MD825Z - Process for producing polyphenols from grape pomace - Google Patents
Process for producing polyphenols from grape pomace Download PDFInfo
- Publication number
- MD825Z MD825Z MDS20140011A MDS20140011A MD825Z MD 825 Z MD825 Z MD 825Z MD S20140011 A MDS20140011 A MD S20140011A MD S20140011 A MDS20140011 A MD S20140011A MD 825 Z MD825 Z MD 825Z
- Authority
- MD
- Moldova
- Prior art keywords
- polyphenols
- pomace
- extract
- solution
- grape pomace
- Prior art date
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- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 24
- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 24
- 235000009754 Vitis X bourquina Nutrition 0.000 title claims abstract description 11
- 235000012333 Vitis X labruscana Nutrition 0.000 title claims abstract description 11
- 235000014787 Vitis vinifera Nutrition 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 title claims abstract description 11
- 240000006365 Vitis vinifera Species 0.000 title 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000284 extract Substances 0.000 claims abstract description 17
- 241000219095 Vitis Species 0.000 claims abstract description 10
- 235000019441 ethanol Nutrition 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- 235000013305 food Nutrition 0.000 abstract description 2
- 238000004821 distillation Methods 0.000 abstract 1
- 230000002225 anti-radical effect Effects 0.000 description 7
- 238000000605 extraction Methods 0.000 description 7
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- CWEZAWNPTYBADX-UHFFFAOYSA-N Procyanidin Natural products OC1C(OC2C(O)C(Oc3c2c(O)cc(O)c3C4C(O)C(Oc5cc(O)cc(O)c45)c6ccc(O)c(O)c6)c7ccc(O)c(O)c7)c8c(O)cc(O)cc8OC1c9ccc(O)c(O)c9 CWEZAWNPTYBADX-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 229920002414 procyanidin Polymers 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000000108 ultra-filtration Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 1
- 229920002770 condensed tannin Polymers 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
Invenţia se referă la industria farmaceutică şi alimentară şi poate fi utilizată pentru obţinerea polifenolilor din tescovină de struguri. The invention relates to the pharmaceutical and food industries and can be used to obtain polyphenols from grape marc.
Este cunoscut procedeul de obţinere a polifenolilor din sâmburi de struguri cu soluţie apoasă de acetonă 80%, evaporarea solventului şi concentrarea polifenolilor, cu refrigerarea ulterioară timp de 24 ore pentru precipitarea procianidelor polimerice şi filtrarea acestora. Metoda include ultrafiltrarea extractului pentru înlăturarea substanţelor cu masă moleculară mare şi o ultrafiltrare suplimentară, pentru a minimiza procianidinele cu masă moleculară mare. Extractul ultrafiltrat este extras repetat cu acetat de etil, pentru a extrage toate procianidinele oligomerice. Faza organică este concentrată în vid, iar oligomerii sunt precipitaţi prin adăugare de clorură de metilen. Precipitatul este centrifugat şi uscat la 50°C în vid, 24 ore, pentru a obţine extractul sub formă de pudră [1]. The process of obtaining polyphenols from grape seeds with 80% aqueous acetone solution, evaporation of the solvent and concentration of polyphenols, with subsequent refrigeration for 24 hours to precipitate polymeric procyanidins and their filtration is known. The method includes ultrafiltration of the extract to remove high molecular weight substances and an additional ultrafiltration to minimize high molecular weight procyanidins. The ultrafiltered extract is extracted repeatedly with ethyl acetate to extract all oligomeric procyanidins. The organic phase is concentrated in vacuo, and the oligomers are precipitated by adding methylene chloride. The precipitate is centrifuged and dried at 50°C in vacuo for 24 hours to obtain the extract in powder form [1].
Dezavantajul acestui procedeu constă în reziduurile de solvenţi rămase în extractele uscate. The disadvantage of this process lies in the solvent residues remaining in the dried extracts.
În calitate de cea mai apropiată soluţie se cunoaşte un procedeu de obţinere a polifenolilor din tescovină de struguri în mai multe etape. Tescovina umedă se depozitează la temperaturi mai mici de 10°C, timp de 24 ore, se usucă la temperaturi cuprinse între 20…85°C, până la o umiditate mai mică de 15%, apoi se triturează şi se macină până la o granulaţie mai mică de 500 µ, polifenolii din tescovină se extrag cu soluţie apoasă de etanol 20…80%, la temperaturi de 20…85°C, timp de 15 min…20 ore, soluţia extractului se filtrează printr-un filtru-presă mai mic de 25 µm, se elimină alcoolul etilic din soluţia extractului prin evaporare pe rotavapor, apoi soluţia apoasă cu extract de polifenoli este pulverizată în atomizor, obţinându-se un extract de polifenoli sub formă de pulbere [2]. As the closest solution, a multi-stage process for obtaining polyphenols from grape pomace is known. The wet pomace is stored at temperatures below 10°C for 24 hours, dried at temperatures between 20…85°C, to a humidity of less than 15%, then triturated and ground to a granulation of less than 500 µ, the polyphenols from the pomace are extracted with an aqueous solution of 20…80% ethanol, at temperatures of 20…85°C, for 15 min…20 hours, the extract solution is filtered through a filter press smaller than 25 µm, the ethyl alcohol is removed from the extract solution by evaporation on a rotary evaporator, then the aqueous solution with polyphenol extract is sprayed in an atomizer, obtaining a polyphenol extract in powder form [2].
Dezavantajul acestui procedeu constă în aceea că sunt prezente mai multe etape în obţinerea polifenolilor şi durata lungă a procesului tehnologic. The disadvantage of this process is that there are several stages in obtaining polyphenols and the technological process is long.
Problema pe care o rezolvă invenţia propusă este accelerarea procesului de extracţie şi mărirea randamentului de polifenoli din tescovină de struguri cu activitatea antiradicalică înaltă. The problem solved by the proposed invention is to accelerate the extraction process and increase the yield of polyphenols from grape pomace with high antiradical activity.
Conform invenţiei, procedeul revendicat constă în aceea că tescovina umedă de struguri se tratează cu curent electric alternativ cu tensiunea de 90…260 V şi intensitatea de 300…866,6 V/cm, care produce 900 de impulsuri electrice cu durata de 900 µs, timp de 15 min, apoi polifenolii din tescovină se extrag cu o soluţie apoasă de etanol de 20…80%, la temperatura de 25…65°C, timp de 15…60 min, după care soluţia de extract se filtrează, se elimină alcoolul etilic prin evaporare pe rotavapor cu obţinerea unui extract de polifenoli sub formă de pastă cu activitatea antiradicalică înaltă. According to the invention, the claimed process consists in treating wet grape pomace with alternating electric current with a voltage of 90…260 V and an intensity of 300…866.6 V/cm, which produces 900 electrical pulses with a duration of 900 µs, for 15 min, then the polyphenols in the pomace are extracted with an aqueous solution of 20…80% ethanol, at a temperature of 25…65°C, for 15…60 min, after which the extract solution is filtered, the ethyl alcohol is eliminated by evaporation on a rotary evaporator, obtaining a polyphenol extract in the form of a paste with high antiradical activity.
Rezultatul invenţiei constă în accelerarea procesului de extracţie şi reducerea pierderilor de polifenoli din tescovină de struguri cu activitatea antiradicalică înaltă. The result of the invention consists in accelerating the extraction process and reducing the losses of polyphenols from grape pomace with high antiradical activity.
Avantajul invenţiei revendicate constă în micşorarea numărului de operaţiuni. În soluţia cea mai apropiată sunt 8 etape, iar în soluţia revendicată 4, durata procedeului de obţinere a polifenolilor în soluţia revendicată constituie maximum 1,25 ore, iar în cea mai apropiată soluţie - 44 ore, randamentul de polifenoli în soluţia revendicată constituie minimum 86%, iar în cea mai apropiată soluţie - 85%, totodată cu cât numărul de operaţiuni şi durata lor pentru extracţia de polifenoli este mai mică, cu atât activitatea antiradicalică a extractului este mai mare. The advantage of the claimed invention lies in the reduction of the number of operations. In the closest solution there are 8 stages, and in the claimed solution 4, the duration of the process of obtaining polyphenols in the claimed solution is a maximum of 1.25 hours, and in the closest solution - 44 hours, the yield of polyphenols in the claimed solution is a minimum of 86%, and in the closest solution - 85%, at the same time, the smaller the number of operations and their duration for the extraction of polyphenols, the higher the antiradical activity of the extract.
Exemplu de realizare a invenţiei Example of embodiment of the invention
O parte de tescovină umedă, în cantitate de 300 g, se amplasează între doi electrozi în camera de prelucrare. Materialul este supus unei tensiuni electrice de 165 V, care generează un curent electric alternativ cu tensiunea de 500 V/cm şi produce 900 de impulsuri electrice cu durata de 900 µs timp de 15 min. Extracţia tescovinei pretratate se realizează într-un vas, prevăzut cu încălzire şi agitare cu 2400 ml soluţie apoasă de etanol de 50%, timp de o oră, la temperatura de 65°C. După extracţie, suspensia se filtrează. Soluţia obţinută este încărcată în rotavapor unde se recuperează alcoolul etilic. Se obţine un extract de polifenoli sub formă de pastă, cu activitatea antiradicalică înaltă. A portion of wet pomace, in an amount of 300 g, is placed between two electrodes in the processing chamber. The material is subjected to an electrical voltage of 165 V, which generates an alternating electric current with a voltage of 500 V/cm and produces 900 electrical pulses with a duration of 900 µs for 15 min. The extraction of the pretreated pomace is carried out in a vessel, equipped with heating and stirring with 2400 ml of 50% ethanol aqueous solution, for one hour, at a temperature of 65°C. After extraction, the suspension is filtered. The solution obtained is loaded into a rotary evaporator where the ethyl alcohol is recovered. A polyphenol extract is obtained in the form of a paste, with high antiradical activity.
Tabel Table
№ Tensiunea, V Intensitatea curentului electric, V/cm Numărul de impulsuri Temperatura procesului de extracţie, °C Masa de taninuri, mg/300 g Activitatea antiradicalică, % 1 90 300 900 25 360,3 84,5 2 165 500 900 25 510,7 85,7 3 260 866,6 900 25 480,3 87,2 4 90 300 900 65 2941,6 88,3 5 165 500 900 65 3180,2 89,5 6 260 866,6 900 65 2804,4 87,1 7 90 300 900 90 253,6 54,6 8 165 500 900 90 312,6 53.1 9 260 866,6 900 90 178,4 52,6№ Voltage, V Electric current intensity, V/cm Number of pulses Extraction process temperature, °C Tannin mass, mg/300 g Antiradical activity, % 1 90 300 900 25 360.3 84.5 2 165 500 900 25 510.7 85.7 3 260 866.6 900 25 480.3 87.2 4 90 300 900 65 2941.6 88.3 5 165 500 900 65 3180.2 89.5 6 260 866.6 900 65 2804.4 87.1 7 90 300 900 90 253.6 54.6 8 165 500 900 90 312.6 53.1 9 260 866.6 900 90 178.4 52.6
Mărirea tensiunii electrice a câmpului electric pulsator, a timpului de aplicare a impulsului electric şi a temperaturii procesului de extracţie duc la degradarea polifenolilor şi scăderea activităţii antiradicalice. Increasing the voltage of the pulsating electric field, the application time of the electric pulse, and the temperature of the extraction process lead to the degradation of polyphenols and a decrease in antiradical activity.
1. US 5484594 A 1996.01.16 1. US 5484594 A 1996.01.16
2. RO 125704 B1 2012.02.28 2. EN 125704 B1 2012.02.28
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| MDS20140011A MD825Z (en) | 2014-01-22 | 2014-01-22 | Process for producing polyphenols from grape pomace |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| MDS20140011A MD825Z (en) | 2014-01-22 | 2014-01-22 | Process for producing polyphenols from grape pomace |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| MD825Y MD825Y (en) | 2014-10-31 |
| MD825Z true MD825Z (en) | 2015-05-31 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| MDS20140011A MD825Z (en) | 2014-01-22 | 2014-01-22 | Process for producing polyphenols from grape pomace |
Country Status (1)
| Country | Link |
|---|---|
| MD (1) | MD825Z (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MD855Z (en) * | 2014-01-29 | 2015-07-31 | Институт Генетики, Физиологии И Защиты Растений Академии Наук Молдовы | Process for preparing antioxidant compounds from kernel peel of walnut Juglans regia L. |
| MD1136Z (en) * | 2016-09-13 | 2017-11-30 | Елена КРИСТЯ | Process for producing an extract from grape pomace |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5484594A (en) * | 1988-06-28 | 1996-01-16 | Tecnofarmaci S.P.A. | Process for preparing grapeseed extracts enriched in procyanidol oligomers |
| MD3866C2 (en) * | 2008-12-19 | 2009-10-31 | Институт Генетики, Физиологии И Защиты Растений Академии Наук Молдовы | 5,4-dimethylcampherol 3-O--D-(6′′-a′-L-rhamnopyranosyl)-glucopyranoside as compound increasing the seed productivity |
| RO125704B1 (en) * | 2009-03-30 | 2012-02-28 | Simona Elena Bişboacă | Process for obtaining polyphenols from marc |
| MD585Z (en) * | 2012-04-13 | 2013-08-31 | Государственный Медицинский И Фармацевтический Университет "Nicolae Testemitanu" Республики Молдова | Method for quantitative determination of flavonoids in egetable raw material |
| MD636Z (en) * | 2012-12-21 | 2013-12-31 | Институт Генетики, Физиологии И Защиты Растений Академии Наук Молдовы | Process for producing flavonoid glycosides from Linaria vulgaris Mill. |
-
2014
- 2014-01-22 MD MDS20140011A patent/MD825Z/en not_active IP Right Cessation
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5484594A (en) * | 1988-06-28 | 1996-01-16 | Tecnofarmaci S.P.A. | Process for preparing grapeseed extracts enriched in procyanidol oligomers |
| MD3866C2 (en) * | 2008-12-19 | 2009-10-31 | Институт Генетики, Физиологии И Защиты Растений Академии Наук Молдовы | 5,4-dimethylcampherol 3-O--D-(6′′-a′-L-rhamnopyranosyl)-glucopyranoside as compound increasing the seed productivity |
| RO125704B1 (en) * | 2009-03-30 | 2012-02-28 | Simona Elena Bişboacă | Process for obtaining polyphenols from marc |
| MD585Z (en) * | 2012-04-13 | 2013-08-31 | Государственный Медицинский И Фармацевтический Университет "Nicolae Testemitanu" Республики Молдова | Method for quantitative determination of flavonoids in egetable raw material |
| MD636Z (en) * | 2012-12-21 | 2013-12-31 | Институт Генетики, Физиологии И Защиты Растений Академии Наук Молдовы | Process for producing flavonoid glycosides from Linaria vulgaris Mill. |
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| Publication number | Publication date |
|---|---|
| MD825Y (en) | 2014-10-31 |
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| FG9Y | Short term patent issued | ||
| KA4Y | Short-term patent lapsed due to non-payment of fees (with right of restoration) | ||
| MM4A | Patent for invention definitely lapsed due to non-payment of fees |