CN105232803A - Method for producing grape seed extract with low pesticide residues and high (-)-epicatechin 3-O-gallate ester content - Google Patents
Method for producing grape seed extract with low pesticide residues and high (-)-epicatechin 3-O-gallate ester content Download PDFInfo
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- CN105232803A CN105232803A CN201510756610.9A CN201510756610A CN105232803A CN 105232803 A CN105232803 A CN 105232803A CN 201510756610 A CN201510756610 A CN 201510756610A CN 105232803 A CN105232803 A CN 105232803A
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- vitis viniferae
- semen vitis
- epicatechin
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Abstract
The invention discloses a method for extracting grape seed extract with low pesticide residues and high (-)-epicatechin 3-O-gallate ester content from grape seeds. The method comprises the following steps that 1, grape seeds which are not smashed are put in n-hexane, sodium chloride is added, and stirring is conducted; 2, the n-hexane is discharged, deionized water is added, stirring is conducted, and heating extraction is conducted; 3, an extracting solution is sent to a macroporous resin and polyamide mixed chromatographic column, and elution, separation and purification are conducted. The extracted grape seed extract is natural extract and has the advantages of being high in polyphenol content, low in pesticide residue and high in (-)-epicatechin 3-O-gallate ester content, and the grape seed extract can be used for foods and health-care products.
Description
Technical field
The invention belongs to the method for extraction and purification of grape seed polyphenols, particularly one extracts the method for the grape seed polyphenols of the residual height () of low agriculture-epicatechin 3-O-gallic acid ester content from Semen Vitis viniferae.
Background technology
20 century 70s, French scientist finds that Semen Vitis viniferae contains abundant procyanidin, procyanidin is a kind of polyphenol substance, research finds, this polyphenol substance of procyanidin has strong anti-oxidation, and its non-oxidizability is ascorbic 20 times, 50 times of vitamin E, especially its activity in vivo, other antioxidants are incomparable especially.Present experimental applications proves, OPC can antiallergic, improve blood vessel intensity and permeability, to nearly 70 various diseases, there is direct or indirect preventive and therapeutic action.
()-epicatechin 3-O-epicatechol gallate, white crystals, molecular formula: C
22h
18o
10, molecular weight: 442.37, dissolves in hot water, ethanol, is insoluble to benzene, chloroform and petroleum ether.Modern study shows, ()-epicatechin 3-O-epicatechol gallate has the effects such as antioxidation, anti-inflammation, anticancer propagation, prevention and cure of cardiovascular disease.
Although Semen Vitis viniferae is wrapped in Fructus Vitis viniferae inside, but the pesticide sprayed during plantation Fructus Vitis viniferae, by absorption and the liquid circulation of grapevine seedling, still can remain in Semen Vitis viniferae, 530 residual discoveries of agriculture are detected, no matter be all residual several or tens kinds of pesticide in import or domestic Semen Vitis viniferae according to EN15662 and EN12393 method.And American-European, Japan and other countries all proposes more and more higher requirement to the pesticide residues of import Semen Vitis viniferae extract.
By contrast test discovery repeatedly, only use hexane agriculture residual, can't make that the agriculture in the Semen Vitis viniferae extract obtained is residual is all less than quantitative limit, and assist eluting by adding sodium chloride, make 530 the residual content of agriculture detected according to EN15662 and EN12393 method all be less than quantitative limit.Such as: do not add sodium chloride eluting, CGA-173506 content: 0.05mg/kg, dimethomorph content: 0.03mg/kg; And add sodium chloride and assist eluting, CGA-173506 content <0.01mg/kg, dimethomorph <0.01mg/kg, eluting rate improves 3 ~ 5 times respectively.
No. 28 macroporous resins, it is the special macroporous resin of purification grape seed polyphenols, found by contrast test, No. 28 macroporous resin column, ethanol elution technique is put on by light water, Semen Vitis viniferae extract polyphenol content after just can making purification reaches more than 80%, and wherein ()-epicatechin 3-O-gallic acid ester content less than 10%; And according to the present invention, while residual by initial stage hexane agriculture, wash away most of liposoluble substance, later stage carries out purification by the hybrid resin of No. 28 macroporous resins and polyamide, not only make the Semen Vitis viniferae extract polyphenol content obtained reach 90% and more than, simultaneously also make ()-epicatechin 3-O-gallic acid ester content exceed 25%.
Summary of the invention
The object of the invention is to make full use of the natural resources, meet both at home and abroad to the residual more and more higher requirement of Semen Vitis viniferae extract agriculture, a kind of method of producing the Semen Vitis viniferae extract of low agriculture residual height ()-epicatechin 3-O-gallic acid ester content is provided.
Technical scheme of the present invention is summarized as follows.
A kind of method of producing the Semen Vitis viniferae extract of low agriculture residual height ()-epicatechin 3-O-gallic acid ester content, comprises the steps:
(1) by Semen Vitis viniferae, add with in the water saturated normal hexane of deionization, quality (kg) volume ratio (L) of Semen Vitis viniferae and normal hexane is 1:3, then sodium chloride is added, quality (kg) volume ratio (L) of sodium chloride and normal hexane is 1:200, stirs eluting 30 minutes, crosses and filters to remove normal hexane;
(2) in Semen Vitis viniferae, add deionized water, quality (kg) volume ratio (L) of Semen Vitis viniferae and deionized water is 1:3 ~ 5, extracts 40 minutes at 100 DEG C, filters, obtains Semen Vitis viniferae crude extract;
(3) by hybrid resin post on gained extracting solution, with the concentration expressed in percentage by volume of 4 ~ 8 times of column volume deionized waters, 1 times of column volume be 20% ethanol water, the concentration expressed in percentage by volume of 2 times of column volumes is 40% ethanol water, the percentage concentration of 2 times of column volumes is that 95% ethanol water carries out eluting, collecting merging percentage concentration is 40% ethanol water and 95% ethanol water eluting liquid, be evaporated to pol 40%, spraying dry, obtains Semen Vitis viniferae extract.Described hybrid resin is polyamide and No. 28 macroporous resins two kinds of resins the mixing of 1:1 in mass ratio.
Described Semen Vitis viniferae is pulverize without any mode or the whole grape seed of fragmentation.
Use the Semen Vitis viniferae extract that the present invention produces, not only ()-epicatechin 3-O-gallic acid ester content is more than 25%, polyphenol content more than 90%, and makes 530 the residual content of agriculture detected according to EN15662 and EN12393 method all be less than quantitative limit.
Detailed description of the invention
Below by specific embodiment, the present invention is described, description is below only to make those skilled in the art understand the present invention better, but does not limit the present invention in any way.
Embodiment 1
A kind of method of producing the Semen Vitis viniferae extract of low agriculture residual height ()-epicatechin 3-O-gallic acid ester content, comprises the steps:
(1) by Semen Vitis viniferae, add with in the water saturated normal hexane of deionization, quality (kg) volume ratio (L) of Semen Vitis viniferae and normal hexane is 1:3, then sodium chloride is added, quality (kg) volume ratio (L) of sodium chloride and normal hexane is 1:200, stirs eluting 30 minutes, crosses and filters to remove normal hexane;
(2) in Semen Vitis viniferae, add deionized water, quality (kg) volume ratio (L) of Semen Vitis viniferae and deionized water is 1:3, extracts 40 minutes at 100 DEG C, filters, obtains Semen Vitis viniferae crude extract;
(3) by hybrid resin post on gained extracting solution, hybrid resin is that No. 28 macroporous resins of 1:1 and the hybrid resin of 30-60 order polyamide form by mass ratio, with the concentration expressed in percentage by volume of 4 times of column volume deionized waters, 1 times of column volume be 20% ethanol water, the concentration expressed in percentage by volume of 2 times of column volumes is 40% ethanol water, the percentage concentration of 2 times of column volumes is that 95% ethanol water carries out eluting, collecting merging percentage concentration is 40% ethanol water and 95% ethanol water eluting liquid, be evaporated to pol 40%, spraying dry, obtains Semen Vitis viniferae extract.()-epicatechin 3-O-gallic acid ester content 28.9%, polyphenol content 92.7%, makes 530 the residual content of agriculture detected according to EN15662 and EN12393 method all be less than quantitative limit.
Embodiment 2
A kind of method of producing the Semen Vitis viniferae extract of low agriculture residual height ()-epicatechin 3-O-gallic acid ester content, comprises the steps:
(1) by Semen Vitis viniferae, add with in the water saturated normal hexane of deionization, quality (kg) volume ratio (L) of Semen Vitis viniferae and normal hexane is 1:3, then sodium chloride is added, quality (kg) volume ratio (L) of sodium chloride and normal hexane is 1:200, stirs eluting 30 minutes, crosses and filters to remove normal hexane;
(2) in Semen Vitis viniferae, add deionized water, quality (kg) volume ratio (L) of Semen Vitis viniferae and deionized water is 1:5, extracts 40 minutes at 100 DEG C, filters, obtains Semen Vitis viniferae crude extract;
(3) by hybrid resin post on gained extracting solution, hybrid resin is that No. 28 macroporous resins of 1:1 and the hybrid resin of 30-60 order polyamide form by mass ratio, with the concentration expressed in percentage by volume of 8 times of column volume deionized waters, 1 times of column volume be 20% ethanol water, the concentration expressed in percentage by volume of 2 times of column volumes is 40% ethanol water, the percentage concentration of 2 times of column volumes is that 95% ethanol water carries out eluting, collecting merging percentage concentration is 40% ethanol water and 95% ethanol water eluting liquid, be evaporated to pol 40%, spraying dry, obtains Semen Vitis viniferae extract.()-epicatechin 3-O-gallic acid ester content 31.2%, polyphenol content 96.3%, makes 530 the residual content of agriculture detected according to EN15662 and EN12393 method all be less than quantitative limit.
Embodiment 3
A kind of method of producing the Semen Vitis viniferae extract of low agriculture residual height ()-epicatechin 3-O-gallic acid ester content, comprises the steps:
(1) by Semen Vitis viniferae, add with in the water saturated normal hexane of deionization, quality (kg) volume ratio (L) of Semen Vitis viniferae and normal hexane is 1:3, then sodium chloride is added, quality (kg) volume ratio (L) of sodium chloride and normal hexane is 1:200, stirs eluting 30 minutes, crosses and filters to remove normal hexane;
(2) in Semen Vitis viniferae, add deionized water, quality (kg) volume ratio (L) of Semen Vitis viniferae and deionized water is 1:4, extracts 40 minutes at 100 DEG C, filters, obtains Semen Vitis viniferae crude extract;
(3) by hybrid resin post on gained extracting solution, hybrid resin is that No. 28 macroporous resins of 1:1 and the hybrid resin of 30-60 order polyamide form by mass ratio, with the concentration expressed in percentage by volume of 6 times of column volume deionized waters, 1 times of column volume be 20% ethanol water, the concentration expressed in percentage by volume of 2 times of column volumes is 40% ethanol water, the percentage concentration of 2 times of column volumes is that 95% ethanol water carries out eluting, collecting merging percentage concentration is 40% ethanol water and 95% ethanol water eluting liquid, be evaporated to pol 40%, spraying dry, obtains Semen Vitis viniferae extract.()-epicatechin 3-O-gallic acid ester content 29.5%, polyphenol content 94.8%, makes 530 the residual content of agriculture detected according to EN15662 and EN12393 method all be less than quantitative limit.
Claims (2)
1. produce a method for the Semen Vitis viniferae extract of low agriculture residual height ()-epicatechin 3-O-gallic acid ester content, it is characterized in that comprising the steps:
(1) by Semen Vitis viniferae, add with in the water saturated normal hexane of deionization, quality (kg) volume ratio (L) of Semen Vitis viniferae and normal hexane is 1:3, then sodium chloride is added, quality (kg) volume ratio (L) of sodium chloride and normal hexane is 1:200, stirs eluting 30 minutes, crosses and filters to remove normal hexane;
(2) in Semen Vitis viniferae, add deionized water, quality (kg) volume ratio (L) of Semen Vitis viniferae and deionized water is 1:3 ~ 5, extracts 40 minutes at 100 DEG C, filters, obtains Semen Vitis viniferae crude extract;
(3) by hybrid resin post on gained extracting solution, with the concentration expressed in percentage by volume of 4 ~ 8 times of column volume deionized waters, 1 times of column volume be 20% ethanol water, the concentration expressed in percentage by volume of 2 times of column volumes is 40% ethanol water, the percentage concentration of 2 times of column volumes is that 95% ethanol water carries out eluting, collecting merging percentage concentration is 40% ethanol water and 95% ethanol water eluting liquid, be evaporated to pol 40%, spraying dry, obtains Semen Vitis viniferae extract; Described hybrid resin is polyamide and No. 28 macroporous resins two kinds of resins the mixing of 1:1 in mass ratio.
2. produce the method for the Semen Vitis viniferae extract of low agriculture residual height ()-epicatechin 3-O-gallic acid ester content according to claim 1 one kind, it is characterized in that described Semen Vitis viniferae is pulverize without any mode or the whole grape seed of fragmentation.
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| CN201510756610.9A CN105232803A (en) | 2015-11-10 | 2015-11-10 | Method for producing grape seed extract with low pesticide residues and high (-)-epicatechin 3-O-gallate ester content |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110981924A (en) * | 2019-12-26 | 2020-04-10 | 天津市尖峰天然产物研究开发有限公司 | Method for preparing Luoshen from rhodiola rosea |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101125844A (en) * | 2007-09-28 | 2008-02-20 | 天津市尖峰天然产物研究开发有限公司 | Method for extracting procyanidins B2 |
| CN101669979A (en) * | 2009-10-09 | 2010-03-17 | 新疆维吾尔自治区药物研究所 | Artemisia scoparia extractive and production method and applications thereof |
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- 2015-11-10 CN CN201510756610.9A patent/CN105232803A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101125844A (en) * | 2007-09-28 | 2008-02-20 | 天津市尖峰天然产物研究开发有限公司 | Method for extracting procyanidins B2 |
| CN101669979A (en) * | 2009-10-09 | 2010-03-17 | 新疆维吾尔自治区药物研究所 | Artemisia scoparia extractive and production method and applications thereof |
Non-Patent Citations (2)
| Title |
|---|
| 冯建光、陈利琼: "葡萄籽提取物中原花青素的测定", 《中国食品添加剂》 * |
| 史国富、王新瑞: "天然高效抗氧化剂原花青素提取工艺研究概况", 《中国药物与临床》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110981924A (en) * | 2019-12-26 | 2020-04-10 | 天津市尖峰天然产物研究开发有限公司 | Method for preparing Luoshen from rhodiola rosea |
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