotene and 13-cis--carotene, respectively. Mercadante, Steck, &
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48 266 Pfander (1999) confirmed the UV-Vis characteristic of these structures by 1H nuclear
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267 magnetic resonance (NMR), C NMR, mass spectrum, and circular dichroism spectrum.
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53 268 The other minor compounds that could not be identified, might include oxygenated
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55 269 compounds such as xanthophylls, which are typically separated in the first minutes of
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270 analysis when employing RP-HPLC (Kobori & Rodriguez Amaya, 2008; Rodriguez-
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60 271 Amaya & Kimura, 2004). In agreement to our results, all-trans--carotene was the
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4 272 main carotenoid reported in hot air-dried Ataulfo mango peel (de Ancos et al., 2018).
5
6
7 273 Ataulfo mango peel also contained other carotenoids, including 9-cis-β-carotene, all-trans-
8
9 274 lutein, 13-cis- β-cryptoxanthin, β-carotene 5,6 epoxide, all-trans-zeaxanthin, 9-cis-
10
11
12 275 zeaxanthin, and 15-cis-β-cryptoxanthin.
13
14
15
276 UV-Vis quantification showed that around 40% of carotenoids compounds were
16
17 277 better preserved by freeze-drying as compared to convectional air flow drying (Table 3).
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19 278 Additionally, RP-UHPLC-DAD revealed that all-trans-β-carotene represented 82 and 74%
20
21
22 279 of the aboundance as compared to the cis isomers for CMP and FMP, respectively. These
23
24 280 results show that freeze-drying was more efficient to avoid degradation of all-trans-β-
25
26
27 281 carotene than convectional air flow drying. However, freeze-drying includes long treatment
28
29 282 times, expensive equipment, and high operational costs, which are difficult to implement as
30
31
32 283 valorization streategy, due to the tons of by-products that have to be treated. These
33
34 284 disadvantages associated to freeze-drying makes hot air-drying more attractive in therms of
35
36
285 its simplicity, speed, and low cost. SFE optimization was, therefore, acomplised with CMP
37
38
39 286 sample.
40
41
42 287 3.3. Effects of pressure, temperature, and co-solvent concentration on global yield
43
44 288 total carotenoid content during scCO2 extraction
45
46
47 289 Table 1 shows the results for the response variables studied in the SFE of carotenoids from
48
49
50 290 mango peel var. Sugar. Response surface methodology was able to provide information
51
52 291 about the importance and statistical significance of individual factors. Based on R2 and the
53
54
55 292 F-test for the regression, among the evaluated responses variables, only carotenoids
56
57 293 extraction yield was highly significant and valid to describe the experimental data. The
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59
60
294 coefficient of determination (R2) of the model for the global extraction yield was 0.70 and
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 1
2
3
4 295 for models the carotenoids concentration in the extract and carotenoids extraction yield
5
6
7 296 were 0.61 and 0.87. Despite the relatively high values found for R2 for either of the three
8
9 297 response variables, the F-test for the lack of fit showed that global extraction yield and
10
11
12 298 concentration of carotenoids in the extract models were not predictive and thus response
13
14 299 surfaces could only be generated with the qualitative and evaluative effects. ANOVA
15
16
300 analysis showed that the ratio between the sum of squares for the pure error and the total
17
18
19 301 sum of squares were small (from 1.63 x 10−3 to 1.35 x 10−2). Those values evidence that the
20
21 302 independent variables studied were under control during the experiments, and that the
22
23
24 303 percentage that the model was not able to explain was not due to operational errors, but to a
25
26 304 lack of fit of the models obtained.
27
28
29 305 The results showed that the global extraction yields varied from 1.602% to 6.249%,
30
31
32 306 being this last one obtained at 30 MPa, 60 °C and 15% w/w ethanol. As it was expected, the
33
34 307 factor with the greatest influence on the extraction yield was ethanol concentration (p =
35
36
308 0.0021) as compared to either pressure (p = 0.0058) or temperature (p = 0.0083) (Figure
37
38
39 309 2a). This behaviour can be explained by the change in the polarity of scCO2 due to the
40
41 310 addition of the co-solvent (positive effect), solubilizing other polar compounds that cannot
42
43
44 311 be extracted exclusively by scCO2. A positive effect was also found for the temperature of
45
46 312 extraction, while an increase in pressure had a negative effect.
47
48
49 313 With respect to the concentration of carotenoids in the extract, the maximum value
50
51
52 314 (62.9 mg all-trans--carotene equivalent g-1 extract) was obtained experimentally at 30.0
53
54 315 MPa, 60 °C, and 5% w/w ethanol, but under such conditions, the lowest global extraction
55
56
57 316 yield was obtained. Of the three factors studied, only two (ethanol concentration and
58
59 317 pressure, see Figure 2b) had significant effects on the concentration of carotenoids in the
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 1
2
3
4 318 extract. On the one hand, an increment on the ethanol concentration promotes a decrease in
5
6
7 319 carotenoid content per gram of extract. It may be because a slight increase in the polarity of
8
9 320 the solvent induces an improvement in the solubility of carotenoids; however, higher
10
11
12 321 concentrations of co-solvent affects the selectivity of the process. On the other hand, the
13
14 322 extraction pressure shows a positive effect on this variable response. An increment on the
15
16
323 pressure promote an increase in fluid density, which might lead to a rapid increase in the
17
18
19 324 solubility of the targeted component (Shi, Mittal, Kim, & Xue, 2007). As reported by Shi et
20
21 325 al. (2007), the solubility of all-trans--carotene in scCO2 is enhanced by an increment of
22
23
24 326 the extraction pressure, and at the same time, by the addition of a co-solvent such ethanol or
25
26 327 vegetable oils. When considering temperature, this factor had the lowest influence on the
27
28
29 328 concentration of carotenoids.
30
31
32 329 When assessing the carotenoids extraction yield, it can be seen that temperature and
33
34 330 once again ethanol concentration in the solvent mixture showed significant effects at the
35
36
37 331 0.05 level (Figure 3a), while the pressure proved not to be an influencing factor. Figure 3b
38
39 332 shows the response surface for the carotenoids extraction yield where the highest extraction
40
41
42 333 yields (>1.8 mg all-trans--carotene equivalent g-1 sample) were obtained in the range from
43
44 334 50 to 60 °C and from 10 to 15% w/w, ethanol. An increase in the carotenoid extraction
45
46
47
335 yield by the use of ethanol as a modifier can be due to two effects: a) the increase of the
48
49 336 solubility of carotenoids in the supercritical solvent (scCO2 + ethanol) due to the slightly
50
51 337 polar character of this type of molecules, allowing an easy formation of hydrogen bonds
52
53
54 338 with the ethanol present in the CO2 stream and b) the expansion of the pores of the matrix,
55
56 339 facilitating the release of the pigments (Shi et al., 2007). The temperature also had a
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60
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 1
2
3
4 340 significantly positive effect on carotenoid extraction yield. From the best of our knowledge,
5
6
7 341 there is only one work about the preparation of extracts from mango peel by using SFE.
8
9
10 342 Garcia-Mendoza et al. (2015) explored neat scCO2 at 40 °C and 30 MPa, achieving
11
12 343 a global extraction yield of 3.15  0.31%. They also reported the concentration of
13
14
15 344 carotenoids in the extract and the carotenoids yield were 5.60  0.51 mg -carotene g-1
16
17 345 extract and 0.17 0.01 mg -carotene g-1 sample, respectively. It is worth noting and
18
19
20 346 confirm by the present study, the positive and important effect of ethanol as co-solvent on
21
22 347 the global extraction yield of those type of compounds. As valorisation strategy for mango
23
24
25 348 peel var. Sugar, the optimum value predicted to maximize the carotenoids extraction yield
26
27 349 was calculated by the combination of the factors studied. The optimum response predicted
28
29
30 350 was 2.13 mg all trans--carotene equivalent g-1 sample and it was found at 25.0 MPa, 60
31
32 351 °C and 15% ethanol. Two replicates experiments at those conditions were carried out to
33
34
35 352 validate the mathematical model obtained (Eq. 2).
36
37
38 353
39
40 354
41
42 355
43 356 Eq.2
44
45
46 357 The experimental value found for the validation model was 1.900  0.023 mg -carotene g-
47
48 1
358 sample. Based on the relative deviation value (12.1%), it was considered that the model
49
50
51 359 used was satisfactory to predict the experimental values of carotenoids extraction yield.
52
53 360 Additionally, other values at optimal conditions validation such as global extraction yield
54
55
56 361 (5.443  0.435%) and concentration of carotenoids (35.002  2.382 all trans--carotene
57
58 362 equivalent g-1 extract) were obtained. The chromatographic profile of the extract obtained
59
60
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 1
2
3
4 363 under SFE optimum conditions is showed in Figure 1A. A similar chromatografic profile
5
6
7 364 was obtained in comparison with the CMP (Figure 1B) and FMP (Figure 1C) samples.
8
9 365 All-trans--carotene was the main compound present in the SFE extract obtained at the
10
11
12 366 optimized conditions, as well as 9-cis- and 13-cis--carotene. Despite the chromatografic
13
14 367 profile was similar among the three analysed samples, All-trans--carotene in SFE extract
15
16
17 368 (23.245  3.58 mg all-trans--carotene g-1 extract) resulted to be much higher than in CMP
18
19
20 369 extract (9.031 mg  0.033 all-trans--carotene g-1 extract ) and FMP extract (9.239  0.097
21
22 370 mg all-trans--carotene g-1 extract) , with both CMP and FMP extracts being obtained by
23
24
25 371 conventional extraction solvent. It demostres the higher selectivity of the SFE technique for
26
27 372 carotenoids compounds, being superior to the conventional extraction solvent.
28
29
30 373
31
32
33 374 3.4. Oxidative stability of sunflower oil with added b-carotene standard and SFE
34
35 375 extract
36
37
38 376 Extract obtained by SFE under optimal conditions of pressure, temperature, and co-solvent
39
40 377 was effective to inhibiting lipid oxidation of a bulk sunflower oil (Figure 4). Protection
41
42
43 378 effect of extract contrasted with the no effect observed when pure all-trans-β-carotene was
44
45 379 tested at equivalent concentrations. Higher effectiveness of SFE-extract as compared to
46
47
48 380 pure all- trans-β-carotene might be explained by cooperative effects among other
49
50 381 carotenoids present in the extract, as revealed by RP-UHPLC-DAD. Furthermore, other
51
52
53 382 compounds different to carotenoids present in the extract might contribute to such positive
54
55 383 effect.
56
57
384
58
59
60 385 4. CONCLUSIONS
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 1
2
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4 386 The chemical characterization of mango peel var. Sugar showed interesting nutritional
5
6
7 387 features, in terms of dietary fiber, crude protein, and total soluble phenols content. Despite
8
9 388 of freeze-drying was more effective to preserve all-trans-β-carotene than convective air
10
11
12 389 drying, this last technique becomes more atractive due to its simplicity, speed, and low cost
13
14 390 for a valorisation strategy. Among the studied factors assesed by SFE optimization, the
15
16
391 ethanol concentration in the solvent mixture showed the greatest significant effect on all the
17
18
19 392 variable responses studied. The maximum carotenoids extration yield was found at 25.0
20
21 393 MPa, 60 °C, and 15% w/w. At such optimal conditions, the carotenoids extraction yield was
22
23
24 394 1.9 mg β-carotene equivalent g-1 sample. SFE extract protected a bulk sunflower oil from
25
26 395 lipid oxidation. In contrast when testing pure all-trans-β-carotene at concentration
27
28
29 396 equivalent to those present in the SFE extract, no effect was observed. All in all, mango
30
31 397 peel is a source of dietary fiber and its SFE extract is able to protect edible oil systems.
32
33
398
34
35
36 399 5. ACKNOWLEDGEMENTS
37
38
39 400 A.P.S-C. thanks to the Administrative Department of Science, Technology, and Innovation
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41 401 COLCIENCIAS (Colombia) for her postdoctoral fellowship (784-2017). Authors want to
42
43
44 402 thank to Yolanda Quiñones and Jorge Enrique Palomino Millan for their help on the
45
46 403 Rancimat assays.
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49 404
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594 Fluid Extraction (SFE) of carotenoids from Persimmon (Diospyros kaki L.). Food
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43 596 Zeb, A. (2011). Effects of β-carotene on the thermal oxidation of fatty acids. AFRICAN
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48 598 https://doi.org/10.5897/AJB11.1013
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4 600 FIGURES
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7 601 Figure 1. Chromatograms (450 nm) corresponding to the (A) optimal extract obtained by
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10 602 SFE, (B) convective-air flow dried mango peel extract and (C) freeze-dried dried mango
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12 603 peel extract. 1. All-trans--carotene; 2. 9-cis-β-carotene; 3. 13-cis-β-carotene
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15 604 Figure 2. Pareto chart of standardized effects for a) global extraction yield and b)
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18 605 carotenoids concentration in the extract. The vertical line defines the 95 percent confidence
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20 606 interval.
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23 607 Figure 3. a) Pareto chart and b) response surfaces for the extraction yield of carotenoids (g
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26 608 -carotene/g sample) as a function of ethanol concentration and temperature at 30.0 MPa.
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29 609 Figure 4. Results for the protection factor of sunflower oil added with SFE optimum
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31 610 extract () and All-trans--carotene () standard at different concentrations.
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4 640 TABLES
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7 641 Table 1. Box-Behnken experimental design for global yield of scCO2 + ethanol extraction
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10 642 of carotenoids compounds, conditions, and results.
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13 Ethanol Carotenoids
Pressure Temper. Global Carotenoids yield
14 concentration concentration
Run (MPa) (°C) extraction (mg -carotene g-1
15 (%w/w) (mg -carotene
16 X1 X2 Yield (%) dried mango peel)
17 X3 g-1 extract)
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1 25 (-1) 50 (0) 15 (+1) 6.123 29.397 1.800
20 2 30 (0) 40 (-1) 15 (+1) 5.897 26.065 1.537
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22 3 25 (-1) 60 (+1) 10 (0) 5.388 29.412 1.585
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24 4 30 (0) 40 (-1) 5 (-1) 2.798 36.003 1.007
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5 30 (0) 60 (+1) 5 (-1) 1.615 62.834 1.015
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27 6 30 (0) 60 (+1) 15 (+1) 6.249 34.369 2.148
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29 7 30 (0) 50 (0) 10 (0) 4.433 30.956 1.372
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31 8 35 (+1) 60 (+1) 10 (0) 5.965 24.296 1.449
32 9 35 (+1) 50 (0) 15 (+1) 3.460 39.533 1.368
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34 10 35 (+1) 40 (-1) 10 (0) 1.602 55.243 0.885
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36 11 30 (0) 50 (0) 10 (0) 4.772 30.323 1.447
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38 12 25 (-1) 50 (0) 5 (-1) 4.477 29.339 1.313
39 13 25 (-1) 40 (-1) 10 (0) 3.657 34.758 1.271
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41 14 35 (+1) 50 (0) 5 (-1) 2.286 57.599 1.316
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43 15 30 (0) 50 (0) 10 (0) 4.562 34.302 1.565
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4 646 Table 2. Chemical composition of mango peel (Mangifera Indica L.) var. Sugar
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7 Components (%) Mango peel var. Sugar
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9 Moisture in fresh 74.60  0.70
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11 Total lipids (Soxhlet)a.b 1.56  0.05
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4.15  0.05
a.b
13 Fixed mineral residue (Ash)
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35.62  0.54
a.b
Total dietary fiber
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16 Soluble dietary fiber a.b 12.09  0.31
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18 Insoluble dietary fiber a.b 23.53  0.44
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20 Total protein (N x 6.25) a.b 6.33  0.12
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22 Carbohydrates a.b.c 52.34  0.56
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Total soluble phenols content (mg GAE g-1 sample) a.b 64.79  0.59
25 647 a b
Values on a dry weight basis (d.w.). Mean of three determinations ± standard deviation.
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648 Calculated by difference with the other components.
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4 654 Table 3. Effect of the drying method of mango peel samples on carotenoids content
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7 Carotenoid content (mg -carotene g-1 sample) CMP FMP
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9 Total carotenoids content. by UV-Vis 1.22  0.02 2.01  0.05
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11 β-carotene content. calculated by RP-UHPLC-DAD 1.121  0.055 1.648  0.017
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Figure
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Figure
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Figure
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Figure
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*Graphical Abstract
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