CN1186345C - Method of extracting peucedanin from angelica - Google Patents
Method of extracting peucedanin from angelica Download PDFInfo
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- CN1186345C CN1186345C CNB011388730A CN01138873A CN1186345C CN 1186345 C CN1186345 C CN 1186345C CN B011388730 A CNB011388730 A CN B011388730A CN 01138873 A CN01138873 A CN 01138873A CN 1186345 C CN1186345 C CN 1186345C
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- silica gel
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- chloroform
- pentosalen
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Abstract
The present invention relates to a method for purifying traditional Chinese medicines, more specifically a method for extracting ammidin from dahurian angelica. The present invention is characterized in that coarse powders of dahurian angelica are taken, extracted by ethanol, decocted and filtered to obtain filter liquor; ethanol in the filter liquor is recovered until no ethanol exists, and after water is diluted, chloroform is used for extraction for three to five times, and chloroform layers are combined; the chloroform of the chloroform layers is evaporated and is heated in vacuum until no water exists to obtain extract; ligarine-acetone is used for elution on a chromatography silica gel column to obtain coarse products of ammidin; a reversed phase high performance liquid chromatography is adopted for refining on liquid phase preparation to obtain reference substances of ammidin, and the purity is more than 98%. In the present invention, the reversed phase high performance liquid chromatography is adopted for refining on liquid phase preparation, and the purity is as high as more than 98%. The products can be used as reference substances and simultaneously can be prepared in a large scale. The technical stability is high, the technology of preparing the coarse products can be used for large scale production of industrialization.
Description
Technical field
The present invention relates to the Chinese medicine method of purification, specifically a kind of method of from the root of Dahurain angelica, extracting pentosalen.
Background technology
China's medicine reference substance is meant that Chinese Pharmacopoeia, ministerial standard record, and is try to achieve discriminating, assay, impurity and related substances inspection etc. accurate consistent when drug assay, in order to the sample contrast, judge the material standard of its quality.Along with development of modern scientific technology, in the medicine analysis field, the range of application of Chinese medicine reference substance is in continuous expansion, to the also constantly increase of demand of its quantity and kind.Usually be the appearance of a reference substance, promptly drive a collection of foundation that contains this kind component drugs product examine proved recipe method and quality standard, the modernization of Chinese medicine is played great pushing effect.
In recent years, the demand to this reference substance of pentosalen in the Chinese medicine root of Dahurain angelica and Chinese patent medicine mass analysis increases day by day, put down in writing the method for separating pentosalen in the literature, have to adopt ether as extracting solvent, and the ether boiling point is low, blast easily; Have the percolation of employing, cold-maceration to extract, but these two kinds of method extraction efficiencies are low and time-consuming; Have and adopt recrystallization to carry out purified, but purity is difficult to reach the requirement of reference substance behind the recrystallization.At the problems referred to above, to the pentosalen Study on extraction process, seek one easy and to prepare the method for pentosalen efficiently most important, also be that relevant department comparatively pays close attention to.
Summary of the invention
The objective of the invention is to provide a kind of method of extracting pentosalen from the root of Dahurain angelica, this method can realize that extraction efficiency is high and save time, and process stabilizing, can obtain the high reference substance of purity.
Get the angelica root meal,, add 10～40 times of amounts, decocted 2～6 hours at every turn through 95% extraction using alcohol 1～4 time, four layers of filtered through gauze, filtrate.The ethanol that reclaims in the filtrate is pure to not having, and with 2～4 times water dilution, divides 3～5 extractions, combined chloroform layer with 2～5 times of amount chloroforms by volume by volume.The chloroform of chloroform layer is volatilized, and vacuum-drying gets medicinal extract to anhydrous.Medicinal extract is by weight measuring silica gel mixed samples with 1.5～2.5 times, on the chromatographic silica gel post (upper prop silica gel is heavy 10～20 times of medicinal extract), with sherwood oil-acetone wash-out, the wash-out ratio was followed successively by 100: 0, and 100: 1,100: 2,100: 4,100: 8,5～20 retention volume of each ratio wash-out, wherein 100: 2 wash-outs partly obtain the pentosalen crude product.Obtain the pentosalen reference substance with reversed-phased high performace liquid chromatographic is refining on the preparation liquid phase, purity is more than 98%.The chromatographic condition that above-mentioned reversed phase high efficiency is annotated phase chromatography is: moving phase second eyeball-water (45: 55) or methanol-water (60: 40), flow velocity 10～15mL/min detects wavelength: 240nm, 260nm, 300nm.The doubly amount that provides in the method is weight ratio except that indicating.
The present invention has following advantage: present method selects 95% ethanol as extracting solvent, and sherwood oil-acetone can be realized having no side effect and the recyclable utilization of solvent as the column chromatography solvent systems; Adopt the reflux method to have the high and timesaving characteristics of extraction efficiency; Adopt reversed-phased high performace liquid chromatographic to make with extra care on the preparation liquid phase, purity is up to more than 98%, and product use in contrast can prepare simultaneously in a large number; Technology stability is good, and the technology of preparation crude product can be used for industrialized production; The pentosalen crude product is expected to become the psoriatic medicine of treatment.
Embodiment
1. get the angelica root 5kg after the pulverizing,, decocted 3 hours at every turn with 95% extraction using alcohol 2 times (add 8 times of amounts for the first time, add 6 times of amounts for the second time), four layers of filtered through gauze, filtrate.The ethanol that reclaims in the filtrate is pure to not having, and with the dilution of 1000mL water, divides 5 extractions, combined chloroform layer with the 3000mL chloroform.The chloroform of chloroform layer is volatilized, and vacuum-drying gets medicinal extract 100g to anhydrous.Medicinal extract 200g silica gel mixed sample, on the chromatographic silica gel post (upper prop silica gel is 1500g), with sherwood oil-acetone wash-out, the wash-out ratio was followed successively by 100: 0, and 100: 1,100: 2,100: 4,100: 8,10 retention volume of each ratio wash-out, wherein 100: 2 wash-outs partly obtain the pentosalen crude product.Obtain pentosalen reference substance 2g with reversed-phased high performace liquid chromatographic is refining on the preparation liquid phase, purity is more than 98%.Chromatographic condition is: mobile phase methanol-water (60: 40), flow velocity 12mL/min detects wavelength: 240nm.
2. get the angelica root 2.5kg after the pulverizing,, decocted 2 hours at every turn with 95% extraction using alcohol 3 times (add 8 times of amounts for the first time, add 6 times of amounts for the second time, add 6 times of amounts for the third time), four layers of filtered through gauze, filtrate.The ethanol that reclaims in the filtrate is pure to not having, and with the dilution of 600mL water, divides 4 extractions, combined chloroform layer with the 2000mL chloroform.The chloroform of chloroform layer is volatilized, and vacuum-drying gets medicinal extract 55g to anhydrous.Medicinal extract 120g silica gel mixed sample, at self-control silicagel column (upper prop silica gel is 1000g), with sherwood oil-acetone wash-out, the wash-out ratio was followed successively by 100: 0,100: 1,100: 2,100: 4,100: 8,12 retention volume of each ratio wash-out, wherein 100: 2 wash-outs partly obtain the pentosalen crude product.Obtain pentosalen reference substance 1g with reversed-phased high performace liquid chromatographic is refining on the preparation liquid phase, purity is more than 98%.Chromatographic condition is: moving phase second eyeball-water (45: 55), flow velocity 14mL/min detects wavelength: 240nm.
3. get the angelica root 10kg after the pulverizing,, decocted 2 hours at every turn with 95% extraction using alcohol 4 times (add 8 times of amounts for the first time, add 6 times of amounts for the second time, add 6 times of amounts for the third time, the 4th time add 4 times of amounts), four layers of filtered through gauze, filtrate.The ethanol that reclaims in the filtrate is pure to not having, and with the dilution of 1500mL water, divides 3 extractions, combined chloroform layer with the 5000mL chloroform.The chloroform of chloroform layer is volatilized, and vacuum-drying gets medicinal extract 230g to anhydrous.Medicinal extract 500g silica gel mixed sample, chromatographic silica gel post (upper prop silica gel is 4500g), with sherwood oil-acetone wash-out, the wash-out ratio was followed successively by 100: 0,100: 1,100: 2,100: 4,100: 8,7 retention volume of each ratio wash-out, wherein 100: 2 wash-outs partly obtain the pentosalen crude product.Obtain pentosalen reference substance 5g with reversed-phased high performace liquid chromatographic is refining on the preparation liquid phase, purity is more than 98%.Chromatographic condition is: mobile phase methanol-water (60: 40), flow velocity 10mL/min detects wavelength: 300nm.
Claims (4)
1. a method of extracting pentosalen from the root of Dahurain angelica is characterized in that getting the angelica root meal, through 95% extraction using alcohol 1～4 time, decocted 2～6 hours at every turn, four layers of filtered through gauze, filtrate; Reclaim ethanol in the filtrate to there not being alcohol, measure chloroforms and divide 3～5 extractions, combined chloroform layer with being 2～5 times with volume ratio again after 2～4 times the water dilution by volume; The chloroform of chloroform layer is volatilized, and vacuum-drying gets medicinal extract to anhydrous; The medicinal extract weight ratio is 1.5～2.5 times of amount silica gel mixed samples, on the chromatographic silica gel post, use sherwood oil-acetone wash-out, the wash-out ratio was followed successively by 100: 0,100: 1,100: 2,100: 4,100: 8,5～20 retention volume of each ratio wash-out, wherein 1 00: 2 wash-outs partly obtain the pentosalen crude product; Obtain the pentosalen reference substance with reversed-phased high performace liquid chromatographic is refining on the preparation liquid phase, purity is more than 98%.
2. in accordance with the method for claim 1, the chromatographic condition that it is characterized in that said reversed-phased high performace liquid chromatographic is: moving phase second eyeball-water (45: 55) or methanol-water (60: 40), flow velocity 10～15mL/min detects wavelength: 240nm, 260nm, 300nm.
3. in accordance with the method for claim 1, it is characterized in that upper prop silica gel on the chromatographic silica gel post is heavy 10～20 times of medicinal extract.
4. in accordance with the method for claim 1, it is characterized in that adding 10～40 times of amounts through 95% extraction using alcohol 1～4 time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011388730A CN1186345C (en) | 2001-12-21 | 2001-12-21 | Method of extracting peucedanin from angelica |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011388730A CN1186345C (en) | 2001-12-21 | 2001-12-21 | Method of extracting peucedanin from angelica |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1427004A CN1427004A (en) | 2003-07-02 |
| CN1186345C true CN1186345C (en) | 2005-01-26 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011388730A Expired - Lifetime CN1186345C (en) | 2001-12-21 | 2001-12-21 | Method of extracting peucedanin from angelica |
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| Country | Link |
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| CN (1) | CN1186345C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805350B (en) * | 2010-04-22 | 2012-08-22 | 南京大学 | Synthesis method of imperatorin derivative |
| CN102344453A (en) * | 2010-08-06 | 2012-02-08 | 苏州瑞蓝博中药技术开发有限公司 | Method for extracting imperatorin |
| CN109406681B (en) * | 2018-12-21 | 2021-11-16 | 广东一方制药有限公司 | Construction method and detection method of UPLC characteristic spectrum of radix angelicae medicinal material |
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2001
- 2001-12-21 CN CNB011388730A patent/CN1186345C/en not_active Expired - Lifetime
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| Publication number | Publication date |
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| CN1427004A (en) | 2003-07-02 |
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Effective date of registration: 20170213 Address after: 313113 Zhejiang city of Huzhou province Changxing County Si'an Town Industrial Zone Patentee after: Giant surplus (Changxin) Biotechnology Co., Ltd. Address before: Heping District, Liaoning city of Shenyang province 110003 Street 19 No. 8 Patentee before: Xiehe Group Co., Ltd., Shenyang |
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Effective date of registration: 20180507 Address after: 518057 A1, unit 303, Kexing Science Park, Keyuan Road, central Nanshan District, Shenzhen, Guangdong. Patentee after: Shenzhen new synergy Health Management Co., Ltd. Address before: 313113 Industrial Zone, Si an town, Changxing County, Huzhou, Zhejiang Patentee before: Giant surplus (Changxin) Biotechnology Co., Ltd. |
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