CN100448871C - Method for extracting nimbin - Google Patents
Method for extracting nimbin Download PDFInfo
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- CN100448871C CN100448871C CNB2006100411447A CN200610041144A CN100448871C CN 100448871 C CN100448871 C CN 100448871C CN B2006100411447 A CNB2006100411447 A CN B2006100411447A CN 200610041144 A CN200610041144 A CN 200610041144A CN 100448871 C CN100448871 C CN 100448871C
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- nimbin
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Abstract
The invention discloses an extracting method of melicitrin, which comprises the following steps: first, immersing peeled melicit seed as 3-5 times organic solvent as melicitrin for 6-12 h; second, adopting high-speed blade to extract; filtering to obtain extract and filter cake; third, removing polarity organic solvent to obtain the product under 40 deg.c.
Description
Technical field
The present invention relates to a kind of extracting method of botanical pesticide, relate in particular to a kind of extracting method of nimbin.
Background technology
Contain a large amount of nim oils in the neem kernel, so that neem kernel is directly pulverized is very difficult, usually easily being clamminess caking causes pulverizer to run well, and causes the seed heating easily, causes nimbin partly to decompose; Also have the squeezing of the elder generation of employing to deoil in the bibliographical information and pulverize then, though can solve the problem of pulverizing caking like this, the part nimbin is dissolved in the pressed oil in expressing process, and easily causes intensification to cause nimbin partly to decompose in expressing process.
Summary of the invention
The invention provides the pulverizing extraction process that a kind of technology is simple, extraction yield is high, cost is low, quality product is high.
The present invention adopts following technical scheme:
A kind of extracting method of nimbin may further comprise the steps,
The first step, the polar organic solvent of doubly removing the peel the neem kernel quality with 3-5 soaked the peeling neem kernel 6-12 hour,
Second step, in above-mentioned polar organic solvent, adopt the high speed blade cut to stir and pulverize the extraction nimbin, refilter, obtain extracting solution and filter cake,
In the 3rd step, extracting solution at 10～40 ℃ of following vacuum concentration, is removed the enriched material that polar organic solvent obtains containing nimbin.
Also can be after second step obtains filter cake among the present invention, adding continues to stir extraction 3-5 hour with the polar organic solvent that 3-5 doubly removes the peel the neem kernel quality in filter cake, filters, and obtains extracting solution and filter cake, again filter cake is repeated to extract 2-5 time according to identical method, again extracting solution is merged.
Among the present invention, the extracting method of nimbin according to claim 1, it is characterized in that the enriched material that contains nimbin that claim 1 obtains is purified, step is: with the 3-5 normal hexane or the sherwood oil doubly of peeling neem kernel quality, adularescent floss precipitation produces, filter, use the solvent wash precipitation identical, drying with soaking the peeling neem kernel after, obtain containing the white dry powder of nimbin.
The present invention adopts the high speed blade cut to stir when pulverizing neem seed in the polar organic solvent medium in second step, produces overheated chuck cooling or the coil pipe cooling exterior cooling of adopting when avoiding high-speed stirring to pulverize.
The present invention obtains following technique effect:
1. the present invention has adopted and has utilized the high speed blade cut stir to pulverize extractive technique in the polar organic solvent medium, and overcome the direct pulverizing of the kind benevolence caking that easily is clamminess and caused and pulverize difficulty, and the squeezing shortcoming of deoiling and causing nimbin to lose.
2. shorten technology, pulverized extraction and unite two into one, reduced the waste of vegetable material, improved the extraction yield of nimbin, reduced cost.
3. the invention provides with to the nimbin solvability preferably polar organic solvent soak softening peeling neem kernel, adopting the high speed blade cut to stir then in the polar organic solvent medium pulverizes, pulverize to extract and to unite two into one, produce when avoiding high-speed stirring to pulverize and overheatedly adopt chuck cooling or coil pipe cooling to solve.The feature of this technology is that the material after neem seed is pulverized easily, pulverized has good mobility and thinner particle helps further extraction, has overcome the shortcoming of existing disintegrating process, has shortened technological process, has improved the nimbin extraction yield.
Principle of the present invention is as follows: peeling kind of benevolence is directly pulverized because it contains the Chuck Steak caking that is clamminess, if the adding appropriate solvent makes it dispersion when pulverizing, reduces the purpose that its viscosity can reach pulverizing.
Description of drawings
Fig. 1 is high pressure liquid chromatography (HPLC) figure of nimbin A extraction product
Fig. 2 is high pressure liquid chromatography (HPLC) figure of nimbin A standard substance
Embodiment
Embodiment 1
A kind of extracting method of nimbin may further comprise the steps,
The first step, the polar organic solvent of doubly removing the peel the neem kernel quality with 3-5 soaked the peeling neem kernel 6-12 hour,
Second step, in above-mentioned polar organic solvent, adopt the high speed blade cut to stir and pulverize the extraction nimbin, refilter, obtain extracting solution and filter cake,
In the 3rd step, under 10～40 ℃, vacuum concentration is removed the enriched material that polar organic solvent obtains containing nimbin with extracting solution.
Above-mentioned polar organic solvent is for being a kind of in the alcohol, ketone, ester, ether, nitrile or their mixture, the proportioning of mixture is any proportioning, as methyl alcohol, ethanol, acetone, butanone, ethyl acetate, methyl acetate, methyl tertiary butyl ether, acetonitrile etc. or its mixture.
A kind of extracting method of nimbin, the polar organic solvent normal temperature (for example can be 20 degrees centigrade or 25 degrees centigrade) of doubly removing the peel the neem kernel quality with 3-5 soaked softening peeling neem kernel 6-12 hour, wherein the quality of polar organic solvent can be 3.2 times of peeling neem kernel quality, 4 times, 4.2 doubly, 4.g doubly, soak time can be 7 hours, 8.5 hour, 9.5 hour, 11 hours, 11.5 hour, in above-mentioned polar organic solvent, adopt the high speed blade cut to stir to pulverize then and (can adopt soybean milk maker, rotating speed can be 10000-22000 rev/min) extract nimbin, obtain extracting solution and filter cake after the filtration, in filter cake, add polar organic solvent that 2-5 doubly removes the peel the neem kernel quality and continue the normal temperature mechanical stirring and (in soybean milk maker, carry out, stirring the speed of extracting is 2000-8000 rev/min) extracted 3-5 hour, wherein the weight of polar organic solvent can be 2.5 times of peeling neem kernel quality, 3 times, and 3.2 times, 4 times, 4.2 doubly, 4.8 times, the time can be 3.3 hours, 4.2 hour, 4.8 hour, so repeat 2-5 time, for example can be 3 or 4 times, again extracting solution is merged, at 10 ℃～40 ℃ following vacuum concentration, remove polar organic solvent, obtain containing the enriched material of nimbin, wherein the vacuum concentration temperature can be chosen for 15 ℃, 22 ℃, 28 ℃, 32 ℃, 38 ℃, pressure can be 0.07-0.095MPa.
In the present embodiment, the enriched material that contains nimbin that claim 1 obtains is purified, step is: enriched material adds 4-8 and doubly plants in the benevolence quality sherwood oil (boiling range is 60-90 ℃), the adularescent floss produces, filter, with non-polar organic solvent such as sherwood oil (boiling range is 60-90 ℃) washing leaching cake, the dry white dry powder that must contain nimbin.
In the polar organic solvent medium, adopt the high speed blade cut to stir when pulverizing neem seed in the present embodiment, produce overheated adopt chuck cooling or coil pipe cooling when avoiding high-speed stirring to pulverize.
Above-mentioned polar organic solvent is a kind of in alcohol, ketone, ester, ether, the nitrile or their mixture, as methyl alcohol, ethanol, acetone, butanone, ethyl acetate, methyl acetate, methyl tertiary butyl ether, acetonitrile etc. or its mixture, the proportioning of mixture can be any proportioning.
Remove the not mouldy neem kernel 100g of skin, soaked softening 12 hours with the 200ml ethyl acetate, the back is stirred pulverizing with nine positive household soy milk machines and is extracted in the ethyl acetate medium, stir and extract four times, and filtrate merges, vacuum concentration is removed ethyl acetate, add 4-8 and doubly plant benevolence quality sherwood oil (boiling range is 60-90 ℃) in enriched material, the adularescent floss produces, and filters, with petroleum ether filter cake, the dry white dry powder that must contain nimbin 23%, nimbin extraction rate reached 0.29%.
And pulverize kind of benevolence with the squeezing degreasing is that raw material is by extracting with quadrat method, promptly soaked 12 hours with ethyl acetate, the back is stirred and is extracted four times, filtrate merges, and vacuum concentration is removed ethyl acetate, adds 4-8 and doubly plant benevolence quality sherwood oil (boiling range is 60-90 ℃) in enriched material, the adularescent floss produces, filter, with sherwood oil (boiling range is 60-90 ℃) washing leaching cake, the dry product that gets, its nimbin extraction yield has only 0.17%.
Embodiment 4
Remove the not mouldy neem kernel 100g of skin, softened 12 hours with the 200ml alcohol immersion, pulverizing is stirred with nine positive household soy milk machines cuttings in the back in ethanol medium, and stirring is extracted four times, filtrate merges, vacuum concentration is removed ethanol, adds 4-8 and doubly plants benevolence quality sherwood oil (boiling range is 60-90 ℃), the adularescent floss produces, filter, with sherwood oil (boiling range is 60-90 ℃) washing leaching cake, the dry white powder that must contain nimbin 19%, nimbin extraction rate reached 0.46%.
And with the squeezing degreasing pulverize kind of benevolence be raw material by extracting with quadrat method, its nimbin extraction yield has only 0.28%.
Embodiment 5
Remove the not mouldy neem kernel 100g of skin, soak softening with 200ml methyl alcohol, pulverizing is stirred with nine positive household soy milk machine cuttings in the back in METHANOL MEDIUM, stir and extract four times, filtrate merges, vacuum concentration is removed methyl alcohol, adds suitable water and suitable ethyl acetate and carry out liquid phase-liquid phase distribution in concentrated solution, and water continues to use ethyl acetate extraction, ethyl acetate merges mutually, use the dewatering agent drying, vacuum is removed ethyl acetate, adds 4-8 and doubly plants benevolence quality sherwood oil (boiling range is 60-90 ℃), the adularescent floss produces in the mixed solution, filter, use the petroleum ether filter cake, the dry white dry powder that must contain nimbin 20%, nimbin extraction rate reached 0.54%.
And with the squeezing degreasing pulverize kind of benevolence be raw material by extracting with quadrat method, its nimbin extraction yield has only 0.30%.
Remove the not mouldy neem kernel 50g of skin, soaked softening 12 hours with the 100ml ethyl acetate, pulverize with nine positive soybean milk maker cutting stirrings in the ethyl acetate medium back, filters filtrate, filter cake disperses with the 100ml ethyl acetate, under certain power condition, ultrasonic power (ultrasonic a minute, intermittently a minute) is set, carry out supersound extraction, reach the setting-up time after-filtration, filter cake adds new solvent and repeats supersound extraction, so repeats four times.The method of aftertreatment is with example one, and the nimbin extraction yield is 0.31%.
Remove the not mouldy neem kernel 50g of skin, softening with the 100ml alcohol immersion, pulverizing is stirred with nine positive household soy milk machine cuttings in the back in ethanol medium, filter filtrate, filter cake disperses with 100ml ethanol, under certain power condition, ultrasonic power (ultrasonic a minute, intermittently a minute) is set, carry out supersound extraction, reach the design time after-filtration, filter cake adds new solvent and repeats supersound extraction, so repeats four times.The method of aftertreatment is with example three, and the nimbin extraction yield is 0.49%.
Remove the not mouldy neem kernel 50g of skin, softening with the immersion of 100ml methyl alcohol, pulverizing is stirred with nine positive household soy milk machines cuttings in the back in METHANOL MEDIUM, filter filtrate, filter cake disperses with 100ml methyl alcohol, under certain power condition, ultrasonic power (ultrasonic a minute, intermittently a minute) is set, carry out supersound extraction, reach the design time after-filtration, filter cake adds new solvent and repeats supersound extraction, so repeats four times.The method of aftertreatment is with example two, and the nimbin extraction yield is 0.56%.
The typing expert evidence
Select Kromasil-C18 stratographic analysis post (4.0mm * 250mm for use, 10 μ m), with methyl alcohol: water (V: V)=65: 35 be moving phase, selecting UV-detector, detection wavelength for use is 217nm, flow velocity is 1mL/min, under the normal temperature condition, to the standard reference material of nimbin A and extract sample and carry out stratographic analysis, the most of peak that extracts in the sample is all effectively separated and favorable reproducibility, and the retention time of nimbin A is about 5.8min.The extraction sample of nimbin A and the high pressure liquid chromatography figure of standard reference material is following (sees Fig. 1, Fig. 2).
Claims (4)
1. the extracting method of a nimbin is characterized in that may further comprise the steps,
The first step, the polar organic solvent of doubly removing the peel the neem kernel quality with 3-5 soaked the peeling neem kernel 6-12 hour,
Second step, in above-mentioned polar organic solvent, adopt the high speed blade cut to stir and pulverize the extraction nimbin, refilter, obtain extracting solution and filter cake,
In the 3rd step, extracting solution at 10～40 ℃ of following vacuum concentration, is removed the enriched material that polar organic solvent obtains containing nimbin.
2. the extracting method of nimbin according to claim 1, it is characterized in that after second step obtained filter cake, adding polar organic solvent that 3-5 doubly removes the peel the neem kernel quality in filter cake continues to stir and extracted 3-5 hour, filter, obtain extracting solution and filter cake, again filter cake is repeated to extract 2-5 time according to identical method, again extracting solution is merged.
3. according to the extracting method of the described nimbin of claim 1, the enriched material that it is characterized in that claim 1 is obtained containing nimbin is purified, step is: the 4-8 sherwood oil doubly that adds peeling neem kernel quality in the described enriched material, adularescent floss precipitation produces, filter, after petroleum ether precipitation, drying, must contain the white dry powder of nimbin, above-mentioned sherwood oil boiling range is 60-90 ℃.
4. the extracting method of nimbin according to claim 1, it is characterized in that, in second step, in the polar organic solvent medium, adopt the high speed blade cut to stir when pulverizing neem kernel, produced cooling of thermal recovery chuck or coil pipe cooling when avoiding high-speed stirring to pulverize.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100411447A CN100448871C (en) | 2006-08-08 | 2006-08-08 | Method for extracting nimbin |
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| CNB2006100411447A CN100448871C (en) | 2006-08-08 | 2006-08-08 | Method for extracting nimbin |
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| CN1907986A CN1907986A (en) | 2007-02-07 |
| CN100448871C true CN100448871C (en) | 2009-01-07 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102887911A (en) * | 2012-11-06 | 2013-01-23 | 白林 | Azadirachtin extraction method |
| CN107522721A (en) * | 2017-08-28 | 2017-12-29 | 云南大学 | A kind of technique of efficiently purification nimbin raw medicine |
| CN107474648A (en) * | 2017-08-29 | 2017-12-15 | 河北晨阳工贸集团有限公司 | A kind of natural botanical extraction liquid repelling mosquitoes and preventing insects health care coating and preparation method thereof |
| CN114874239A (en) * | 2022-04-29 | 2022-08-09 | 保山嘉宏生物科技有限公司 | Method for extracting high-purity azadirachtin |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5397571A (en) * | 1993-03-25 | 1995-03-14 | W. R. Grace & Co.-Conn. | Co-extraction of azadirachtin and neem oil |
| US5736145A (en) * | 1995-07-17 | 1998-04-07 | Dalmia Centre For Biotechnology | Process for preparing purified Azadirachtin in powder form from neem seeds and storage stable aqueous composition containing Azadirachtin |
| EP0834254A1 (en) * | 1996-10-02 | 1998-04-08 | Council of Scientific and Industrial Research | Azadirachtin formulations and a process for preparing them from neem seed/kernel |
| US6193974B1 (en) * | 1995-07-17 | 2001-02-27 | Dalmia Center For Research And Development | Process of preparing purified azadirachtin in powder form from neem seeds and storage stable aqueous composition containing azadirachtin |
| CN1423938A (en) * | 2002-12-02 | 2003-06-18 | 华南农业大学 | Preparation for high-content nimbin powder |
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2006
- 2006-08-08 CN CNB2006100411447A patent/CN100448871C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5397571A (en) * | 1993-03-25 | 1995-03-14 | W. R. Grace & Co.-Conn. | Co-extraction of azadirachtin and neem oil |
| US5736145A (en) * | 1995-07-17 | 1998-04-07 | Dalmia Centre For Biotechnology | Process for preparing purified Azadirachtin in powder form from neem seeds and storage stable aqueous composition containing Azadirachtin |
| US6193974B1 (en) * | 1995-07-17 | 2001-02-27 | Dalmia Center For Research And Development | Process of preparing purified azadirachtin in powder form from neem seeds and storage stable aqueous composition containing azadirachtin |
| EP0834254A1 (en) * | 1996-10-02 | 1998-04-08 | Council of Scientific and Industrial Research | Azadirachtin formulations and a process for preparing them from neem seed/kernel |
| CN1423938A (en) * | 2002-12-02 | 2003-06-18 | 华南农业大学 | Preparation for high-content nimbin powder |
Non-Patent Citations (4)
| Title |
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| 4种提取印楝素方法的比较. 段琼芬等.农药，第44卷第10期. 2005 |
| 4种提取印楝素方法的比较. 段琼芬等.农药，第44卷第10期. 2005 * |
| 溶剂法萃取印楝素的研究进展. 王秋芬等.精细与专用化学品，第16期. 2003 |
| 溶剂法萃取印楝素的研究进展. 王秋芬等.精细与专用化学品，第16期. 2003 * |
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