Optimization of antioxidant extraction and characterization of oil obtained by pressing cold from <i>Vitis labrusca</i> seeds

DALPOSSO, Pâmela Vanessa; AGUIAR, Caroline Mariana de; TORQUATO, Alex Sanches; TIUMAN, Tatiana Shioji; MARTIN, Clayton Antunes; ZARA, Ricardo Fiori; COTTICA, Solange Maria

doi:10.1590/fst.47420

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Original Article • Food Sci. Technol (Campinas) 42 • 2022 • https://doi.org/10.1590/fst.47420 copy

Optimization of antioxidant extraction and characterization of oil obtained by pressing cold from Vitis labrusca seeds

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Abstract

This study aimed to optimize the extraction solvents for Bordo grape (Vitis labrusca) seeds by response surface methodology regarding to the antioxidant activity (AA) and trans-resveratrol content. Fatty acids (FA) and AA of the oil obtained by pressing cold method were also determined. The extraction optimization was determined by the statistical simplex-centroid mixing scheme, enabling the analysis of solvents effects (water, ethanol and acetone) and their mixtures on the responses. AA was performed by DPPH, ABTS and FRAP methods, and by total phenolic compounds and flavonoids. FA were determined by GC and trans-resveratrol by HPLC. The extracts containing ternary fraction of solvents showed greater AA, increasing about 20 times compared to pure solvent. The composition that showed the best response ranged between 45-48% of water, 14-20% of ethanol and 35-38% of acetone for both grape seeds, with polarity ranged from 0.705 to 0.706. The oil from seeds showed high concentrations of PUFA, particularly linoleic acid. The optimized extraction method improved the use of this residue as a potential antioxidant source for food industry.

Keywords:
industrial by-products; solvent extraction; mixture modeling; phenolic compounds; Trans-resveratrol; fatty acids

Extracts	Water (W)	Ethanol (E)	Acetone (A)
1	1^a a Volumetric proportion: 1= 100%; 1/2= 50%; 1/3= 33.33%.	0	0
2	0	1	0
3	0	0	1
4	1/2	1/2	0
5	1/2	0	1/2
6	0	1/2	1/2
7	1/3	1/3	1/3

	Fermented (%)	Unfermented (%)
Moisture	10.16 ± 0.19^B	12.52 ± 0.20^A
Ash	1.76 ± 0.05^A	1.67 ± 0.02^B
Protein	8.60 ± 0.27^A	8.26 ± 0.27^A
Lipid	13.46 ± 0.18^A	13.73 ± 0.15^A

Extracts	DPPH	ABTS	FRAP	Phenolic compounds	Flavonoids	trans – resveratrol
Extracts	µmol TE g^-1 extract	µmol TE g^-1 extract	µmol EFeSO₄ g^-1 extract	mg EAG g^-1 extract	mg EQ g^-1 extract	(mg L^-1)
Fermented
W (1)	104.44 ± 11.49^C	62.26 ± 0.00^E	599.6 ± 4.24^D	18.35 ± 1.25^D	0.36 ± 0.03^C	ND
E (1)	269.77 ± 71.75^C	160.26 ± 21.68^E	180.93 ± 40.07^F	24.86 ± 1.51^CD	1.22 ± 0.09^BC	0.21 ± 0.03^C
A (1)	62.66 ± 5.33^C	117.82 ± 16.67^E	51.60 ± 3.30^G	14.19 ± 0.71^D	0.58 ± 0.05^C	0.04 ± 0.00^C
W/E (1/2:1/2)	952.00 ± 32.00^B	1140.13 ± 75.08^C	4192.53 ± 29.70^B	190.71 ± 3.03^B	8.42 ± 0.38^A	1.39 ± 0.07^AB
W/A (1/2:1/2)	1184.88 ± 42.86^AB	1452.13 ± 14.04^B	4557.11 ± 78.12^A	263.07 ± 8.61^A	8.80 ± 0.30^A	1.18 ± 0.12^B
A/E (1/2:1/2)	342.00 ± 14.00^C	370.71 ± 33.89^D	349.27 ± 32.26^E	42.86 ± 1.89^C	1.84 ± 0.15^B	0.24 ± 0.07^C
A/E/W (1/3:1/3:1/3)	1296.00 ± 256.62^A	1684.80 ± 127.27^A	4061.09 ± 59.09^C	244.44 ± 17.99^A	8.12 ± 0.86^A	2.01 ± 0.70^A
Unfermented
W (1)	247.11 ± 34.21^EF	324.93 ± 23.24^E	791.89 ± 48.57^C	31.64 ± 2.13^D	1.14 ± 0.19^D	0.22 ± 0.05^D
E (1)	394.22 ± 71.02^E	578.71± 2.77^E	500.82 ± 45.82C^D	44.76 ± 3.17^CD	1.82 ± 0.38^CD	1.99 ± 0.19^C
A (1)	121.33 ± 39.62^F	321.37 ± 79.88^E	276.04 ± 50.53^D	21.91 ± 2.73^D	1.18 ± 0.10^D	2.78 ± 0.27^C
W/E (1/2:1/2)	1060.44 ± 49.55^C	1385.46 ± 128.33^C	4424.36 ± 111.91^B	221.16 ± 4.48^B	10.38 ± 0.51^B	8.94 ± 1.12^AB
W/A (1/2:1/2)	1453.33 ± 58.84^B	1980.13 ± 61.49^B	5372.66 ± 215.72^A	292.56 ± 9.86^A	11.75 ± 0.41^A	8.28 ± 0.24^B
A/E (1/2:1/2)	705.33 ± 25.75^D	918.31 ± 76.19^D	789.33 ± 32.51^C	64.19 ± 5.48^C	2.29 ± 0.28^C	2.59 ± 0.16^C
A/E/W (1/3:1/3:1/3)	1704.00 ± 80.13^A	2835.77 ± 116.71^A	4512.66 ± 155.06^B	311.66 ± 19.72^A	12.36 ± 0.57^A	9.84 ± 0.37^A

Fermented seed
Assay	Predicted values	Obtained values
DPPH	1195.38^a a water:etanol:acetone - 0.48:0.14:0.38 (v/v);	1144.00 ± 124.19
ABTS	1684.81	1138.00 ± 137.76
FRAP	4585.22	3449.33 ± 98.99
FC	264.55	179.97 ± 8.65
FLA	8.10	8.79 ± 1.13
Unfermented seed
DPPH	1800.24^b b water:etanol:acetone - 0.45:0.20:0.35 (v/v). Where DPPH (µmol TE g-1 extract), ABTS (µmol TE g-1 extract), FRAP (µmol EFeSO4 g-1 extract), FC = phenolic compounds (mg EAG g-1 extract) and FLA = flavonoids (mg EQ g-1 extract).	1340.00 ± 97.07
ABTS	2630.95	1486.88 ± 127.25
FRAP	5120.55	4512.66 ± 175.24
FC	341.57	220.31 ± 3.88
FLA	13.53	10.89 ± 1.01

Assay	Fermented	Unfermented
Assay	(mg g^-1 oil)	(mg g^-1 oil)
Fatty acids
14:0	0.65 ± 0.04^A	0.49 ± 0.00^B
15:0	0.39 ± 0.02^A	0.35 ± 0.01^A
16:0	72.35 ± 3.49^A	66.05 ± 0.35^B
16:1	1.16 ± 0.07^A	0.77 ± 0.01^B
17:0	0.68 ± 0.02^A	0.65 ± 0.00^A
18:0	33.26 ± 0.73^A	32.94 ± 0.15^A
18:1n9c	184.62 ± 7.03^A	175.13 ± 0.29^A
18:2n6t	6.59 ± 0.23^A	5.98 ± 0.24^B
18:2n6c	744.94 ± 37.86^A	713.90 ± 2.77^A
20:0	1.68 ± 0.04^A	1.73 ± 0.00^A
18:3n3	3.96 ± 0.23^A	3.54± 0.03^B
20:1	0.35 ± 0.01^A	0.36 ± 0.03^A
∑ SFA	109.04 ± 4.36^A	102.24 ± 0.52^A
∑ MUFA	186.13 ± 7.11^A	176.27 ± 0.31^A
∑ PUFA	755.50 ± 38.33^A	723.43 ± 3.90^A
IA	0.08 ± 0.00 ^A	0.08 ± 0.00^A
IT	0.22 ± 0.00 ^A	0.22 ± 0.00 ^A
HH	12.88 ± 0.06 ^A	13.50 ± 0.08 ^B
Antioxidant activity
DPPH (µmol TE g^-1 sample)	20.00 ± 5.65^A	15.33 ± 2.31^A
ABTS (µmol TE g^-1 sample)	13.60 ± 4.6^A	14.26 ± 0.00^A
FRAP (µmol EFeSO₄ g^-1 sample)	17.93 ± 0.94^A	10.60 ± 1.88^B
Phenolic compounds (mg EAG g^-1 sample)	ND	ND
Flavonoids (mg EQ g^-1 sample)	0.05 ± 0.00^B	0.17 ± 0.00^A

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[1] *Corresponding author: smcottica@utfpr.edu.br