RED WINE EXTRACT OBTAINED BY MEMBRANE-BASED SUPERCRITICAL FLUID EXTRACTION: PRELIMINARY CHARACTERIZATION OF CHEMICAL PROPERTIES.

Silva, W.; Romero, J.; Morales, E.; Melo, R.; Mendoza, L.; Cotoras, M.

doi:10.1590/0104-6632.20170342s20150631

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Separation Processes • Braz. J. Chem. Eng. 34 (2) • Apr 2017 • https://doi.org/10.1590/0104-6632.20170342s20150631 copy

RED WINE EXTRACT OBTAINED BY MEMBRANE-BASED SUPERCRITICAL FLUID EXTRACTION: PRELIMINARY CHARACTERIZATION OF CHEMICAL PROPERTIES.

Authorship SCIMAGO INSTITUTIONS RANKINGS

ABSTRACT

This study aims to obtain an extract from red wine by using membrane-based supercritical fluid extraction. This technique involves the use of porous membranes as contactors during the dense gas extraction process from liquid matrices. In this work, a Cabernet Sauvignon wine extract was obtained from supercritical fluid extraction using pressurized carbon dioxide as solvent and a hollow fiber contactor as extraction setup. The process was continuously conducted at pressures between 12 and 18 MPa and temperatures ranged from 30 to 50ºC. Meanwhile, flow rates of feed wine and supercritical CO₂ varied from 0.1 to 0.5 mL min^-1 and from 60 to 80 mL min^-1 (NCPT), respectively. From extraction assays, the highest extraction percentage value obtained from the total amount of phenolic compounds was 14% in only one extraction step at 18MPa and 35ºC. A summarized chemical characterization of the obtained extract is reported in this work; one of the main compounds in this extract could be a low molecular weight organic acid with aromatic structure and methyl and carboxyl groups. Finally, this preliminary characterization of this extract shows a remarkable ORAC value equal to 101737 ± 5324 µmol Trolox equivalents (TE) per 100 g of extract.

Keywords
Supercritical fluid extraction; wine; membrane contactor; extract; chemical characterization

Variables	Low level (-1)	Medium level (0)	High level (+1)
Liquid solution flow rate (mL min ^-1 )	0.1	0.3	0.5
CO ₂ flow rate, NCPT (mL min ^-1 )	60	70	80
Temperature (°C)	30	40	50
Pressure (bar)	120	150	180

Time (min)	Volumetricflow (mLmin^-1 )	A (Acetic acid 1%)	B (Acetonitrile)
0	0.8	90	10
20	0.8	80	20
41	0.8	80	20
45	0.8	50	50
65	0.8	50	50

Effects	Extraction percentage (%)				Transmembrane flux (molGAE h^-1 m^-2 )
	Estimated (± 3.0596)	Optimum level	Magnitude	Value (%)	Estimated (± 0.0035518)	Optimum level	Magnitude	Value (mol h^-1 m^-2 )
13.99	0.034
		Temperature (ºC)	-0.4053	-0.5	35	-0.0004220	34.4	34.4
		Pressure (bar)	1.7059	0.7	170	0.0030090	178	178
		Red wine flow (mLmin^-1)	3.4962	1	0.5	0.0242481	0.5	0.5
CO₂ SC flow (mL min^-1)	3.1773	80	80	0.0055239	75	75

Matrix	Solvent	Operational conditions	Extraction Yield	Ref.
Grape pomace	Subcritical water	Batch system; 11.6 MPa - 140 °C.	Phenolic compounds/31.69 mg GAE g^-1 db.	Aliakbarian B. et al. 2012
Grape seed	Subcritical water	Batch system; 1500 psig- 150 °C.	Catechins and Proanthocyanidins/ 70% db.	García-Marino et al. 2006
Grape seed	Supercritical CO₂	Batch system; 250-300 bar; 2 - 5% ethanol	Complex phenols and tannins/ less [EtOH] and pressure ( less [Polyphenols]	Murga et al. 2000
Grape seed		Batch system; 35 MPa - 313 K.	13.42 % of extraction yield db at 430 min.	Meireles et al. 2012
Grape seed		Batch system; 250-300 bar; 30-50 °C; 15-20 % ethanol	Gallic acid 2.6 - 32.9 mg kg^-1 db. Catechins 5.8 - 78.83 mg kg^-1 db. Epicatechins 4.8 - 35.15 mg kg^-1 db.	Yilmaz et al. 2011
Seed, stem, skin and grape pomace		Batch system, 400 bar; 308 K; 5 % v/v ethanol	Resveratrol with extraction yield between 15 and 21 times greater than conventional methods.	Goli, Barzegar and Sahari 2005

Factor	Value	Optimum level
Temperature	32 ºC	-0.9
Pressure	180 bar	1
Red wine flow rate	0.5 mL min^-1	1
scCO₂ flow rate	70 mL min^-1 NCPT	0

mmol TE g^-1	µM Trolox	µmol TE g^-1	µmol TE per 100 g
1.017	10878.69	1017.37	101737.07

Substance/Food	ORAC value	Unit	Source
Ascorbic Acid	40.4 ± 2.1	µM TE	Zulueta et al. (2009)
Gallic Acid	161 ± 4.8	µM TE
β - carotene	582 ± 30.3	µM TE
Zeaxanthin	1108 ± 5.9	µM TE
BHA (Butylated Hydroxy anisole)	13500 ± 332	µmol TE g^-1	Dávalos et al. (2004)
Squalene	304.3	µmol TE g^-1	Kraujalis and Venskutonis (2013)
Cinnamon, ground	131420 ± 13867	µmol TE/100g^-1	Haytowitz and Bhagwat (2010)
Rosemary, dried	165280 ± 1319	µmol TE/100g^-1
Oregano, dried	175295 ± 7683	µmol TE/100g^-1
Cloves, ground	290283 ± 3292	µmol TE/100g^-1
Red wine Cabernet Sauvignon
Santa Tierra (Chile)	28.064 ± 2.073	µmol TE mL^-1	Van Leew et al. (2014)
Casillero del Diablo (Chile)	42.669 ± 1,14	µmol TE mL^-1
Sunrise (Chile)	25.773 ± 1.493	µmol TE mL^-1
Chocolate, Dark
Black & Green´s Organic	118.9	µM TEg^-1	Stockham et al. (2011)
Lindt, 70 %	171.8	µM TE g^-1
Lindt, 90 %	290.0	µM TE g^-1
Fruits
Strawberry	154	µmol TEg^-1	Yilmaz et al. (2006)
Plum	80	µmol TE g^-1
Red Grape	36	µmol TE g^-1
Orange	52	µmol TE g^-1
Blueberries	63 - 282	µmol TE g^-1
Blackberries	8650 ± 200	µM TE	Atala et al. (2009)
Raspberry	2870 ± 700	µM TE	Atala et al. (2009)
Tomato dry	222.3 ± 285.61	µmol TE g^-1	Li et al. (2012)

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[1] *To whom correspondence should be addressed. E-mail: julio.romero@usach.cl. Phone: +56 2 27181821