CN100357251C - Technique for producing purple common perilla rosemary acid - Google Patents
Technique for producing purple common perilla rosemary acid Download PDFInfo
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- CN100357251C CN100357251C CNB200410075747XA CN200410075747A CN100357251C CN 100357251 C CN100357251 C CN 100357251C CN B200410075747X A CNB200410075747X A CN B200410075747XA CN 200410075747 A CN200410075747 A CN 200410075747A CN 100357251 C CN100357251 C CN 100357251C
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- rosmarinic acid
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Abstract
The present invention relates to a technique for producing perilla derived rosmarinic acids, which can realize industrialization large-scale production. Perilla leaves are used as the raw materials, soaked in acidic water, filtered and extracted. Macroporous adsorption resin columns on extract are absorbed and desorbed, and desorbed liquid is decompressed and vaporized to obtain rosmarinic acid products of which purity is 10%. Rosmarinic acid product solution of which purity is 10% is extracted by petroleum ether, and rosmarinic acid products of which purity is 50% are obtained through organic phase decompression, vaporization and concentration. Gradient elution is carried out for the adsorption resin columns on the rosmarinic acid products of which purity is 50% by etanol solution of different concentrations. Rosmarinic acid products of which purity is 95% are obtained by crystallizing the decompressed and condensed eluant with 95% of constituents. The present invention has the advantages of simple technology, easy operation, low production cost, multiple product specifications, high safety and reliability, and can be used in the technical fields of food additives, medicine intermediate, cosmetic additives, etc.
Description
Technical field:
But the present invention relates to a kind of technology of large-scale industrial production purple common perilla rosemary acid, belong to natural crops deep process technology field.
Technical background:
Rosmarinic acid (Rosmarinic acid is called for short RosA) is a kind of multi-functional phenolic acid compound, exists in the various plants of Labiatae, and it has multiple biological activity.Rosmarinic acid has the activity of extremely strong removing interior free yl as antioxidant, and its anti-oxidant activity is better than coffic acid, chlorogenic acid, folic acid, forulic acid, vitamin-E etc.; Rosmarinic acid can also suppress the oxidation of the low-density lipoprotein of endotheliocyte adjusting as antioxidant.Rosmarinic acid also has antiviral activity, and the pure water extract of discovery wood marchs such as Arda has the activity of anti-HIV, and the essential substance that wherein works is a rosmarinic acid; The research of Mazumder etc. shows that further rosmarinic acid can suppress the activity of HIV-1 (humanimmunodeficiency virus) intergrase; The research of Borkowski etc. shows that also rosmarinic acid is a kind of effective constituent of control simplexvirus, and its antiviral activity is except that the activity that suppresses virus some enzyme in life cycle, and it can also combine with virus capsid protein rapidly, thereby makes virally inactivated.In addition, rosmarinic acid also has otherwise function, and the extract that discoveries such as Lopes contain rosmarinic acid has good treatment effect to auditory disorder and hemorrhoid, and is free from side effects.Rosmarinic acid can suppress acute and chronic infection as the additive of makeup, and uvioresistant suppresses the degraded of elastin, increases cell membrane stability.Rosmarinic acid in the discovery reds sage root such as Zou Zhengwu also has the effect of antithrombotic and anti-platelet aggregation.The domestic and international at present research about rosmarinic acid has shown that it has important use and is worth in fields such as pharmacy, food, makeup, therefore many investigators are arranged all at chemosynthesis and the biosynthetic means of studying rosmarinic acid, but its method is loaded down with trivial details, the cost height is difficult to realize suitability for industrialized production.Also few to the research of extensive separating and purifying rosmarinic acid both at home and abroad now, therefore set up a kind of technology that can fast, simply produce rosmarinic acid and be necessary.
Summary of the invention:
Purpose of the present invention aims to provide a kind of technology that can the large-scale industrial production rosmarinic acid, this production technique is a raw material with natural phant purple perilla leaf, adopt acid extraction, absorption with macroporous adsorbent resin, wash-out, concentrate, steps such as extraction, crystallization, produce the rosmarinic acid of different purity, product safety is reliable, environmental protection can be widely used in various fields such as foodstuff additive, cosmetics additive and pharmaceutical.
In order to realize the foregoing invention purpose, concrete production technique of the present invention is as follows: (1) is soaked in the purple perilla leaf in the sour water, filters and extracts clear aqueous solution, and repeated multiple times is extracted, and with macroporous adsorptive resins absorption on the extracting solution, uses 95% alcohol desorb again; (2), obtain purity and be 10% rosmarinic acid product with the stripping liquid reduction vaporization; (3) with the rosmarinic acid product solution petroleum ether extraction of 10% purity, the organic phase reduction vaporization concentrates and obtains purity is 50% rosmarinic acid product; (4) with adsorption resin column on the rosmarinic acid product of 50% purity, use Different concentrations of alcohol solution gradient wash-out respectively, with 95% component elutriant concentrating under reduced pressure, crystallization under 4 ℃ of temperature condition obtains purity and is 95% rosmarinic acid product.
The outstanding advantage that the present invention compared with prior art has is: only promptly obtain purity by a cover technology and be respectively 10%, 50%, 95% rosmarinic acid, product specification is abundant, production technique is simple, and production cost is lower, is fit to realize the demand of large-scale industrial production.
Embodiment:
Below by embodiment production technique of the present invention is described further.
Embodiment 1:
The sour water of 20 kilograms of purple perilla leaves with pH2-4 extracted 4 hours under 40 ℃ of temperature condition, repeat to extract 3 times, XAD-4 macroporous adsorbent resin (10 * 80cm) on the united extraction liquid, use 95% alcohol desorb again, obtain 4 kilograms of stripping liquids, with stripping liquid concentrating under reduced pressure to 0.5 kilogram, promptly obtain purity and be 10% rosmarinic acid product; With the rosmarinic acid product petroleum ether extraction secondary of 200 grams, 10% purity, the organic phase reduction vaporization concentrates and to obtain 15 to restrain purity be 50% rosmarinic acid product; With AB-8 polymeric adsorbent (5 * 60cm) posts on the rosmarinic acid product of 4 grams, 50% purity, it with concentration respectively 30%, 95% ethanolic soln stepwise elution, with 95% component concentrating under reduced pressure to 3mL, crystallization under 4 ℃ of temperature condition, obtaining 1.9 gram purity is 95% rosmarinic acid product.
Embodiment 2:
The sour water of 300 kilograms of purple perilla leaves with pH2-4 extracted 4 hours under 40 ℃ of temperature condition, extract repeatedly 3 times, XAD-4 macroporous adsorptive resins (30 * 150cm) on the united extraction liquid, use 95% alcohol desorb again, obtain 40 kilograms of stripping liquids, with stripping liquid concentrating under reduced pressure to 3 kilogram, obtain purity and be 10% rosmarinic acid product; The rosmarinic acid of 2 kilogram of 10% purity with distilled water diluting to 5 kilogram, is used 2 kilograms of petroleum ether extractions three times respectively, merge organic phase, the organic phase reduction vaporization is concentrated to 0.38 kilogram, obtain purity and be 50% rosmarinic acid product; With AB-8 adsorption resin column on the rosmarinic acid of 100 grams, 50% purity, it with concentration respectively 30%, 95% ethanolic soln stepwise elution, again with 95% component elutriant concentrating under reduced pressure, crystallization under 4 ℃ of temperature condition obtains 45 gram purity and is 95% rosmarinic acid product.
Claims (1)
1, a kind of production technique of purple common perilla rosemary acid is characterized in that the purple perilla leaf is soaked in the sour water of pH2-4, filters and extracts clear aqueous solution, and repeated multiple times is extracted, and with XAD-4 macroporous adsorptive resins absorption on the extracting solution, uses the alcohol desorb again; With the stripping liquid reduction vaporization, obtain purity and be 10% rosmarinic acid product; With the rosmarinic acid product solution petroleum ether extraction of 10% purity, the organic phase reduction vaporization concentrates and to obtain purity is 50% rosmarinic acid product; With AB-8 adsorption resin column on the rosmarinic acid product of 50% purity, with concentration respectively 30%, 95% ethanolic soln gradient elution, with 95% component elutriant concentrating under reduced pressure, crystallization under 4 ℃ of temperature condition obtains purity and is 95% rosmarinic acid product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410075747XA CN100357251C (en) | 2004-12-23 | 2004-12-23 | Technique for producing purple common perilla rosemary acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410075747XA CN100357251C (en) | 2004-12-23 | 2004-12-23 | Technique for producing purple common perilla rosemary acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1796362A CN1796362A (en) | 2006-07-05 |
| CN100357251C true CN100357251C (en) | 2007-12-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB200410075747XA Expired - Fee Related CN100357251C (en) | 2004-12-23 | 2004-12-23 | Technique for producing purple common perilla rosemary acid |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186572B (en) * | 2007-12-19 | 2010-05-19 | 天津大学 | Method for separating and purifying salvianolic acid from red sage root liquid extract by one step |
| CN101401632B (en) * | 2008-04-14 | 2012-05-16 | 浙江工业大学 | Purple perilla flavoring liquid and method of preparing the same |
| CN102952018B (en) * | 2011-08-17 | 2014-08-27 | 湖北中烟工业有限责任公司 | Purification method of antioxidant rosmarinic acid for tobacco |
| CN102850219B (en) * | 2012-09-28 | 2014-06-18 | 中北大学 | Method for extracting rosmarinic acid from folia perillae acutae |
| CN103848740B (en) * | 2012-11-30 | 2015-12-09 | 沈阳药科大学 | A kind of method preparing rosmarinic acid from plant oil meal |
| CN103099845B (en) * | 2013-02-25 | 2015-03-11 | 中国农业科学院农业质量标准与检测技术研究所 | Method for extracting perillaseed hydrophilic chemical component from perillaseed oil residue |
| CN105315706B (en) * | 2015-12-11 | 2017-07-04 | 杨永 | A kind of natural pigment color stabilizer, preparation method and application |
| CN106565489A (en) * | 2016-10-10 | 2017-04-19 | 广西来宾绿翔生物科技有限公司 | Process for extracting rosmarinic acid from perilla |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1306815A (en) * | 2000-01-25 | 2001-08-08 | 殷芳 | Skin care cream with medical effect and its preparation |
| JP2001342489A (en) * | 2000-03-31 | 2001-12-14 | Sanei Gen Ffi Inc | Agent for suppressing deterioration of taste and flavor and method for suppressing deterioration of taste and flavor |
-
2004
- 2004-12-23 CN CNB200410075747XA patent/CN100357251C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1306815A (en) * | 2000-01-25 | 2001-08-08 | 殷芳 | Skin care cream with medical effect and its preparation |
| JP2001342489A (en) * | 2000-03-31 | 2001-12-14 | Sanei Gen Ffi Inc | Agent for suppressing deterioration of taste and flavor and method for suppressing deterioration of taste and flavor |
Non-Patent Citations (2)
| Title |
|---|
| 分光光度法测定苏叶中的迷迭香酸含量 杜桂彩等.青岛大学学报，第18卷第4期 2003 * |
| 紫苏愈伤组织迷迭香酸的纯化及抗菌活性研究 李荣贵等.微生物学报，第27卷第5期 2000 * |
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| Publication number | Publication date |
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| CN1796362A (en) | 2006-07-05 |
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Application publication date: 20060705 Assignee: Shandong Tianyin Biotechnology Co., Ltd. Assignor: Qingdao University Contract record no.: 2010370000088 Denomination of invention: Technique for producing purple common perilla rosemary acid Granted publication date: 20071226 License type: Exclusive License Record date: 20100319 |
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Granted publication date: 20071226 Termination date: 20101223 |