CN103483358A - Method for producing neem crude drug by extracting neem with supercritical CO2 - Google Patents
Method for producing neem crude drug by extracting neem with supercritical CO2 Download PDFInfo
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- CN103483358A CN103483358A CN201310480938.3A CN201310480938A CN103483358A CN 103483358 A CN103483358 A CN 103483358A CN 201310480938 A CN201310480938 A CN 201310480938A CN 103483358 A CN103483358 A CN 103483358A
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- extraction
- chinaberry
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D519/00—Heterocyclic compounds containing more than one system of two or more relevant hetero rings condensed among themselves or condensed with a common carbocyclic ring system not provided for in groups C07D453/00 or C07D455/00
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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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
- Extraction Or Liquid Replacement (AREA)
- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a method for producing a neem crude drug by extracting neem with supercritical CO2, and aims to solve the problems that the existing preparation method is relatively low in efficiency and relatively high in cost and the content of nimbin in a product is low. The method disclosed by the invention comprises the following steps: (1) material preparation, (2) extraction, (3) crystallization and (4) re-crystallization, wherein the content of nimbin in a final product is more than or equal to 20%. Through the method disclosed by the invention, the production efficiency is improved while the production cost is reduced, and the prepared product is extremely high in nimbin content, so that growing requirements for nimbin crude drugs can be met.
Description
Technical field
The present invention is specifically related to a kind of supercritical CO
2extraction prints chinaberry and produces the method that prints the former medicine of chinaberry.
Background technology
Printing chinaberry is Meliaceae Melia arbor, extensively plants in tropical and subtropical region.Originate in Burma and India, have and distribute and plantation in more than 70 countries, with Asian countries's output maximums such as India.All contain active substance in fruit, seed, kind core, branch, leaf, bark and the resin of seal chinaberry, but with seed more so.So far, print in chinaberry and found 100 multiple compounds, have at least 70 kinds of compounds to have biological activity, they are diterpenes, triterpenes, five triterpeness and non-terpenoid.Be mainly margosa tree element, melianotriol and nimbin etc., these extracts to insect food refusal is arranged, disturb lay eggs, the interference insect variation, it can't be changed in quality and reaches the desinsection purpose for adult, repellent larva and the effect that suppresses its growth.Nimbin is that a class is isolated the strongest active compound from print chinaberry, and it belongs to tetracyclic triterpenes.And Chinese patent ZL01108503.7, there is following defect in it: (1) production efficiency is lower, be difficult to meet the demand of growing nimbin raw medicine industry, (2) in production process, energy consumption is larger, makes product cost higher, makes its competitive power not high, (3) use existing carbon dioxide abstraction to print chinaberry production seal chinaberry medicinal extract content not high, impurity phase is to more, and product is stable not, for producing formulation products, has certain risk and problem.
Summary of the invention
The object of the present invention is to provide a kind of supercritical CO
2extraction prints chinaberry and produces the method that prints the former medicine of chinaberry, and the efficiency that solves existing preparation method is lower, and cost is higher, and the not high problem of Azadirachtin Cotent in product.
The present invention is achieved through the following technical solutions:
A kind of supercritical CO
2extraction prints chinaberry and produces the method that prints the former medicine of chinaberry, comprises the following steps:
(1) get the raw materials ready: get the neem kernel after pulverizing, CO 2 fluid, 95% chloroform, wherein the weight ratio of the flow of carbonic acid gas and neem kernel is 100～200:1, carbonic acid gas and chloroform weight ratio are 100:6～8;
(2) extraction: neem kernel is placed in to extraction plant, at pressure, be 2～24.9Mpa, temperature is that under 30～60 ℃ of conditions, the carbonic acid gas that passes into the above-critical state that carries chloroform by above-mentioned weight ratio is extracted, extraction time is 2～5 hours, has both obtained paste;
(3) crystallization: paste is transferred in crystallization kettle, now the paste Azadirachtin Cotent is 10%, adds acetone to make it to dissolve, and the add-on of acetone is different can be advisable in submergence, acetone is evaporated to dry under 55 ℃ of conditions, the nimbin crystal that now to obtain Azadirachtin Cotent be 15%;
(4) recrystallization: add tetracol phenixin in above-mentioned nimbin crystal, the weight ratio of nimbin crystal and tetracol phenixin is 1:3～5, heats to 55 ℃ and makes it to dissolve fully, progressively be cooled to 1～5 ℃, the still intercrystalline is separated out again, and goes out still and filters, crystal is the elaboration nimbin, content >=20%.
Further, the specifically implementation method of described step (2) is as follows: neem kernel is placed in to the one-level extraction kettle, at pressure, be 2～24.9Mpa, temperature is under 30～60 ℃ of conditions, the carbonic acid gas that passes into the above-critical state that carries chloroform by above-mentioned weight ratio carries out the one-level extraction, and the time is 1～2 hour; Extraction liquid passes into primary separator, at pressure, is 2～7Mpa, and temperature is to isolate paste solution and waste residue under 30～40 ℃ of conditions; Paste solution is passed into to the secondary extraction, and the time is 0.5～2 hour, and the secondary extract is passed into to second-stage separator, at pressure, is 2～7Mpa, and temperature is under 30～50 ℃ of conditions, by second-stage separator, separates, and obtains paste; Whole extraction time is 2～5 hours.
In order to reduce production costs, described secondary extract also comprises carbonic acid gas and chloroform by the isolated material of second-stage separator; Wherein carbonic acid gas again carries chloroform and enters in the one-level extraction kettle and carry out the next round extraction after condensation, compression.This step can, by the carbon dioxide recovery utilization, have been saved production cost greatly.
As a kind of preferred, in described step (1), flow and the neem kernel weight ratio of carbonic acid gas are 150:1, and carbonic acid gas and chloroform weight ratio are 100:6.
Perhaps, in described step (1), the flow of carbonic acid gas and the weight ratio of neem kernel are 100:1, and carbonic acid gas and chloroform weight ratio are 100:8.
Perhaps, in described step (1), the flow of carbonic acid gas and the weight ratio of neem kernel are 200:1, and carbonic acid gas and chloroform weight ratio are 100:7.
In addition, in described step (2), pressure is 24.9Mpa, and temperature is 50 ℃.
The present invention has the following advantages and beneficial effect:
(1) entrainment agent of the present invention is selected chloroform, and do not use the entrainment agents such as traditional methyl alcohol, ethanol, thereby improved the leaching effect, its reason is that methyl alcohol, ethanol etc. are relatively poor to the solvability of nimbin, the leaching effect is very not good, after the long-time practice of applicant and test, find to use chloroform respond well as entrainment agent, effect improves 10% left and right.
(2) method of the present invention has realized carbon dioxide recycling, improves raw-material rate of utilization, reduces energy consumption, thereby has reduced production cost.
(3) method of the present invention is carried out specific crystallization and re-crystallization step to the paste obtained, thereby has improved the content of nimbin in the product.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated, but embodiments of the present invention are not limited to this.
Embodiment 1
A kind of supercritical CO
2extraction prints chinaberry and produces the method that prints the former medicine of chinaberry, comprises the following steps:
(1) get the raw materials ready: get the neem kernel after pulverizing, CO 2 fluid, 95% chloroform, wherein the weight ratio of the flow of carbonic acid gas and neem kernel is 150:1, carbonic acid gas and chloroform weight ratio are 100:6.
(2) extraction: neem kernel is placed in to the one-level extraction kettle, is 24.9Mpa at pressure, and temperature is under 50 ℃ of conditions, and the carbonic acid gas that passes into the above-critical state that carries chloroform by above-mentioned weight ratio carries out the one-level extraction, and the time is 1.5 hours; Extraction liquid passes into primary separator, at pressure, is 5Mpa, and temperature is to isolate paste solution and waste residue under 40 ℃ of conditions; Paste solution is passed into to the secondary extraction, time is 1.5 hours, the secondary extract is passed into to second-stage separator, at pressure, be 5Mpa, temperature is under 50 ℃ of conditions, by second-stage separator, isolates paste, chloroform and carbonic acid gas, and carbonic acid gas again carries chloroform after condensation, compression to carry out the one-level extraction kettle and carry out the next round extraction, to realize carbon dioxide recycling, complete a circulation.The whole cycling extraction time is 4 hours.
(3) crystallization: paste is transferred in crystallization kettle, now the paste Azadirachtin Cotent is 10%, adds acetone to make it to dissolve, and the add-on of acetone being advisable in submergence, acetone is evaporated to dry under 55 ℃ of conditions, the nimbin crystal that now to obtain Azadirachtin Cotent be 15%.
(4) recrystallization: add tetracol phenixin in above-mentioned nimbin crystal, the weight ratio of nimbin crystal and tetracol phenixin is 1:4, heats to 55 ℃ and makes it to dissolve fully, progressively be cooled to 1 ℃, the still intercrystalline is separated out again, and goes out still and filters, crystal is the elaboration nimbin, content >=20%.
Then detected, if less than index, recrystallization again, know and meet index.Finally only need the lucifuge packing to get final product.
Embodiment 2
A kind of supercritical CO
2extraction prints chinaberry and produces the method that prints the former medicine of chinaberry, comprises the following steps:
(1) get the raw materials ready: get the neem kernel after pulverizing, CO 2 fluid, 95% chloroform, wherein the weight ratio of the flow of carbonic acid gas and neem kernel is 100:1, carbonic acid gas and chloroform weight ratio are 100:7.
(2) extraction: neem kernel is placed in to the one-level extraction kettle, is 20Mpa at pressure, and temperature is under 30 ℃ of conditions, and the carbonic acid gas that passes into the above-critical state that carries chloroform by above-mentioned weight ratio carries out the one-level extraction, and the time is 2 hours; Extraction liquid passes into primary separator, at pressure, is 2Mpa, and temperature is to isolate paste solution and waste residue under 30 ℃ of conditions; Paste solution is passed into to the secondary extraction, time is 1 hour, the secondary extract is passed into to second-stage separator, at pressure, be 2Mpa, temperature is under 30 ℃ of conditions, by second-stage separator, isolates paste, chloroform and carbonic acid gas, and carbonic acid gas again carries chloroform after condensation, compression to carry out the one-level extraction kettle and carry out the next round extraction, to realize carbon dioxide recycling, complete a circulation.The whole cycling extraction time is 4 hours.
(3) crystallization: paste is transferred in crystallization kettle, now the paste Azadirachtin Cotent is 10%, adds acetone to make it to dissolve, and the add-on of acetone is different can be advisable in submergence, acetone is evaporated to dry under 55 ℃ of conditions, the nimbin crystal that now to obtain Azadirachtin Cotent be 15%.
(4) recrystallization: add tetracol phenixin in above-mentioned nimbin crystal, the weight ratio of nimbin crystal and tetracol phenixin is 1:3, heats to 55 ℃ and makes it to dissolve fully, progressively be cooled to 3 ℃, the still intercrystalline is separated out again, and goes out still and filters, crystal is the elaboration nimbin, content >=20%.
Then detected, if less than index, recrystallization again, until meet index.Finally only need the lucifuge packing to get final product.
Embodiment 3
A kind of supercritical CO
2extraction prints chinaberry and produces the method that prints the former medicine of chinaberry, comprises the following steps:
(1) get the raw materials ready: get the neem kernel after pulverizing, CO 2 fluid, 95% chloroform, wherein the weight ratio of the flow of carbonic acid gas and neem kernel is 200:1, carbonic acid gas and chloroform weight ratio are 100:8.
(2) extraction: neem kernel is placed in to the one-level extraction kettle, is 2Mpa at pressure, and temperature is under 40 ℃ of conditions, and the carbonic acid gas that passes into the above-critical state that carries chloroform by above-mentioned weight ratio carries out the one-level extraction, and the time is 1 hour; Extraction liquid passes into primary separator, at pressure, is 7Mpa, and temperature is to isolate paste solution and waste residue under 35 ℃ of conditions; Paste solution is passed into to the secondary extraction, time is 2 hours, the secondary extract is passed into to second-stage separator, at pressure, be 7Mpa, temperature is under 40 ℃ of conditions, by second-stage separator, isolates paste, chloroform and carbonic acid gas, and carbonic acid gas again carries chloroform after condensation, compression to carry out the one-level extraction kettle and carry out the next round extraction, to realize carbon dioxide recycling, complete a circulation.The whole cycling extraction time is 4 hours.
(3) crystallization: paste is transferred in crystallization kettle, now the paste Azadirachtin Cotent is 10%, adds acetone to make it to dissolve, and the add-on of acetone is different can be advisable in submergence, acetone is evaporated to dry under 55 ℃ of conditions, the nimbin crystal that now to obtain Azadirachtin Cotent be 15%.
(4) recrystallization: add tetracol phenixin in above-mentioned nimbin crystal, the weight ratio of nimbin crystal and tetracol phenixin is 1:5, heats to 55 ℃ and makes it to dissolve fully, progressively be cooled to 5 ℃, the still intercrystalline is separated out again, and goes out still and filters, crystal is the elaboration nimbin, content >=20%.
Then detected, if less than index, recrystallization again, until meet index.Finally only need the lucifuge packing to get final product.
Should be noted that, above embodiment is the unrestricted technical scheme of the present invention in order to explanation only, although with reference to above-described embodiment, the present invention is had been described in detail, those of ordinary skill in the art is to be understood that: still can modify or be equal to replacement the present invention, and not breaking away from any modification or partial replacement of the spirit and scope of the present invention, it all should be encompassed in claim scope of the present invention.
Claims (7)
1. a supercritical CO
2extraction prints chinaberry and produces the method that prints the former medicine of chinaberry, it is characterized in that, comprises the following steps:
(1) get the raw materials ready: get the neem kernel after pulverizing, CO 2 fluid, 95% chloroform, wherein the weight ratio of the flow of carbonic acid gas and neem kernel is 100～200:1, carbonic acid gas and chloroform weight ratio are 100:6～8;
(2) extraction: neem kernel is placed in to extraction plant, at pressure, be 2～24.9Mpa, temperature is under 30～60 ℃ of conditions, by the flow of the carbonic acid gas of above-mentioned weight ratio and the carbonic acid gas that neem kernel passes into the above-critical state that carries chloroform, extracted, extraction time is 2～5 hours, has both obtained paste;
(3) crystallization: paste is transferred in crystallization kettle, and now the paste Azadirachtin Cotent is 10%, adds acetone to make it to dissolve, and acetone is evaporated to dry under 55 ℃ of conditions, the nimbin crystal that now to obtain Azadirachtin Cotent be 15%;
(4) recrystallization: add tetracol phenixin in above-mentioned nimbin crystal, the weight ratio of nimbin crystal and tetracol phenixin is 1:3～5, heats to 55 ℃ and makes it to dissolve fully, progressively be cooled to 1～5 ℃, the still intercrystalline is separated out again, and goes out still and filters, crystal is the elaboration nimbin, content >=20%.
2. a kind of supercritical CO according to claim 1
2extraction prints chinaberry and produces the method that prints the former medicine of chinaberry, it is characterized in that, the specifically implementation method of described step (2) is as follows: neem kernel is placed in to the one-level extraction kettle, at pressure, be 2～24.9Mpa, temperature is under 30～60 ℃ of conditions, the carbonic acid gas that passes into the above-critical state that carries chloroform by above-mentioned weight ratio carries out the one-level extraction, and the time is 1～2 hour; Extraction liquid passes into primary separator, at pressure, is 2～7Mpa, and temperature is to isolate paste solution and waste residue under 30～40 ℃ of conditions; Paste solution is passed into to the secondary extraction, and the time is 0.5～2 hour, and the secondary extract is passed into to second-stage separator, at pressure, is 2～7Mpa, and temperature is under 30～50 ℃ of conditions, by second-stage separator, separates, and obtains paste; Whole extraction time is 2～5 hours.
3. a kind of supercritical CO according to claim 2
2extraction prints chinaberry and produces the method that prints the former medicine of chinaberry, it is characterized in that, described secondary extract also comprises carbonic acid gas and chloroform by the isolated material of second-stage separator; Wherein carbonic acid gas again carries chloroform and enters in the one-level extraction kettle and carry out the next round extraction after condensation, compression.
4. a kind of supercritical CO according to claim 1
2extraction prints chinaberry and produces the method that prints the former medicine of chinaberry, it is characterized in that, in described step (1), the flow of carbonic acid gas and the weight ratio of neem kernel are 150:1, and carbonic acid gas and chloroform weight ratio are 100:6.
5. a kind of supercritical CO according to claim 1
2extraction prints chinaberry and produces the method that prints the former medicine of chinaberry, it is characterized in that, in described step (1), the flow of carbonic acid gas and the weight ratio of neem kernel are 100:1, and carbonic acid gas and chloroform weight ratio are 100:8.
6. a kind of supercritical CO according to claim 1
2extraction prints chinaberry and produces the method that prints the former medicine of chinaberry, it is characterized in that, in described step (1), the flow of carbonic acid gas and the weight ratio of neem kernel are 200:1, and carbonic acid gas and chloroform weight ratio are 100:7.
7. a kind of supercritical CO according to claim 1
2extraction prints chinaberry and produces the method that prints the former medicine of chinaberry, it is characterized in that, in described step (2), pressure is 24.9Mpa, and temperature is 50 ℃.
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| CN201310480938.3A CN103483358B (en) | 2013-10-15 | 2013-10-15 | A kind of supercritical CO 2extraction print chinaberry produces the method for the former medicine of print chinaberry |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106674253A (en) * | 2016-09-30 | 2017-05-17 | 王尔贵 | Method for subcritically extracting azadirachtin from azadirachta indica seeds with tetrafluoroethane fluid |
Citations (4)
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| CN1373132A (en) * | 2002-02-08 | 2002-10-09 | 云南中科生物产业有限公司 | Process for supercritical extracting nimbin |
| CN1389465A (en) * | 2001-06-06 | 2003-01-08 | 成都绿金生物科技有限责任公司 | Supercritical fluid extraction process of nim to produce mimbin extract |
| CN101029276A (en) * | 2006-03-03 | 2007-09-05 | 中国林业科学研究院资源昆虫研究所 | Fast method for continuouslly extracting nim oil and nimbin raw medicine from nim seed |
| CN101857603A (en) * | 2010-05-07 | 2010-10-13 | 中国科学院地球化学研究所 | Multi-stage countercurrent extraction method for azadirachtin |
-
2013
- 2013-10-15 CN CN201310480938.3A patent/CN103483358B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1389465A (en) * | 2001-06-06 | 2003-01-08 | 成都绿金生物科技有限责任公司 | Supercritical fluid extraction process of nim to produce mimbin extract |
| CN1373132A (en) * | 2002-02-08 | 2002-10-09 | 云南中科生物产业有限公司 | Process for supercritical extracting nimbin |
| CN101029276A (en) * | 2006-03-03 | 2007-09-05 | 中国林业科学研究院资源昆虫研究所 | Fast method for continuouslly extracting nim oil and nimbin raw medicine from nim seed |
| CN101857603A (en) * | 2010-05-07 | 2010-10-13 | 中国科学院地球化学研究所 | Multi-stage countercurrent extraction method for azadirachtin |
Non-Patent Citations (2)
| Title |
|---|
| 李永红: "印楝（Azadirachta indica）种仁中印楝素的提取及其杀虫活性研究", 《中国优秀硕士学位论文全文数据库（硕士）农业科技辑》, no. 02, 31 December 2003 (2003-12-31), pages 16 * |
| 赵淑英等: "新工艺萃取印楝素及机理初探", 《山东化工》, vol. 38, no. 10, 31 December 2009 (2009-12-31) * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106674253A (en) * | 2016-09-30 | 2017-05-17 | 王尔贵 | Method for subcritically extracting azadirachtin from azadirachta indica seeds with tetrafluoroethane fluid |
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