CN101215307B - Method for preparing hydroxyl carthamus tinctorius yellow color A - Google Patents
Method for preparing hydroxyl carthamus tinctorius yellow color A Download PDFInfo
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Abstract
A process for preparing hydroxyl carthamus tinctorius yellow color A comprises using dry carthanus tinctorius as raw material, using deionized water and water alcohol as extracting solution, passing through preliminary separating column and refining column, using deionized water and water alcohol as eluent, and then obtaining hydroxyl carthamus tinctorius yellow color A after frozen and dried, and the content can reach 85%-99%. The invention uses cheap material, no toxic and safe solution, and has simple technology, high carthamus tinctorius usage and low cost, which is suitable to the industrialized industry, and the extracting rate is 0.8%-1.5% according to different purify requests of hydroxyl carthamus tinctorius yellow color A for various applications.
Description
Technical field:
The present invention relates to the method for extracting effective components from medicinal plant, specifically is a kind of preparation method of hydroxyl radical carthamin yellow carthamus A.
Background technology:
Safflower (Catthamus tinctotins L.) is a composite family annual herb plant, in China cultivation and the medication history in existing more than 2100 year.Its dry tubiform floret is a conventional Chinese medicine simply, has effect promoting blood circulation and removing obstruction in channels, stasis-dispelling and pain-killing.Be commonly used to treat metremia clinically, disease such as cardiovascular, thrombosis is also made pain relieving, antiphlogistic.Hydroxyl yellow pigment A is one of safflower effective ingredients that gets the nod at present, and pharmacological evaluation proof hydroxyl radical carthamin yellow carthamus A can obviously improve anoxia endurance, makes coronary dilation, increases coronary flow, and the effect of obvious inhibition ADP inductive rabbit platelet aggregation is arranged.
Hydroxyl radical carthamin yellow carthamus A is mainly as lyophilized injectable powder.The extraction purifying of hydroxyl radical carthamin yellow carthamus A, the subject matter that needs at present to solve is effectively to remove impurity, improves the content of hydroxyl radical carthamin yellow carthamus A, reduces production costs.Current, work to the research of the process for refining of hydroxyl radical carthamin yellow carthamus A (HSYA) both at home and abroad mainly contains: 1. Meselhy (Chem Phar-m.Bull..1993 in 1993,41 (10): 1796-1802) reported and pass through acetone extraction, the ethyl acetate precipitation is passed through the method that fibre columns SephadexLH-20 gel chromatographic columns prepares hydroxyl radical carthamin yellow carthamus A repeatedly then.When gel chromatographic columns separated, another safflower phenyl styryl ketone composition and HSYA mixed, and needed to make with extra care preparation HSYA with preparation type polymeric amide thin layer plate, and this method is not suitable for suitability for industrialized production.2. Li Sheng in 2004 learn (application number: CN02132781.5) Flos Carthami extract is carried out column chromatography, alcohol precipitation, carry out again afterwards 3-5 time repeatedly column chromatography make with extra care, lyophilize obtains the hydroxyl radical carthamin yellow carthamus A dry powder of 90%-99%.This technology need be carried out chromatography repeatedly, and what select for use in treating process is that the dextrane gel of price comparison costliness is as filler.3. reports such as 2004 Jin Ming (herbal medicine, 2004,35 (1) 25-28) are with impurity such as D-4020 type non-polar macroporous resin post water elution carbohydrates, with 30% and 10% ethanol elution respectively SY and HSYA; Contained SY and HSYA purity are respectively 92.4% and 83.0% in two elutriants.
Summary of the invention
The purpose of this invention is to provide that a kind of production cost is low, technology is simple, pollution-free, yield is high, purity is high, be fit to the preparation method of the yellow A of hydroxyl safflower of suitability for industrialized production.
The preparation method of the yellow A of a kind of hydroxyl safflower provided by the invention comprises the steps:
(1) extract: get dry safflower, the deionized water extraction twice with 20～40 times of safflower weight extracts 30～90min at every turn, extract 40 ℃～90 ℃ of temperature, twice gained extracting solution merged, filter, remove the dregs of a decoction, 60 ℃ are evaporated to proportion is 1.05～1.15 water extract;
(2) separate: above-mentioned water extract is with macroporous adsorbent resin or hydrogen bonding type column chromatography material column chromatography, applied sample amount is 1: 1～3 (w/w), earlier with 2～4 column volumes of water wash, be 1～5 column volume of 10%～60% aqueous ethanolic solution drip washing with concentration again, collect pure water wash liquid, 60 ℃ be evaporated to proportion be 1.05～1.15 the initial gross separation concentrated solution;
(3) refining: with above-mentioned initial gross separation concentrated solution with nonpolar reversed phase chromatography material column chromatography, applied sample amount is 0.5～2: 1 (w/w), be 2～4 column volumes of 0%～10% aqueous ethanolic solution drip washing with concentration earlier, be 2～5 column volumes of 10%～70% aqueous ethanolic solution drip washing with concentration again, collect pure water wash liquid, 60 ℃ are evaporated to proportion is 1.05～1.2 must make with extra care concentrated solution;
(4) lyophilize: above-mentioned refining concentrated solution gets safran hydroxyl radical carthamin yellow carthamus A product through lyophilize.
Measure the content of the hydroxyl radical carthamin yellow carthamus A of above-mentioned products obtained therefrom with HPLC, can reach 85%～99.9%.
Macroporous adsorbent resin in the described step (2) can be AB-8 or H103; Hydrogen bonding type column chromatography material can be a polymeric amide.A large amount of impurity can be effectively removed in initial gross separation, lay the foundation for next step column chromatography obtains high purity product.
Nonpolar reversed phase chromatography material in the described step (3) can be selected MDS for use; The renewable recycling of MDS is as making material regeneration with 95% ethanol drip washing cylinder.
Hydroxyl radical carthamin yellow carthamus A content assaying method of the present invention is measured (pressing external standard method) with HPLC.The HPLC chromatographic condition is: moving phase: methyl alcohol: the second eyeball: 0.25% phosphoric acid=33.5: 0.7: 65.8; Chromatographic column: Hypersil C
18(4.0 * 250mm); Column temperature: 25 ℃; Flow velocity: 1.0mL/min; Measure wavelength: 402nm, the 10u1 sample introduction.
Compared with prior art the present invention has following advantage:
(1) process for refining of the present invention is simple, the extraction efficiency height.By the requirement of the different purposes of hydroxyl radical carthamin yellow carthamus A to purity, purity can reach 85%～99.9%, and extraction yield can reach 0.8%～1.5%.
(2) the present invention uses solvent safety nontoxic, cheap recyclable usefulness again, environmentally safe;
(3) the present invention uses the separation and purification material cheap, and is easy to wash-out regeneration, can repeatedly utilize;
In a word, the preparation method of hydroxyl radical carthamin yellow carthamus A of the present invention, not only production cost is low, technology is simple, pollution-free, and the yield height of gained hydroxyl radical carthamin yellow carthamus A, purity height, is fit to suitability for industrialized production.
Embodiment:
Embodiment 1
Get the dry safflower of 0.4Kg,, extract 60 ℃ of temperature with 12Kg deionized water extraction twice, extraction time 45min, united extraction liquid filters, and it is 1.10 water extract that 60 ℃ of filtrates are evaporated to about proportion; Polyamide column separates (blade diameter length ratio is 1: 20) on the water extract, and applied sample amount is 1: 3.Earlier, use 4 column volumes of 50% ethanol drip washing again, collect leacheate with 3 column volumes of deionized water drip washing, 60 ℃ be evaporated to proportion be 1.05 the initial gross separation concentrated solution; Initial gross separation concentrated solution upper prop MDS-5 (blade diameter length ratio is 1: 10), applied sample amount is 0.5: 1, earlier with 2 column volumes of 10% ethanol drip washing, uses 4 column volumes of 20% ethanol drip washing again, collects 20% pure leacheate.(developping agent is an ethyl acetate: methyl alcohol: 3.6% hydrochloric acid=1: 3: 6) in the thin-layer chromatography detection, merge the leacheate that contains the single spot of hydroxyl radical carthamin yellow carthamus A, 60 ℃ are evaporated to proportion is 1.16, and lyophilize promptly gets safran hydroxyl radical carthamin yellow carthamus A product.With the hydroxyl radical carthamin yellow carthamus A is reference substance, and the content that records hydroxyl radical carthamin yellow carthamus A with HPLC is 99.9%, and yield is 0.8%.
Embodiment 2
Get the dry safflower of 0.4Kg,, extract 80 ℃ of temperature with 15Kg deionized water extraction twice, extraction time 60min, united extraction liquid filters, and it is 1.05 water extract that 60 ℃ of filtrates are evaporated to about proportion; The AB-8 post separates (blade diameter length ratio is 1: 20) on the water extract, and applied sample amount is 1: 2.Earlier, use 4 column volumes of 30% ethanol drip washing again, collect leacheate with 2 column volumes of deionized water drip washing, 60 ℃ be evaporated to proportion be 1.10 the initial gross separation concentrated solution; Initial gross separation concentrated solution upper prop MDS-5 (blade diameter length ratio is 1: 10), applied sample amount is 1: 1, earlier with 3 column volumes of deionized water drip washing, use 4 column volumes of 30% ethanol drip washing again, collect 30% pure leacheate, thin-layer chromatography detects, and merges the leacheate that contains the hydroxyl radical carthamin yellow carthamus A spot, 60 ℃ are evaporated to proportion is 1.10, and lyophilize promptly gets safran hydroxyl radical carthamin yellow carthamus A product.With the hydroxyl radical carthamin yellow carthamus A is reference substance, and the content that records hydroxyl radical carthamin yellow carthamus A with HPLC is 92.%, and yield is 1.2%.
Embodiment 3
Get the dry safflower of 1Kg,, extract 70 ℃ of temperature with 30Kg deionized water extraction twice, extraction time 80min, united extraction liquid filters, and it is 1.12 water extract that 60 ℃ of filtrates are evaporated to about proportion; The H103 post separates (blade diameter length ratio is 1: 20) on the water extract, and applied sample amount is 1: 3.Earlier, use 4 column volumes of 40% ethanol drip washing again, collect leacheate with 4 column volumes of deionized water drip washing, 60 ℃ be evaporated to proportion be 1.10 the initial gross separation concentrated solution; Initial gross separation concentrated solution upper prop MDS-5 (blade diameter length ratio is 1: 10), applied sample amount is 2: 1, earlier with 3 column volumes of deionized water drip washing, use 3 column volumes of 40% ethanol drip washing again, collect 40% pure leacheate, thin-layer chromatography detects, and merges the leacheate that contains the hydroxyl radical carthamin yellow carthamus A spot, 60 ℃ are evaporated to proportion is 1.12, and lyophilize promptly gets safran hydroxyl radical carthamin yellow carthamus A product.With the hydroxyl radical carthamin yellow carthamus A is reference substance, and the content that records hydroxyl radical carthamin yellow carthamus A with HPLC is 86.%, and yield is 1.5%.
Claims (1)
1. the preparation method of a hydroxyl radical carthamin yellow carthamus A is characterized in that comprising the steps:
(1) extract: get dry safflower, the deionized water extraction twice with 20～40 times of safflower weight extracts 30～90min at every turn, extract 40 ℃～90 ℃ of temperature, twice gained extracting solution merged, filter, remove the dregs of a decoction, 60 ℃ are evaporated to proportion is 1.05～1.15 water extract;
(2) separate: above-mentioned water extract is with macroporous adsorbent resin or hydrogen bonding type column chromatography material column chromatography, applied sample amount is 1: 1～3, earlier with 2～4 column volumes of water wash, be 1～5 column volume of 10%～60% aqueous ethanolic solution drip washing with concentration again, collect pure water wash liquid, 60 ℃ be evaporated to proportion be 1.05～1.15 the initial gross separation concentrated solution;
(3) refining: with above-mentioned initial gross separation concentrated solution with nonpolar reversed phase chromatography material column chromatography, applied sample amount is 0.5～2: 1, be 2～4 column volumes of 0%～10% aqueous ethanolic solution drip washing with concentration earlier, be 2～5 column volumes of 10%～70% aqueous ethanolic solution drip washing with concentration again, collect pure water wash liquid, 60 ℃ are evaporated to proportion is 1.05～1.2 must make with extra care concentrated solution;
(4) lyophilize: above-mentioned refining concentrated solution gets safran hydroxyl radical carthamin yellow carthamus A product through lyophilize;
Macroporous adsorbent resin is AB-8 or H103 described in the step (2); The material of hydrogen bonding type column chromatography described in the step (2) is a polymeric amide; Reversed phase chromatography material described in the step (3) is MDS.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102675379B (en) * | 2011-03-15 | 2015-08-19 | 河北以岭医药研究院有限公司 | A kind of method of Hydrolysis kinetics hydroxyl radical carthamin yellow carthamus A from safflower |
| CN103054040B (en) * | 2013-01-13 | 2014-05-21 | 浙江奥默生物医药有限公司 | Pharmaceutical composition for increasing hypoxia tolerance |
| CN104230864A (en) * | 2013-06-08 | 2014-12-24 | 浙江永宁药业股份有限公司 | Novel hydroxysafflor yellow A divalent medicinal salts, and preparing method and uses thereof |
| CN103980239B (en) | 2013-02-07 | 2016-04-13 | 浙江永宁药业股份有限公司 | Hydroxyl radical carthamin yellow carthamus A sodium and production method thereof and purposes |
| CN106496172B (en) * | 2016-10-21 | 2018-12-25 | 乌鲁木齐上善元生物科技有限公司 | A method of extracting carthamin yellow from safflower |
| CN108395420B (en) * | 2018-03-05 | 2023-03-21 | 上海诗丹德标准技术服务有限公司 | Preparation method of hydroxysafflor yellow A |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1475272A (en) * | 2002-08-17 | 2004-02-18 | 李盛学 | Sydroxy carthamin A and its preparation method and use |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1475272A (en) * | 2002-08-17 | 2004-02-18 | 李盛学 | Sydroxy carthamin A and its preparation method and use |
Non-Patent Citations (6)
| Title |
|---|
| Meselhy R. Meselhy et al,.Two new quinochalcone yellow pigments from carthamustinctorius and Ca2+ antagonistic activity of tinctormine.Chem. Pharm. Bull.41 10.1993,41(10),1796-1802. |
| Meselhy R. Meselhy et al,.Two new quinochalcone yellow pigments from carthamustinctorius and Ca2+ antagonistic activity of tinctormine.Chem. Pharm. Bull.41 10.1993,41(10),1796-1802. * |
| 金鸣等.大孔树脂柱色谱法制备红花黄色素和羟基红花黄色素A.中草药35 1.2004,35(1),25-28. |
| 金鸣等.大孔树脂柱色谱法制备红花黄色素和羟基红花黄色素A.中草药35 1.2004,35(1),25-28. * |
| 陈燕忠等.红花中红花黄色素A的分离工艺研究.中药材27 9.2004,27(9),645-647. |
| 陈燕忠等.红花中红花黄色素A的分离工艺研究.中药材27 9.2004,27(9),645-647. * |
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