CN1569865A - Process for separating and extracting lipids general alkaloid from aconites and wolfsbanes - Google Patents
Process for separating and extracting lipids general alkaloid from aconites and wolfsbanes Download PDFInfo
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- CN1569865A CN1569865A CN 200410010820 CN200410010820A CN1569865A CN 1569865 A CN1569865 A CN 1569865A CN 200410010820 CN200410010820 CN 200410010820 CN 200410010820 A CN200410010820 A CN 200410010820A CN 1569865 A CN1569865 A CN 1569865A
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Abstract
The invention relates to a process for separating and extracting lipids general alkaloid from aconites and wolfsbanes, wherein the long ester chain, small polarity and property of infusible to water for the lipid alkaloid are utilized for carry out the extraction, the process consists of ethanol cold soaking, acid water treatment, and performing chromatography with silica gel column.
Description
Technical field
The invention belongs to the alkaloidal method of extraction separation lipid from monkshood and aconitum plant.
Background technology
Monkshood and aconitum plant are the conventional Chinese medicine materials of traditional tcm clinical practice medication.Have effects such as cardiac stimulant, diuresis, analgesia, anesthesia, anti-inflammatory, raising immunizing power.Mainly contain three Alkaloids in monkshood and the aconitum plant: monoester alkaloid, diester-type alkaloids and lipid alkaloid.Modern pharmacological research proves that the lipid alkaloid has significant biological activity such as analgesia, anti-inflammatory, compares with diester-type alkaloids, and its toxicity is less, is a kind of medicine with extensive pharmacologically active, has important researching value and wide application prospect.
(Wang Yong is high, Acta Pharmaceutica Sinica: Vol.15 (9), 1968,527-531 for alkaloid in the early stage normal employing benzene extraction rhizome of Chinese monkshood and the monkshood; Wang Jie etc., Acta Pharmaceutica Sinica: Vol.20 (1), 1973,71-73; Chen Yan etc., Acta Pharmaceutica Sinica: Vol.12 (7), 1965,435-439), though use benzene extraction alkaloid impurity less, the solubleness of the alkaloid in the rhizome of Chinese monkshood and the monkshood in benzene is also bad, so productive rate is not high.At present, domestic normal employing sour water diacolation (Li Zhengbang etc., research and development of natural products: Vol.9 (1), 1997,9-14) or ethanol (Ding Lisheng etc., right Study on product and exploitation: Vol.6 (3), 1994,50-54) extract alkaloid in the rhizome of Chinese monkshood and the monkshood, report alkaloid (Katagawa, Chem.Pharm.Bull.30 (2) 758-761 (1982)) in the methanol extraction monkshood is abroad also arranged.But because the lipid alkaloid is insoluble in sour water, not comprehensive with the alkaloid that the sour water percolation extracts, lipid alkaloid yield is lower; And the alkaloid in the rhizome of Chinese monkshood and the monkshood easily decomposes in methyl alcohol, is difficult to a large amount of the extraction; Use extraction using alcohol alkaloid efficient higher, but the composition of extraction using alcohol is more extensive, the foreign matter content height, it is extremely important how further to separate purification.Although so very urgent to the research of lipid alkaloid, because the separation and Extraction difficulty, the practical study progress is very slow.
Summary of the invention
The purpose of this invention is to provide a kind of from monkshood and aconitum plant the alkaloidal separating and extracting method of lipid.
Because the alkaloid efficient in the extraction using alcohol rhizome of Chinese monkshood and the monkshood is higher, so the present invention adopts the ethanol cold soaking, steams ethanol, medicinal extract.Be not soluble in sour water according to the lipid alkaloid again, and the alkaloid of other type is soluble in the character of sour water, medicinal extract is handled with hydrochloric acid or aqueous sulfuric acid, filter to such an extent that precipitate, precipitation is dissolved in chloroform or sherwood oil, extract repeatedly several times with hydrochloric acid or aqueous sulfuric acid, steam chloroform or sherwood oil, promptly obtain thick lipid biology total alkali.Use silicagel column, hexanaphthene-ethanol system carries out column chromatography, promptly obtains purified lipid biology total alkali.
The present invention is with monkshood, radix aconiti agrestis, monkshood or Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani) are processed into powder, adding concentration of volume percent is 90-95% ethanol, add-on is to there be not medicinal material to be advisable, supersound extraction 1-3 hour, cold soaking 2-14 days, steam ethanol to doing, get medicinal extract, adding volume by volume concentration is 0.04-0.5% hydrochloric acid or aqueous sulfuric acid, add-on is not advisable to have too the volume of medicinal extract fully, stir, static, filter to such an extent that precipitate, add chloroform or sherwood oil, stirring is dissolved precipitation fully, use volume by volume concentration to be 0.04-0.5% hydrochloric acid or aqueous sulfuric acid continuous extraction 2-6 time, the each consumption of hydrochloric acid or aqueous sulfuric acid is identical with the volume of chloroform or petroleum ether solution, steams chloroform or sherwood oil, promptly obtains thick lipid biology total alkali; Use silicagel column, hexanaphthene-ethanol is with 8-9: 1-2 ratio gradient column chromatography, promptly obtain purified lipid biology total alkali, and detect by electrospray ionization mass spectrum, only contain the lipid alkaloid, do not contain any monoester type and diester-type alkaloids.
Present method first from monkshood and aconitum plant a large amount of extraction separation gone out the lipid biology total alkali, and the lipid alkaloid is carried out purifying, productive rate is more than 0.21%.
Description of drawings
Accompanying drawing 1 is for comprising all alkaloidal ethanolic soln electrospray ionization mass spectrums, and the alkaloid component of extraction using alcohol is more as seen from the figure, comprises all types of alkaloids in the medicinal material, illustrates that the extraction using alcohol ability is stronger;
Accompanying drawing 2 is that the mass spectrum of monoester type and diester-type alkaloids does not wherein comprise the lipid alkaloid, has avoided the waste of sample through after separating;
Accompanying drawing 3 does not wherein comprise monoester type and diester-type alkaloids for separating the alkaloidal mass spectrum of back lipid, illustrates that separation is more complete, and efficient is higher.
Embodiment
Embodiment 1:
It is supersound extraction 1 hour in 95% ethanol that 2000 gram unprocessed Radix Aconiti Lateralis are dipped in volume by volume concentration, and cold soaking 48 hours leaches ethanol extract, 60 ℃ of decompressions steam ethanol to doing, obtain ethanol extract, adding volume by volume concentration is 0.04% aqueous hydrochloric acid, add-on be 10 times to the medicinal extract volume, stir, static, filter to such an extent that precipitate, precipitation is dissolved in chloroform, with volume by volume concentration be 0.04% aqueous hydrochloric acid extraction 2 times, each consumption is identical with the volume of chloroformic solution.40 ℃ of decompressions steam chloroform, promptly obtain thick lipid biology total alkali 9.5 grams.Use silicagel column, 8: 2 system column chromatographies of hexanaphthene-ethanol obtain purified lipid biology total alkali 4.3 grams (yield is 0.21%), use electrospray ionization mass spectrum to detect, and do not contain monoester type and diester-type alkaloids as shown in Figure 3.
Embodiment 2:
Restraining monkshoods with 5000, to be dipped in volume by volume concentration be supersound extraction 2 hours in 95% ethanol, cold soaking 48 hours, leach ethanol extract, 60 ℃ of decompressions steam ethanol to doing, obtain ethanol extract, adding volume by volume concentration is 0.04% aqueous hydrochloric acid, 8 times of add-ons stir to the medicinal extract volume, and are static, filter to such an extent that precipitate, precipitation is dissolved in chloroform, the 0.04% aqueous hydrochloric acid extraction of usefulness 4 times, each consumption is identical with the volume of chloroformic solution, 40 ℃ of decompressions steam chloroform, promptly obtain thick lipid biology total alkali 23 grams.Use silicagel column, 8: 2 system column chromatographies of hexanaphthene-ethanol obtain purified lipid biology total alkali 13.5 grams (0.27%), use electrospray ionization mass spectrum to detect, and do not contain monoester type and diester-type alkaloids as shown in Figure 3.
Embodiment 3:
It is 90% ethanol that monkshood 2000 gram is dipped in volume by volume concentration, supersound extraction 3 hours, and cold soaking 3 days leaches ethanol extract; It is to repeat to extract twice under 90% ethanol the same terms that impregnated monkshood is used volume by volume concentration, obtain ethanol extract, 60 ℃ of decompressions steam ethanol to doing, obtain medicinal extract, the adding volume by volume concentration is 0.3% aqueous sulfuric acid, 6 times of add-ons are to the medicinal extract volume, stir, static, filter to such an extent that precipitate, precipitation is dissolved in sherwood oil, the volume by volume concentration that uses is 0.3% aqueous sulfuric acid extraction 4 times, each consumption is identical with the volume of sherwood oil, and 40 ℃ of decompressions steam sherwood oil, promptly obtains thick lipid biology total alkali 19 grams.Use silicagel column, 8: 1 system column chromatographies of hexanaphthene-ethanol promptly obtain purified lipid biology total alkali 6.09 grams (yield is 0.30%), use electrospray ionization mass spectrum to detect, and do not contain monoester type and diester-type alkaloids as shown in Figure 3.
Embodiment 4:
Is one week of ethanol cold soaking of 95% with 3000 gram radix aconiti agrestis with volume by volume concentration, leaches ethanol extract, and 60 ℃ of decompressions steam ethanol to dried, obtain medicinal extract.Adding volume by volume concentration is 0.5% aqueous hydrochloric acid, and 5 times of add-ons stir to the medicinal extract volume, and are static, filter precipitation.With chloroform dissolving, using volume by volume concentration is that 0.5% aqueous hydrochloric acid extracts 6 times repeatedly precipitation, and each consumption is identical with the chloroformic solution volume, and 40 ℃ of decompressions steam chloroform, promptly obtain thick lipid biology total alkali 19.9 and restrain.Use silicagel column, 8: 1 column chromatographies of hexanaphthene-ethanol system promptly obtain purified lipid biology total alkali 9.6 grams (0.32%), use electrospray ionization mass spectrum to detect, and do not contain monoester type and diester-type alkaloids as shown in Figure 3.
Embodiment 5:
Two weeks of alcohol immersion with Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani) 2000 restrains with 95% leach ethanol extract, and 60 ℃ of decompressions steam ethanol to doing, and obtain medicinal extract.Adding volume by volume concentration is 0.5% aqueous hydrochloric acid, and 10 times of add-ons stir to the medicinal extract volume, and are static, filter precipitation.With chloroform dissolving, using volume by volume concentration is that 0.5% aqueous hydrochloric acid extracts 4 times repeatedly precipitation, and each consumption is identical with the chloroformic solution volume, and 40 ℃ of decompressions steam chloroform, promptly obtain thick lipid biology total alkali 16.7 and restrain.Use silicagel column, hexanaphthene-ethanol (9: 1) system column chromatography obtains purified lipid biology total alkali 5.7 grams (0.28%), uses electrospray ionization mass spectrum to detect, and does not contain monoester type and diester-type alkaloids as shown in Figure 3.
Claims (1)
1. alkaloidal separating and extracting method of lipid from monkshood and aconitum plant, it is characterized in that, with monkshood, radix aconiti agrestis, monkshood or Radix Aconiti Brachypodi (Radix Aconiti Szechenyiani) are processed into powder, adding concentration of volume percent is 90-95% ethanol, add-on is to there be not medicinal material to be advisable, supersound extraction 1-3 hour, cold soaking 2-14 days, steam ethanol to doing, get medicinal extract, adding volume by volume concentration is 0.04-0.5% hydrochloric acid or aqueous sulfuric acid, add-on is advisable with the volume that there was not medicinal extract, stir, static, filter to such an extent that precipitate, add chloroform or sherwood oil, stir, use volume by volume concentration to be 0.04-0.5% hydrochloric acid or aqueous sulfuric acid continuous extraction 2-6 time, each consumption is identical with the volume of chloroform or petroleum ether solution, steams chloroform, promptly obtains thick lipid biology total alkali; Use silicagel column, hexanaphthene-ethanol system is pressed gradient ratio 8-9: the 1-2 column chromatography promptly obtains purified lipid biology total alkali.
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| CN 200410010820 CN1257911C (en) | 2004-04-23 | 2004-04-23 | Process for separating and extracting lipids general alkaloid from aconites and wolfsbanes |
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| CN1257911C CN1257911C (en) | 2006-05-31 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1935203B (en) * | 2005-09-20 | 2010-07-28 | 成都中医药大学 | Radix aconiti agrestis extract and its preparing method |
| CN101129500B (en) * | 2007-08-21 | 2010-09-22 | 中国科学院长春应用化学研究所 | Methods for extracting monoester/bifendate type alkaloid and grease type alkaloid from aconitom traditional Chinese medicine |
| CN101108826B (en) * | 2006-07-17 | 2012-09-12 | 修涞贵 | Method for normal-temperature high-pressure aconine extracting and formulated product thereof |
| CN102798687A (en) * | 2012-08-06 | 2012-11-28 | 中国科学院长春应用化学研究所 | In-site quality detection method of aconite Chinese patent medicines |
| CN103340944A (en) * | 2013-07-22 | 2013-10-09 | 黑龙江大学 | Method for quickly preparing aliphatic alkaloid from aconitum plant |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109453169B (en) * | 2018-11-19 | 2021-05-14 | 云南昊邦制药有限公司 | Application of bulleyaconitine A |
-
2004
- 2004-04-23 CN CN 200410010820 patent/CN1257911C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1935203B (en) * | 2005-09-20 | 2010-07-28 | 成都中医药大学 | Radix aconiti agrestis extract and its preparing method |
| CN101108826B (en) * | 2006-07-17 | 2012-09-12 | 修涞贵 | Method for normal-temperature high-pressure aconine extracting and formulated product thereof |
| CN101129500B (en) * | 2007-08-21 | 2010-09-22 | 中国科学院长春应用化学研究所 | Methods for extracting monoester/bifendate type alkaloid and grease type alkaloid from aconitom traditional Chinese medicine |
| CN102798687A (en) * | 2012-08-06 | 2012-11-28 | 中国科学院长春应用化学研究所 | In-site quality detection method of aconite Chinese patent medicines |
| CN102798687B (en) * | 2012-08-06 | 2014-11-12 | 中国科学院长春应用化学研究所 | In-site quality detection method of aconite Chinese patent medicines |
| CN103340944A (en) * | 2013-07-22 | 2013-10-09 | 黑龙江大学 | Method for quickly preparing aliphatic alkaloid from aconitum plant |
| CN103340944B (en) * | 2013-07-22 | 2014-08-20 | 黑龙江大学 | Method for quickly preparing aliphatic alkaloid from aconitum plant |
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