CN102633861A - Preparation method of physalin B - Google Patents
Preparation method of physalin B Download PDFInfo
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- CN102633861A CN102633861A CN2012101192688A CN201210119268A CN102633861A CN 102633861 A CN102633861 A CN 102633861A CN 2012101192688 A CN2012101192688 A CN 2012101192688A CN 201210119268 A CN201210119268 A CN 201210119268A CN 102633861 A CN102633861 A CN 102633861A
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- physalin
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- chloroform
- extraction
- acetone
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Medicines Containing Plant Substances (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention provides a preparation method of physalin B. The invention is characterized in that supercritical CO2 extraction, silicagel column separation, recrystallization and other steps are utilized to extract and separate physalin B from the overground part of Physalis alkekengi. The method has the advantages of high extraction efficiency and high product purity, and can easily implement industrial production.
Description
Technical field
The invention belongs to the traditional Chinese medicine extraction separation technology field, relate to the preparation method of a kind of physalin B.
Background technology
Physalin B (Physalin B), colourless needle (acetone-methyl alcohol), mp264-266 ℃, molecular formula is C
28H
30O
9, molecular weight is 510.54, is a kind of steroid compound that obtains from plant of Solanaceae wintercherry over-ground part extraction separation.Pharmacological research shows that physalin B has anti-tumor activity, is 137% to the ratio (T/C) of the survival time of mouse leukemia (3PS) when the 300mg/kg dosage; Can suppress some human-like leukemia cells' growth (as: HL-60, KG-1, CTV1, K562, APM1840 and B cell); Have anti-inflammatory activity, the generation to active many types of nuclear neutrophil leucocyte (PMN) chemoluminescence and H2O2 when different concns of these article is the relevant restraining effect of dosage; ED to mouse leukemic lymphoblastoid 9PS
50Be 0.01 μ g/ml, to the ED of nasopharyngeal carcinoma (9KB)
50Be 3.1 μ g/ml.The present invention provides the preparation method of a kind of physalin B, supports with theoretical for the further development and use of wintercherry provide the pharmacology raw material.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of physalin B, adopt supercritical CO
2Step extraction separation physalin B from the wintercherry over-ground part such as extraction, silicagel column separation and recrystallization, this method extraction efficiency is high, product purity is high, be easy to realize suitability for industrialized production.
The present invention realizes through following technical scheme:
The preparation method of a kind of physalin B is characterized in that may further comprise the steps: with the wintercherry over-ground part is raw material, adds supercritical CO
2Extractor is an entrainment agent with acetone, and extraction 4-8h collects extract; Extract with dissolved in chloroform, is added silica gel, mix the back oven drying at low temperature thoroughly, the dress post; The chloroform-methanol gradient elution is collected the corresponding flow point of physalin B, reclaim under reduced pressure reagent, and acetone-recrystallizing methanol promptly gets product.
Said entrainment agent is the acetone soln of 90-100%, and add-on is the 8-15% of medicinal material amount.
Said supercritical CO
2Extracting pressure is 28-35MPa, and extraction temperature is 35-55 ℃, and separating still pressure is 5-7MPa, and separation temperature is 25-45 ℃.
Said chloroform-methanol volume ratio is 1-9:1.
Beneficial effect of the present invention is: the present invention adopts critical CO
2Extraction conditions is gentle, extraction time is fast, with short production cycle, operating parameters is controlled easily; Therefore, effective constituent and constant product quality, and technical process is simple; Easy to operate; Save labor force and a large amount of organic solvents, reduce " three wastes " and pollute, be a kind of environmental protection, be applicable to the method for suitability for industrialized production.
Embodiment
To combine specific embodiment that the present invention is described further below, the following example is intended to describe for example the present invention, rather than limits the present invention by any way.
Embodiment 1:
The wintercherry dry aerial parts are pulverized, got 5kg and drop in the supercritical extraction jar, the acetone soln of adding 100% is as entrainment agent, and add-on is 12% of a medicinal material amount, CO
2Flow is 25L/h, and extracting pressure is 35MPa, and extraction temperature is 35 ℃, and separating still pressure is 6MPa; Separation temperature is 25 ℃, gets wintercherry over-ground part extract, and extract is used dissolved in chloroform, filters; Add silica gel in the filtrating, mix the back oven drying at low temperature thoroughly, dress post, chloroform-methanol 1:1,5:1,9:1 gradient elution; Collect the corresponding flow point of physalin B, reclaim under reduced pressure reagent leaves standstill crystallization; Coarse-grain with acetone-recrystallizing methanol, is obtained 4.55g physalin B monomeric compound, and its purity is 88.6%.
Embodiment 2:
The wintercherry dry aerial parts are pulverized, got 5kg and drop in the supercritical extraction jar, the acetone soln of adding 90% is as entrainment agent, and add-on is 10% of a medicinal material amount, CO
2Flow is 18L/h, and extracting pressure is 32MPa, and extraction temperature is 55 ℃, and separating still pressure is 5.5MPa; Separation temperature is 45 ℃, gets wintercherry over-ground part extract, and extract is used dissolved in chloroform, filters; Add silica gel in the filtrating, mix the back oven drying at low temperature thoroughly, dress post, chloroform-methanol 2:1,4:1,8:1 gradient elution; Collect the corresponding flow point of physalin B, reclaim under reduced pressure reagent leaves standstill crystallization; Coarse-grain with acetone-recrystallizing methanol, is obtained 5.53g physalin B monomeric compound, and its purity is 85.2%.
Embodiment 3:
The wintercherry dry aerial parts are pulverized, got 5kg and drop in the supercritical extraction jar, the acetone soln of adding 90% is as entrainment agent, and add-on is 12% of a medicinal material amount, CO
2Flow is 20L/h, and extracting pressure is 30MPa, and extraction temperature is 45 ℃, and separating still pressure is 6MPa; Separation temperature is 35 ℃, gets wintercherry over-ground part extract, and extract is used dissolved in chloroform, filters; Add silica gel in the filtrating, mix the back oven drying at low temperature thoroughly, dress post, chloroform-methanol 1:1,5:1,9:1 gradient elution; Collect the corresponding flow point of physalin B, reclaim under reduced pressure reagent leaves standstill crystallization; Coarse-grain with acetone-recrystallizing methanol, is obtained 4.03g physalin B monomeric compound, and its purity is 83.4%.
Embodiment 4:
The wintercherry dry aerial parts are pulverized, got 5kg and drop in the supercritical extraction jar, the acetone soln of adding 90% is as entrainment agent, and add-on is 8% of a medicinal material amount, CO
2Flow is 22L/h, and extracting pressure is 28MPa, and extraction temperature is 50 ℃, and separating still pressure is 5MPa; Separation temperature is 30 ℃, gets wintercherry over-ground part extract, and extract is used dissolved in chloroform, filters; Add silica gel in the filtrating, mix the back oven drying at low temperature thoroughly, dress post, chloroform-methanol 2:1,5:1,8:1 gradient elution; Collect the corresponding flow point of physalin B, reclaim under reduced pressure reagent leaves standstill crystallization; Coarse-grain with acetone-recrystallizing methanol, is obtained 4.82g physalin B monomeric compound, and its purity is 87.9%.
Embodiment 5:
The wintercherry dry aerial parts are pulverized, got 5kg and drop in the supercritical extraction jar, the acetone soln of adding 100% is as entrainment agent, and add-on is 15% of a medicinal material amount, CO
2Flow is 25L/h, and extracting pressure is 35MPa, and extraction temperature is 50 ℃, and separating still pressure is 7MPa; Separation temperature is 40 ℃, gets wintercherry over-ground part extract, and extract is used dissolved in chloroform, filters; Add silica gel in the filtrating, mix the back oven drying at low temperature thoroughly, dress post, chloroform-methanol 1:1,4:1,9:1 gradient elution; Collect the corresponding flow point of physalin B, reclaim under reduced pressure reagent leaves standstill crystallization; Coarse-grain with acetone-recrystallizing methanol, is obtained 4.11g physalin B monomeric compound, and its purity is 92.5%.
Claims (4)
1. the preparation method of a physalin B, it is characterized in that may further comprise the steps: with the wintercherry over-ground part is raw material, adds supercritical CO
2Extractor is an entrainment agent with acetone, and extraction 4-8h collects extract; Extract with dissolved in chloroform, is added silica gel, mix the back oven drying at low temperature thoroughly, the dress post; The chloroform-methanol gradient elution is collected the corresponding flow point of physalin B, reclaim under reduced pressure reagent, and acetone-recrystallizing methanol promptly gets product.
2. the preparation method of a kind of physalin B as claimed in claim 1 is characterized in that said entrainment agent is the acetone soln of 90-100%, and add-on is the 8-15% of medicinal material amount.
3. the preparation method of a kind of physalin B as claimed in claim 1 is characterized in that said supercritical CO
2Extracting pressure is 28-35MPa, and extraction temperature is 35-55 ℃, and separating still pressure is 5-7MPa, and separation temperature is 25-45 ℃.
4. the preparation method of a kind of physalin B as claimed in claim 1 is characterized in that said chloroform-methanol volume ratio is 1-9:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101192688A CN102633861A (en) | 2012-04-23 | 2012-04-23 | Preparation method of physalin B |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101192688A CN102633861A (en) | 2012-04-23 | 2012-04-23 | Preparation method of physalin B |
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| CN102633861A true CN102633861A (en) | 2012-08-15 |
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| CN2012101192688A Pending CN102633861A (en) | 2012-04-23 | 2012-04-23 | Preparation method of physalin B |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288846A (en) * | 2013-05-15 | 2013-09-11 | 浙江大学 | Method for extracting and purifying total physalin from physalis plants |
| CN103755719A (en) * | 2013-12-31 | 2014-04-30 | 广东食品药品职业学院 | Physalin B crystal and extraction and preparation methods as well as application of physalin B crystal in preparing anti-inflammatory medicines |
| WO2016110269A1 (en) * | 2015-01-08 | 2016-07-14 | Tseng Wei-Kung | Antiplatelte agent and uses thereof |
| CN105979955A (en) * | 2013-12-12 | 2016-09-28 | 凯敏工业公司 | Personal care products containing extracts of Chinese lantern (physalis alkekengi) |
| CN107011357A (en) * | 2017-03-31 | 2017-08-04 | 浙江大学 | A kind of preparation method of Physalin B and its application in resisting tumor of lung pharmacy |
| CN109776565A (en) * | 2019-01-28 | 2019-05-21 | 浙江省中医药研究院 | A kind of bitter taste chlorins compound and the preparation method and application thereof |
| CN115569098A (en) * | 2022-10-12 | 2023-01-06 | 蓝科医美科学技术(吉林)有限公司 | A herba Oxalidis Corniculatae extract for skin care |
-
2012
- 2012-04-23 CN CN2012101192688A patent/CN102633861A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288846A (en) * | 2013-05-15 | 2013-09-11 | 浙江大学 | Method for extracting and purifying total physalin from physalis plants |
| CN105979955A (en) * | 2013-12-12 | 2016-09-28 | 凯敏工业公司 | Personal care products containing extracts of Chinese lantern (physalis alkekengi) |
| EP3091993A4 (en) * | 2013-12-12 | 2017-11-01 | Kemin Industries, Inc. | Personal care products containing extracts of chinese lantern (physalis alkekengi) |
| CN103755719A (en) * | 2013-12-31 | 2014-04-30 | 广东食品药品职业学院 | Physalin B crystal and extraction and preparation methods as well as application of physalin B crystal in preparing anti-inflammatory medicines |
| CN103755719B (en) * | 2013-12-31 | 2016-06-08 | 广东食品药品职业学院 | Physalin B crystal and extract preparation method and Physalin B crystal in the application prepared in anti-inflammation drugs |
| WO2016110269A1 (en) * | 2015-01-08 | 2016-07-14 | Tseng Wei-Kung | Antiplatelte agent and uses thereof |
| CN107011357A (en) * | 2017-03-31 | 2017-08-04 | 浙江大学 | A kind of preparation method of Physalin B and its application in resisting tumor of lung pharmacy |
| CN109776565A (en) * | 2019-01-28 | 2019-05-21 | 浙江省中医药研究院 | A kind of bitter taste chlorins compound and the preparation method and application thereof |
| CN115569098A (en) * | 2022-10-12 | 2023-01-06 | 蓝科医美科学技术(吉林)有限公司 | A herba Oxalidis Corniculatae extract for skin care |
| CN115569098B (en) * | 2022-10-12 | 2024-03-15 | 蓝科医美科学技术(吉林)有限公司 | A Physalis alkekengi extract for caring skin |
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Application publication date: 20120815 |