CN1128145C - Process for preparing piperine - Google Patents
Process for preparing piperine Download PDFInfo
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- CN1128145C CN1128145C CN 00130395 CN00130395A CN1128145C CN 1128145 C CN1128145 C CN 1128145C CN 00130395 CN00130395 CN 00130395 CN 00130395 A CN00130395 A CN 00130395A CN 1128145 C CN1128145 C CN 1128145C
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- piperine
- pepper
- preparing
- organic solvent
- powder
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention provides a preparation method for piperine which is extract of effective chemical components in pepper. The piperine is leached by pepper by two or more kinds of mixed organic solvent, and chemical solvent is separated from the mixed organic solvent by distillation. A mixed product of liquid pepper oil resin and piperine can be obtained. The pepper oil resin is separated from the mixture in a temperature drop cooling method. Moreover, a final product, namely piperine can be obtained by further purification. The piperine extracted by the method has simple technology. The present invention improves extraction rates of the piperine and separation effect, and reduces the extraction cost of the piperine. Moreover, the obtained piperine has high purity.
Description
Technical field
A kind of pepper extracting method or technology have been the present invention relates to.
Background technology
Piperine is a kind of Chemical Composition of most worthy in the pepper, has tranquilizing and allaying excitement, warming spleen and stomach for dispelling cold, and the appetizing therapeutic method to keep the adverse qi flowing downward, the five internal organs are transferred in dissolving phlegm, strong kidney qi, unique effects such as fat-reducing, beauty treatment, detoxifcation.Be used for gastrofrigid vomiting, stomachache is had loose bowels, poor appetite, and epilepsy phlegm is many.And to the rib adenositis, sore is swollen, and venomous snake bite etc. are effective in cure.Treatment chronic tracheitis, asthma, rheumatism, vitiligo, obesity, baby's simple diarrhea there is obvious curative effects.Be the major ingredient of medicine " antiepilepsirin ", still essential intermediate and the additive of multiple medicine in the pharmaceutical industry simultaneously, and, become the insecticide of high-efficiency low-toxicity as the consonance agent of pyrethrum insecticides.Piperine also is widely used in wine brewing and the catering industry and makes additive.
Traditional piperine extraction process is the single solvents that use in leaching process more, and leaching yield is lower; Many by adding mineral alkali/salt (KOH/KCl) stripping oleo-resinous in sepn process, and the hydrolysis of minimizing piperine, and then utilizing ether and ethanol that coarse crystallization is purified, this process operation is more numerous and diverse, and separating effect is not satisfactory.
Summary of the invention
The object of the present invention is to provide a kind of extraction piperine method, it is simple to extract piperine technology with this method, piperine extraction yield and separating effect all obviously are improved, the cost low (ratio for input and output is more than 2: 1) that makes the piperine extraction, and gained piperine purity height (highest purity can reach more than 98%).
The object of the present invention is achieved like this, and promptly extract piperine with step as follows: the black/white pepper dry fruit of learning from else's experience selected is ground into the pepper powder of certain particle size with it; Get the pepper powder of pulverizing, add two or more mixed organic solvents, after the stirring, solid powder is separated with liquid mixture; With distilling in resulting all vat liquors (liquid mixture) adding still kettle, isolate organic solvent wherein.Steam after the organic solvent, the gained enriched material is the pepper oleoresin that contains the higher proportion piperine; The pepper oleoresin that will contain the higher proportion piperine adopts cooling cooling way, and piperine can be crystallized out from mixture smoothly, and resulting coarse crystallization contains a spot of pepper oleoresin.And then adopt Ethylene Dichloride or ethyl acetate equal solvent that resulting coarse crystallization is carried out repeatedly recrystallization and handle, thereby can obtain the very high piperine of purity.
The present invention compared with prior art, its technology is simple, has improved piperine extraction yield and separating effect, has reduced piperine extraction cost (ratio for input and output is more than 2: 1), and gained piperine purity height (highest purity can reach more than 98%).
Embodiment
Below in detail most preferred embodiment of the present invention is described.
1, piperic is pulverized.The black/white pepper dry fruit of learning from else's experience selected is ground into certain particle size (＜2mm) pepper powder.
2, the organic solvent lixiviate of pepper powder.Get the pepper powder of pulverizing, the mixed organic solvents (ratio of organic solvent and pepper powder is 1: 1～6: 1) that adds two or more, under 25 ℃～40 ℃ temperature, under intermittence or continuously stirring effect, through certain hour (t=1～6 hour) afterwards, solid powder (impurity in the pepper) separation is removed, thereby the mixed solution of acquisition pepper oleoresin and organic solvent, separation method can be following method, and two or more combines: press filtration, suction filtration, membrane filtration and chromatographic separation.
3, the distillation of vat liquor.With distilling in the above-mentioned mixed solution adding still kettle, isolate organic solvent wherein.This process can be air distillation, or underpressure distillation, or the rectifying of multistage column plate.Steam after the organic solvent, the gained enriched material is the pepper oleoresin that contains the higher proportion piperine.
4, the Separation ﹠ Purification of piperine.And then adopt Ethylene Dichloride or ethyl acetate equal solvent that resulting coarse crystallization is carried out repeatedly recrystallization and handle, thereby can obtain the very high piperine of purity.
Embodiment 1
Getting 100Kg Qionghai white pepper and being ground into particle diameter is 80 purpose pepper powders, add 300Kg with ethanol and acetone in 1: 1 ratio then and carry out lixiviate, stirred 5 minutes in per 30 minutes, adopted membrane filtration to carry out separating of solid powder and liquid phase later in 2 hours in conjunction with suction filtration.Repeat lixiviate and separating process 4 times.Air distillation is carried out in all vat liquors merging, after steaming organic solvent fully, resulting enriched material is cooled to-10 ℃ (cooling rate is controlled at 1 ℃/minute), an amount of piperine crystal seed that adds in temperature-fall period.Get final product behind this end of processing the piperine coarse crystallization.Afterwards, utilizing Ethylene Dichloride that the piperine coarse crystallization is carried out recrystallization purifies.Obtain the flaxen piperine powder of 3Kg at last, purity is greater than 95%, and fusing point is 129 ℃～131 ℃.
Embodiment 2
Getting 100Kg Qionghai piper nigrum and being ground into particle diameter is 60 purpose pepper powders, add 200Kg with ethanol and ethyl acetate in 2: 1 ratio then and carry out lixiviate, continuously stirring in the leaching process adopted membrane filtration to carry out separating of solid powder and liquid phase in conjunction with suction filtration later in 1 hour.Repeat lixiviate and separating process 4 times.Underpressure distillation is carried out in all vat liquors merging, after steaming organic solvent fully, resulting enriched material is cooled to-10 ℃ (cooling rate is controlled at 1 ℃/minute), an amount of piperine crystal seed that adds in temperature-fall period.Get final product behind this end of processing the piperine coarse crystallization.Afterwards, utilize ethyl acetate and Ethylene Dichloride the piperine coarse crystallization to be carried out the recrystallization purification in the mixed solvent of 2: 1 ratios.Obtain the flaxen piperine powder of 5Kg at last, purity is greater than 95%, and fusing point is 129 ℃～131 ℃.
The piperine extract that the present invention is made and edible oil with after other medicament mixes, can be made into the special effect medicine " antiepilepsirin " of treatment epileptics in about 80% ratio; With the piperine that the present invention makes, the ratio with about 1% is applied in the general medicine as additive, can improve drug effect to a great extent, reduces the consumption of medicament; The piperine that the present invention makes can add in 1% ratio in the drinks goods such as brandy, can strengthen the fragrant hot flavor of wine, this wine and have health care, keep out the cold functions such as wind-damp dispelling; That the piperine that the present invention is made, the ratio in 1%～2% add is anticancer, weight reducing, and medicine such as smoking cessation in, can obviously strengthen the drug effect of medicine.
Annotate: the above ratio all is weight percentage.
Claims (8)
1. process for preparing piperine, this method may further comprise the steps successively: the black/white pepper dry fruit of learning from else's experience selected is ground into the pepper powder of certain particle size with it; Get the pepper powder of pulverizing, add two or more mixed organic solvents, after the mechanical stirring, solid powder is separated with liquid mixture; With distilling in resulting all vat liquors adding still kettles, isolate organic solvent wherein; Steam after the organic solvent, the gained enriched material is the pepper oleoresin that contains the higher proportion piperine; The pepper oleoresin that will contain the higher proportion piperine adopts cooling cooling way, and piperine can be crystallized out from mixture smoothly, and resulting coarse crystallization contains a spot of pepper oleoresin; And then adopt Ethylene Dichloride or ethyl acetate equal solvent that resulting coarse crystallization is carried out repeatedly recrystallization and handle, thereby can obtain the very high piperine of purity.
2. process for preparing piperine according to claim 1 is characterized in that said ground pepper is the pepper powder of particle diameter less than 2mm, and pepper can be piper nigrum or white pepper.
3. process for preparing piperine according to claim 1, the ratio that it is characterized in that described mixed organic solvents and pepper powder is 1: 1～6: 1.
4. process for preparing piperine according to claim 1 is characterized in that organic solvent with after the pepper powder mixes, under 25 ℃～40 ℃ temperature, intermittently or continuously stirring 1～6 hour.
5. process for preparing piperine according to claim 1 is characterized in that it can be combining of following two or more method that solid powder and liquid mixture are carried out isolating method: press filtration, suction filtration, membrane filtration and chromatographic separation.
6, process for preparing piperine according to claim 1, it is characterized in that above-mentioned enriched material, adopt cooling to be cooled to+30 ℃～-10 ℃ way, and in the refrigerative process an amount of piperine crystal seed that adds, make a large amount of piperines to crystallize out from mixture smoothly, resulting coarse crystallization contains a spot of pepper oleoresin.
7, process for preparing piperine according to claim 1 is characterized in that used organic solvent includes ethanol, methyl alcohol, acetone, ether, ethyl acetate, ethylene dichloride, benzene and chloroform.
8. process for preparing piperine according to claim 1 is characterized in that the mechanical stirring mode can be intermittently or continuously stirring.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00130395 CN1128145C (en) | 2000-11-03 | 2000-11-03 | Process for preparing piperine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00130395 CN1128145C (en) | 2000-11-03 | 2000-11-03 | Process for preparing piperine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1294127A CN1294127A (en) | 2001-05-09 |
| CN1128145C true CN1128145C (en) | 2003-11-19 |
Family
ID=4594154
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 00130395 Expired - Fee Related CN1128145C (en) | 2000-11-03 | 2000-11-03 | Process for preparing piperine |
Country Status (1)
| Country | Link |
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| CN (1) | CN1128145C (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102068501B (en) * | 2009-11-24 | 2012-07-25 | 江苏神华药业有限公司 | Black pepper extract, preparation method thereof and application in preparation of medicaments for preventing and treating cough |
| CN101985440B (en) * | 2010-10-30 | 2013-05-01 | 暨南大学 | Method for producing piperine |
| CN103931668B (en) * | 2014-04-08 | 2015-09-09 | 许银亚 | Vaporizer mosquito liquid |
| CN104311530A (en) * | 2014-10-09 | 2015-01-28 | 浙江农林大学 | Method for extracting high-purity piperine with low pollution |
| CN109875109B (en) * | 2019-01-30 | 2020-12-01 | 湖北中烟工业有限责任公司 | Preparation method of allspice oleoresin for cigarettes and application of allspice oleoresin in cigarettes |
| CN113801580A (en) * | 2020-06-11 | 2021-12-17 | 晨光生物科技集团股份有限公司 | Preparation method of low-viscosity pepper oleoresin and pepper oleoresin prepared by preparation method |
| CN111879886B (en) * | 2020-08-07 | 2023-05-05 | 山东省分析测试中心 | Efficient separation and detection method for active components of peppers |
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2000
- 2000-11-03 CN CN 00130395 patent/CN1128145C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1294127A (en) | 2001-05-09 |
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