CN1313460C - Method for extracting anthocyanidin - Google Patents
Method for extracting anthocyanidin Download PDFInfo
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- CN1313460C CN1313460C CNB2004100732716A CN200410073271A CN1313460C CN 1313460 C CN1313460 C CN 1313460C CN B2004100732716 A CNB2004100732716 A CN B2004100732716A CN 200410073271 A CN200410073271 A CN 200410073271A CN 1313460 C CN1313460 C CN 1313460C
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Abstract
The present invention relates to a preparation method of anthocyanidin, particularly to a method for extracting anthocyanidin in grape seeds by making use of macroporous resin. The present invention is characterized in that the method adopts grapes as raw materials; after the grapes are extracted with organic solvent, crude extract is obtained; the crude extract uses water solvent as a mobile phase; anthocyanidin is obtained by eluent through drying after separation on columns by macroporous resin. The method has the following extraction process: the pulverized grape seeds are extracted by 60 to 90%organic solvent; at the temperature less than 80 to 85 DEG C, after extracting liquid is decompressed and evaporated at the vacuum degree of 0.06 to 0.09MPA, crude extract is obtained; after the crude extract is dissolved by dissolving agents, the chromatographic separation of the crude extract is carried out by macroporous absorption resin; the ratio of the resin to raw materials is 1:1 to 3, and eluent is adopted for elution. The method for extracting anthocyanidin has the characteristics of high extraction rate of anthocyanidin, favorable product shade, simple operation and low production cost.
Description
Affiliated technical field: the present invention relates to a kind of preparation method of cyanidin(e), particularly about utilizing the method for anthocyanidin in the macroporous resin extraction Semen Vitis viniferae.
Background technology: anthocyanidin or cyanidin(e) (Proanthocyanidins) belong to condensed tannin class material, are to be linked with C-C and the class polyphenolic substance (polyphenols) that forms by hydroxyflavan compounds.The existing preparation technology of cyanidin(e) is: water, Diluted Alcohol, rare acetone extraction, and extracting solution concentrating under reduced pressure, filtration or centrifugal except that obtaining the aqueous solution behind the insoluble impurity that anhydrates, this aqueous solution needs refining because of containing a large amount of water-soluble impurities.The further refining general solvent extration that adopts, the concentrating under reduced pressure convection drying obtains product then.Among the above-mentioned preparation technology, refining use solvent extraction, has following shortcoming: (1) cyanidin(e) with the immiscible solvent of water in solubleness lower, so the yield of this process for purification is extremely low: (2) solvent-oil ratio is big, the cost height: (3) grasp do loaded down with trivial details; (4) because the dissolving properties of impurity dissolving properties and effective ingredient is more close, so be difficult for eliminating, make it product color and flowability does not reach standard.
Summary of the invention: the purpose of this invention is to provide a kind of method of extracting anthocyanidin, it has anthocyanidin extraction yield height, product color is good, the simple to operate and low characteristics of production cost.
Technical scheme of the present invention is: design a kind of method of extracting anthocyanidin, it is characterized in that: it adopts grape is raw material, with getting crude extract behind the organic solvent extraction; Crude extract is done moving phase with water solvent, separates through macroporous resin column, and elutriant drying process gets anthocyanidin.
Concrete extraction process is: with the Semen Vitis viniferae the pulverized organic solvent extraction through 60-90%, be not higher than under 80-85 ℃ the condition, extracting solution reduction vaporization under vacuum tightness 0.06-0.09MPA gets crude extract; Crude extract separates portions of resin raw material=1: 1-3 again through macroporous adsorption resin chromatography after the solvating agent dissolving; Adopt the elutriant wash-out.
Described organic solvent is ethanol, acetone, methyl alcohol, propyl alcohol, Virahol, ethyl acetate.
The water solvent of described crude extract is methyl alcohol, ethanol, acetone, Virahol, water.
Described upper column quantity is portions of resin sample=1: 1-3 (W/W).
Described upper prop rate of adsorption is 2.5L/ hour-5.5L/ hour, and elution speed is 4.0L/ hour-8.0L/ hour.
Described elutriant is sherwood oil, ethanol, acetone, water solvent.
The present invention has following characteristics:
1. constant product quality, product purification degree height is removed most impurity.
2. after handling through macroporous adsorbent resin, can effectively remove its moisture absorption products, increase the stability of product.
3. after macroporous resin treatment, can effectively remove heavy metal, guarantee its quality product.
Technical process of the present invention is simple, be easy to control, can carry out normalizing operation, anthocyanidin extraction yield height, simple to operate, production cost is low.
Embodiment: the present invention is raw material with the Semen Vitis viniferae, through preparation, macroporous resin absorption, the wash-out of the pulverizing, the anthocyanidin crude extract that comprise Semen Vitis viniferae, concentrate, dry purity is 95% product, product yield 4-6%: after the preparation of its anthocyanidin crude extract is the organic agent extraction of Semen Vitis viniferae with 60%-90% that will pulverize, be not higher than under 80-85 ℃ the condition, extracting solution reduction vaporization under vacuum tightness 0.06-0.09MPa gets the crude extract concentrated solution.Add the precipitation agent of 40-70mL by the 10mL concentrated solution, place after-filtration, crude extract.Crude extract is mixed with the solution of 5%-40% concentration with lysate and by macroporous resin: the amount upper prop of raw material=1: 1-3 (W/W).Adopt the elutriant wash-out, the post rate of adsorption is 2.5L/ hour-5.5L/ hour, and elution speed is 4.0L/ hour-8.0L/ hour, (concrete produce and equipment is pressed the chemical standard execution).
Embodiment 1: the ethanol 3000ml with 75% extracts the Semen Vitis viniferae 500g that pulverizes, and then merge behind 75% the extraction using alcohol with 2500ml, be not higher than under 80-85 ℃ the condition, reduction vaporization reclaims solvent and gets medicinal extract under vacuum tightness 0.06MPa, in medicinal extract, add 2000ml water then, centrifugation gets supernatant liquor: be washed with distilled water to no ethanol, the adsorption column of packing into, watering balance after 1500 gram DM130 resins are fully soaked swelling with ethanol; Supernatant liquor added adsorption rate is 2.5L/ hour in the adsorption column; The distilled water flushing adsorption column is used in the absorption back that finishes, and 50% ethanol elution analyses that to take off speed be 4.5L/ hour; The concentrating under reduced pressure ethanol eluate gets medicinal extract, and dry that product yield is 22.6g, content is 96.3%
Embodiment 2: the methyl alcohol 6000ml with 78% extracts the Semen Vitis viniferae 1000g that pulverizes, and then merge behind 75% the extraction using alcohol with 6000ml, reduction vaporization reclaims solvent and gets medicinal extract under vacuum tightness 0.09MPa, adds 4800ml water then in medicinal extract, and centrifugation gets supernatant liquor; Be washed with distilled water to no ethanol, the adsorption column of packing into, watering balance after 1500 gram H-107 resins are fully soaked swelling with ethanol; Supernatant liquor added adsorption rate is 3.5L/ hour in the adsorption column; The distilled water flushing adsorption column is used in the absorption back that finishes, and 70% ethanol elution analyses that to take off speed be 6.5L/ hour; The concentrating under reduced pressure ethanol eluate gets medicinal extract, and dry that product yield is 58.7g, content is 95.4%.
Claims (1)
1, a kind of method of extracting anthocyanidin, it is characterized in that: the ethanol 3000ml with 75% extracts the Semen Vitis viniferae 500g that pulverizes, and then merge behind 75% the extraction using alcohol with 2500ml, be not higher than under 80-85 ℃ the condition, reduction vaporization reclaims solvent and gets medicinal extract under vacuum tightness 0.06MPa, add 2000ml water then in medicinal extract, centrifugation gets supernatant liquor; Be washed with distilled water to no ethanol, the adsorption column of packing into, watering balance after 1500 gram DM130 resins are fully soaked swelling with ethanol; Supernatant liquor added adsorption rate is 2.5L/ hour in the adsorption column; The distilled water flushing adsorption column is used in the absorption back that finishes, and 50% ethanol elution analyses that to take off speed be 4.5L/ hour; The concentrating under reduced pressure ethanol eluate gets medicinal extract, and dry that product yield is 22.6g, content is 96.3%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100732716A CN1313460C (en) | 2004-11-15 | 2004-11-15 | Method for extracting anthocyanidin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100732716A CN1313460C (en) | 2004-11-15 | 2004-11-15 | Method for extracting anthocyanidin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1634915A CN1634915A (en) | 2005-07-06 |
| CN1313460C true CN1313460C (en) | 2007-05-02 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100732716A Expired - Fee Related CN1313460C (en) | 2004-11-15 | 2004-11-15 | Method for extracting anthocyanidin |
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| CN (1) | CN1313460C (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101703635B (en) * | 2009-12-03 | 2012-08-08 | 应维强 | Production technology of grape pip and grape skin extract |
| CN101948628B (en) * | 2010-09-03 | 2013-03-27 | 河北食品添加剂有限公司 | Method for preparing high-purity norbixin |
| CN102229633B (en) * | 2011-05-31 | 2014-01-08 | 江南大学 | Method for separating and preparing five high-purity anthocyanidin monomers from grape skins |
| CN102277008B (en) * | 2011-06-28 | 2013-09-04 | 安徽省科学技术研究院 | Extraction and preparation method of natural Fragaria ananassa Duch haematochrome |
| CN102942549B (en) * | 2012-11-27 | 2015-06-03 | 长沙哈根生物科技有限公司 | Method for extracting blueberry anthocyanin |
| CN103145681B (en) * | 2013-03-15 | 2015-01-28 | 中国农业科学院农产品加工研究所 | Method for extracting anthocyanin |
| CN104496957A (en) * | 2014-12-01 | 2015-04-08 | 成都红柿子科技有限公司 | Method for extracting procyanidine from grape skins |
| CN105136546B (en) * | 2015-10-22 | 2018-03-20 | 国家林业局泡桐研究开发中心 | A kind of red-leaf plants prevent the paraffin section method that blade anthocyanin is lost in |
| CN105777696B (en) * | 2016-04-06 | 2020-11-13 | 华南理工大学 | Method for extracting anthocyanin by using deep eutectic solvent |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1506362A (en) * | 2002-12-06 | 2004-06-23 | 沈阳中科药业公司 | Resin process of extracting proanthocyanidin from graup seed |
| CN1603320A (en) * | 2004-07-23 | 2005-04-06 | 浙江大学 | Method for preparing high content proanthocyanidin |
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2004
- 2004-11-15 CN CNB2004100732716A patent/CN1313460C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1506362A (en) * | 2002-12-06 | 2004-06-23 | 沈阳中科药业公司 | Resin process of extracting proanthocyanidin from graup seed |
| CN1603320A (en) * | 2004-07-23 | 2005-04-06 | 浙江大学 | Method for preparing high content proanthocyanidin |
Non-Patent Citations (1)
| Title |
|---|
| 葡萄籽中原花青素提取方法的进一步研究 樊丽华，新疆大学学报，第21卷第1期 2004 * |
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| CN1634915A (en) | 2005-07-06 |
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Effective date of registration: 20090703 Address after: Huahai Industrial Park, No. 21 solidarity South Road, hi tech Zone, Shaanxi, Xi'an: 710075 Co-patentee after: Jilin Hao Tian Bioengineering Technology Co., Ltd. Patentee after: Xi'an Hao Tian Bioengineering Technology Co., Ltd. Address before: Shaanxi province Xi'an city high tech Development Zone of High Road No. 36 layer zip code: 710075 Patentee before: Xi'an Haotian Bioengineering Tech. Co., Ltd. |
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