CN1458153A - Process for extracting piperine - Google Patents
Process for extracting piperine Download PDFInfo
- Publication number
- CN1458153A CN1458153A CN 02119672 CN02119672A CN1458153A CN 1458153 A CN1458153 A CN 1458153A CN 02119672 CN02119672 CN 02119672 CN 02119672 A CN02119672 A CN 02119672A CN 1458153 A CN1458153 A CN 1458153A
- Authority
- CN
- China
- Prior art keywords
- piperine
- temperature
- solution
- pepper
- coarse crystallization
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- WVWHRXVVAYXKDE-UHFFFAOYSA-N piperine Natural products O=C(C=CC=Cc1ccc2OCOc2c1)C3CCCCN3 WVWHRXVVAYXKDE-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 235000019100 piperine Nutrition 0.000 title claims abstract description 52
- MXXWOMGUGJBKIW-YPCIICBESA-N piperine Chemical compound C=1C=C2OCOC2=CC=1/C=C/C=C/C(=O)N1CCCCC1 MXXWOMGUGJBKIW-YPCIICBESA-N 0.000 title claims abstract description 50
- 229940075559 piperine Drugs 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 235000008184 Piper nigrum Nutrition 0.000 claims abstract description 23
- 235000002566 Capsicum Nutrition 0.000 claims abstract description 21
- 239000006002 Pepper Substances 0.000 claims abstract description 21
- 241000722363 Piper Species 0.000 claims abstract description 21
- 235000016761 Piper aduncum Nutrition 0.000 claims abstract description 21
- 235000017804 Piper guineense Nutrition 0.000 claims abstract description 21
- 238000002425 crystallisation Methods 0.000 claims abstract description 17
- 230000008025 crystallization Effects 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 14
- 238000004821 distillation Methods 0.000 claims abstract description 8
- 239000007791 liquid phase Substances 0.000 claims description 10
- 238000007654 immersion Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 7
- 239000007790 solid phase Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 210000001124 body fluid Anatomy 0.000 claims description 3
- 239000010839 body fluid Substances 0.000 claims description 3
- 238000005352 clarification Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000003204 osmotic effect Effects 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 238000001953 recrystallisation Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000003828 vacuum filtration Methods 0.000 claims description 2
- 238000002386 leaching Methods 0.000 abstract description 6
- 238000000605 extraction Methods 0.000 abstract description 4
- 239000000654 additive Substances 0.000 abstract description 2
- 230000000996 additive effect Effects 0.000 abstract description 2
- 230000002411 adverse Effects 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- 210000002784 stomach Anatomy 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 230000002936 tranquilizing effect Effects 0.000 abstract description 2
- 206010061218 Inflammation Diseases 0.000 abstract 1
- 230000003467 diminishing effect Effects 0.000 abstract 1
- 229940079593 drug Drugs 0.000 abstract 1
- 230000004054 inflammatory process Effects 0.000 abstract 1
- 230000007721 medicinal effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 19
- 235000019441 ethanol Nutrition 0.000 description 18
- 238000001035 drying Methods 0.000 description 3
- 235000008534 Capsicum annuum var annuum Nutrition 0.000 description 2
- 240000008384 Capsicum annuum var. annuum Species 0.000 description 2
- 244000203593 Piper nigrum Species 0.000 description 2
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- 235000013614 black pepper Nutrition 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000001931 piper nigrum l. white Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 210000000952 spleen Anatomy 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
- Seasonings (AREA)
Abstract
The present invention discloses a process of extracting piperine from pepper. The extraction process includes crushing pepper into pepper powder, lixiviating with edible alcohol to obtain leaching liquor, distillation to separate alcohol and obtain brown concentrated solution, adding alcohol for coarse crystallization, further purification to obtain crystallized piperine. Piperine as one chemical component in pepper has the unique medicinal effects of tranquilizing mind, worming stomach, expelling cold, appetizing, keeping the adverse energy downwards, diminishing inflammation, etc. and is used as intermediate and additive in preparing several medicines. The said process can extract high purity piperine in high yield.
Description
The present invention relates to a kind of method of from pepper, extracting piperine.
Piperine is a kind of chemical ingredients in the pepper, has unique drug effects such as tranquilizing and allaying excitement, warming spleen and stomach for dispelling cold, the appetizing therapeutic method to keep the adverse qi flowing downward, anti-inflammatory, detoxifcation, is essential intermediate and the additive of multiple medicine in the pharmaceutical industry.Piperine has immeasurable using value in pharmaceutical industries.At present, the process of extracting piperine from pepper adopts the process of lixiviate, Crystallization Separation more, but use left standstill immersion more in leaching process, so the leaching yield of piperine is lower.When crystallization, add to wash, but it has promoted the hydrolysis of piperine simultaneously into basic solution, gained piperine first product purity difference, fusing point is on the low side, the recrystallization difficulty, the yielding poorly of last gained piperine, purity is low.
The purpose of this invention is to provide a kind of method of extracting piperine from pepper, this method can improve the extraction yield of piperine, reduces the extraction cost of piperine.And production technique is simple.
In order to achieve the above object, technical scheme proposed by the invention is: get the pepper dry powder and be broken into the pepper powder, under the situation of normal temperature or heating, soak the pepper powder with a certain amount of edible ethanol then, in immersion process, mixture is interrupted or the successive stirring, after after a while, liquid phase in the mixture is separated with solid phase, separate the resulting liquid phase in back and be vat liquor; Repeat above-mentioned immersion and sepn process, be clarification, transparent state until soaking body fluid.All vat liquor is merged and carry out air distillation, isolate alcohol wherein, the resulting tan solution that contains piperine.In the tan solution of gained, add a certain amount of edible ethanol again, reduce temperature then gradually, in solution, add a spot of piperine crystal seed simultaneously, make piperine in temperature-fall period from solution coarse crystallization and separating quickly.A certain amount of alcohol joined in the piperine coarse crystallization body carry out heat of solution, and then decrease temperature crystalline, purer piperine crystal both can have been obtained.
The extracting method technology of the piperine that the present invention proposes is simple, and required equipment is simple, the piperine output height of extraction, purity height.
Fig. 1 is a piperine extracting method process flow sheet.
The invention will be further described below in conjunction with accompanying drawing.
1, the pulverizing of pepper. The pepper dry fruit of learning from else's experience selected is ground into recklessly after clean the drying The green pepper powder.
2, the lixiviate of pepper powder. With 1-4 doubly to the edible wine of pepper powder weight Essence is soaked the pepper powder at normal temperature or heating in the temperature range below 40 ℃, soaking Make mixture keep being interrupted or continuous stirring with the screw mixing oar in the journey, soaking 1-4 After hour, the solid phase in the mixture is separated with liquid phase, the gained liquid phase is after separating Leaching liquor. Its separation method is first naturally osmotic, utilizes then the principle of multistage natural subsidence Tiny solid particle separation in the solution is come out, then adopt the mode of vacuum filtration with molten Solid phase in the liquid is separated fully with liquid phase, obtains leaching liquor. Repeat above-mentioned immersion and separated Journey is until leaching liquor is clarification, transparent state.
3, soak the distillation of body fluid.Above-mentioned all vat liquors that obtain are joined in the still kettle, in 78 ℃-85 ℃ temperature range, carry out air distillation, isolate alcohol wherein, can obtain containing the tan solution of piperine.
4, the coarse crystallization of piperine.Add edible ethanol in above-mentioned resulting tan solution, the ratio of edible ethanol and brown solution is by weight calculating 0.2: 1-1: between 1, utilize the method for temperature programmed control to make its temperature evenly with low then.Reach 0 ℃ until temperature, in cooling, in solution, add a spot of piperine crystal seed, make piperine coarse crystallization and it is separated quickly from solution.
5, the purification of piperine.Add edible ethanol and carry out heat of solution in resulting piperine coarse crystallization body, the ratio of edible ethanol and piperine coarse crystallization is by weight calculating 0.1: 1-0.5: between 1.And then decrease temperature crystalline, can improve crystalline purity like this.Repeatedly repeat this step, can obtain purity greater than 90% piperine xln.
Embodiment 1
Get double centner Qionghai white pepper and clean and to be ground into pepper powder after drying, soak with 200 kilograms of edible ethanols then, every 30 minutes with spiral stirring rake stirring 5 minutes, after 2 hours solid phase in the mixture is separated with the liquid phase row.Repeat immersion and sepn process 4 times.All vat liquors are merged and under 78 ℃-85 ℃ temperature, carry out air distillation, after steaming alcohol, can obtain the tan solution that contains piperine.In this solution, add the alcohol of isodose, carry out uniform decrease in temperature, in cooling, add the piperine crystal seeds of 5 grams according to 2 ℃/minute speed, near 0 ℃ the time, but just coarse crystallization and separating of piperine.Coarse crystallization body and function edible ethanol is carried out heat of solution and decrease temperature crystalline repeatedly, can obtain purity at last and be 1.5 kilograms of 90% piperines.
Embodiment 2
Get the clean back of drying of double centner Qionghai piper nigrum and pulverize poling green pepper powder, soak pepper powder at normal temperatures with 300 kilograms of edible ethanols then, in immersion process,, after 1 hour the solid phase in the mixture is separated with liquid phase with spiral stirring rake continuously stirring.Repeat above-mentioned immersion and sepn process 4 times.All vat liquors are merged and under 78 ℃-85 ℃ temperature, carry out air distillation.After distilling out alcohol, can obtain the tan solution that contains piperine.Add edible ethanol in this solution, the ratio of edible ethanol and this solution is 3: 10, carries out uniform decrease in temperature according to 10 ℃/minute speed, adds the piperine crystal seeds of 3 grams in cooling, near 0 ℃ the time, but just coarse crystallization and separating of piperine.Coarse crystallization body and function edible ethanol is carried out heat of solution and decrease temperature crystalline repeatedly, can obtain purity at last and be 2 kilograms of 90% piperines.
Claims (4)
1, a kind of extracting method of piperine is characterized in that getting selected pepper dry powder and is broken into the pepper powder; Then with edible ethanol by weight with 1: 1-4: 1 ratio is soaked the pepper powder at normal temperature or heating in the temperature range below 40 ℃, in immersion process, be interrupted or successional stirring, after soaking 1-4 hour, solid phase in the mixture is separated with liquid phase, and the gained liquid phase is vat liquor; Repeat above-mentioned immersion and sepn process, till vat liquor is clarification, transparent state; All vat liquors that obtain are merged and carry out air distillation, isolate alcohol wherein, obtain the tan concentrated solution that contains piperine; In above-mentioned concentrated solution, add edible ethanol while hot then, the ratio of edible ethanol and concentrated solution is 0.2: 1-1: between 1, its temperature is reduced, in cooling, add a spot of piperine crystal seed, reach 0 ℃ until temperature, can obtain piperine coarse crystallization body and it is separated; Then by 0.1: 1-0.5: 1 part by weight adds edible ethanol and carries out heat of solution in piperine coarse crystallization body, and then decrease temperature crystalline; Repeat repeatedly heat of solution, the recrystallization process of above-mentioned piperine coarse crystallization body, can obtain purity greater than 90% piperine xln.
2, the extracting method of piperine according to claim 1, it is characterized in that the said separation method that soaks body fluid is first naturally osmotic, utilize the principle of multistage natural subsidence that the tiny solid particle in the solution is separated then, with the mode of vacuum filtration the solid phase in the solution is separated fully with liquid phase again.
3, the extracting method of piperine according to claim 1, the temperature that it is characterized in that said air distillation process are between 78 ℃-85 ℃.
4, the extracting method of piperine according to claim 1 is characterized in that the temperature-fall period in the coarse crystallization of said piperine is to lower the temperature equably with the mode of temperature programmed control.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02119672 CN1458153A (en) | 2002-05-17 | 2002-05-17 | Process for extracting piperine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02119672 CN1458153A (en) | 2002-05-17 | 2002-05-17 | Process for extracting piperine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1458153A true CN1458153A (en) | 2003-11-26 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02119672 Pending CN1458153A (en) | 2002-05-17 | 2002-05-17 | Process for extracting piperine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1458153A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101985440A (en) * | 2010-10-30 | 2011-03-16 | 暨南大学 | Method for producing piperine |
| CN104910127A (en) * | 2015-04-24 | 2015-09-16 | 东北制药集团股份有限公司 | Preparation method of highly pure homopiperonylnitrile |
-
2002
- 2002-05-17 CN CN 02119672 patent/CN1458153A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101985440A (en) * | 2010-10-30 | 2011-03-16 | 暨南大学 | Method for producing piperine |
| CN101985440B (en) * | 2010-10-30 | 2013-05-01 | 暨南大学 | Method for producing piperine |
| CN104910127A (en) * | 2015-04-24 | 2015-09-16 | 东北制药集团股份有限公司 | Preparation method of highly pure homopiperonylnitrile |
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| WD01 | Invention patent application deemed withdrawn after publication |