CN104058988B - Utilize two-phase abstraction technique from chilli extract, extract the method for capsicine - Google Patents
Utilize two-phase abstraction technique from chilli extract, extract the method for capsicine Download PDFInfo
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- CN104058988B CN104058988B CN201410287885.8A CN201410287885A CN104058988B CN 104058988 B CN104058988 B CN 104058988B CN 201410287885 A CN201410287885 A CN 201410287885A CN 104058988 B CN104058988 B CN 104058988B
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- capsicine
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- salt
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- YKPUWZUDDOIDPM-SOFGYWHQSA-N capsaicin Chemical compound COC1=CC(CNC(=O)CCCC\C=C\C(C)C)=CC=C1O YKPUWZUDDOIDPM-SOFGYWHQSA-N 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000000284 extract Substances 0.000 title claims abstract description 29
- 240000004160 Capsicum annuum Species 0.000 title claims abstract 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000000605 extraction Methods 0.000 claims abstract description 28
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims abstract description 18
- 239000007787 solid Substances 0.000 claims abstract description 15
- 235000015320 potassium carbonate Nutrition 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 239000008346 aqueous phase Substances 0.000 claims description 29
- 239000012071 phase Substances 0.000 claims description 22
- 230000009514 concussion Effects 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 abstract description 6
- 239000012141 concentrate Substances 0.000 abstract description 5
- 238000001291 vacuum drying Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000004821 distillation Methods 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- 240000008574 Capsicum frutescens Species 0.000 description 13
- 238000005516 engineering process Methods 0.000 description 5
- QNEFNFIKZWUAEQ-UHFFFAOYSA-N carbonic acid;potassium Chemical compound [K].OC(O)=O QNEFNFIKZWUAEQ-UHFFFAOYSA-N 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 235000002566 Capsicum Nutrition 0.000 description 3
- XJQPQKLURWNAAH-UHFFFAOYSA-N dihydrocapsaicin Chemical compound COC1=CC(CNC(=O)CCCCCCC(C)C)=CC=C1O XJQPQKLURWNAAH-UHFFFAOYSA-N 0.000 description 3
- RBCYRZPENADQGZ-UHFFFAOYSA-N dihydrocapsaicin Natural products COC1=CC(COC(=O)CCCCCCC(C)C)=CC=C1O RBCYRZPENADQGZ-UHFFFAOYSA-N 0.000 description 3
- -1 methyl capsicine Chemical compound 0.000 description 3
- VQEONGKQWIFHMN-UHFFFAOYSA-N Nordihydrocapsaicin Chemical compound COC1=CC(CNC(=O)CCCCCC(C)C)=CC=C1O VQEONGKQWIFHMN-UHFFFAOYSA-N 0.000 description 2
- 239000001390 capsicum minimum Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- 239000006002 Pepper Substances 0.000 description 1
- 235000016761 Piper aduncum Nutrition 0.000 description 1
- 235000017804 Piper guineense Nutrition 0.000 description 1
- 244000203593 Piper nigrum Species 0.000 description 1
- 235000008184 Piper nigrum Nutrition 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000036592 analgesia Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000036528 appetite Effects 0.000 description 1
- 235000019789 appetite Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- 229960002504 capsaicin Drugs 0.000 description 1
- 235000017663 capsaicin Nutrition 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 229920001477 hydrophilic polymer Polymers 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 239000002858 neurotransmitter agent Substances 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 235000019633 pungent taste Nutrition 0.000 description 1
- 238000005185 salting out Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to biomedicine field, particularly disclose a kind of method utilizing aqueous two phase extraction technique to extract capsicine from chilli extract.The method is raw material with chilli extract, it is characterized in that: get appropriate chilli extract, adds ethanol and salt of wormwood aqueous two-phase system, mixes, is divided into upper and lower two-phase; Take out the ethanol phase containing a large amount of capsicine, carry out underpressure distillation to it and concentrate, vacuum-drying, obtains solid capsicine.The present invention can operate at normal temperatures, improves the extraction yield of capsicine, and organic solvent used is less, and method not only economy but also simple to operate itself, is applicable to suitability for industrialized production.
Description
(1) technical field
The invention belongs to biomedicine field, particularly a kind of method utilizing two-phase abstraction technique to extract capsicine from chilli extract.
(2) background technology
Pungency component in pepper fruit is the capsaicinoid of a class based on capsicine, they are respectively: capsicine, Dihydrocapsaicin, Nordihydrocapsaicin, homocpsaicin and to methyl capsicine, to methyl capsicine alkene chain, to methyl capsicine saturated aliphatic hydrocarbon, p-methylphenyl capsicine etc., wherein based on capsicine, capsicine (capsaicin) and Dihydrocapsaicin (Dihydrocapsaicin) account for more than 90% of total amount.Capsicine has analgesia, anti-inflammatory, promotion appetite, improves digestion, antibacterial desinsection and to pharmacological actions such as the selectivity of neurotransmitter.Based on the character being soluble in organic solvent and basic solution of capsicine, the extraction of capsicine mainly contains organic solvent extraction, acid-base method, supercritical carbon dioxide extraction, Enzymatic Extraction, salting-out process, carbon tetrachloride method, benzene method etc., and organic solvent extractionprocess is combined the research having carried out ultrasound-enhanced extraction, microwave extraction, homogenate extraction capsicine by researchist with multiple auxiliary extraction technology.Although these methods or have that extraction yield is low, the shortcoming that is not suitable for suitability for industrialized production or simple to operate, disposable input is excessive.
Aqueous two phase extraction technique (Two-aqueousphaseextraction) is that hydrophilic polymers different for two kinds of chemical structures or polymkeric substance and inorganic salt are formed immiscible two-phase in water, distribute the object reaching isolation of target substances in two alternate selectivity according to material, it is the extremely promising new separation technology of one, the method has the activity that can retain product, operation can serialization, energy consumption is low, and process capacity is large and be easy to the advantage that expands.
(3) summary of the invention
The present invention, in order to make up the deficiencies in the prior art, provides the two-phase abstraction technique that utilizes that a kind of consumption of organic solvent is few, product yield is high from chilli extract, extracts the method for capsicine.
The present invention is achieved through the following technical solutions:
Utilize two-phase abstraction technique from chilli extract, extract a method for capsicine, be raw material with chilli extract, comprise the steps:
(1) get salt of wormwood be dissolved in Bloomsbury smooth-Robison's buffered soln in, add ethanol, after mixing, obtain ethanol-salt of wormwood double-aqueous phase system;
(2) chilli extract is joined in ethanol-salt of wormwood double-aqueous phase system, be placed in shaking table concussion and extract;
(3) until double water-phase extract system centrifugal after become complete mutually, take out be rich in capsicine ethanol on phase, in matrass, carry out concentrating under reduced pressure;
(4) concentrated solution drying is obtained solid capsicine.
The present invention utilize capsicine in ethanol-salt of wormwood double-aqueous phase system up and down phase selectivity distribute, reach the object of rapidly and efficiently extracting capsicum alkali.
More excellent technical scheme of the present invention is:
In step (1), in ethanol-salt of wormwood double-aqueous phase system, the weight fraction of salt of wormwood is 17-30%, and the weight fraction of ethanol is 17-25%, and Bloomsbury is smooth-and the pH value of Robison's buffered soln is 2-5, and temperature is 25 DEG C.
In step (2), the addition of chilli extract accounts for the 3-6% of ethanol-salt of wormwood double-aqueous phase system weight, and concussion extraction time is 30-90min.
In step (3), the vacuum tightness of concentrating under reduced pressure is 0.1MPa, and temperature is 30-45 DEG C.
Extraction yield is calculated by the content of Determination of Capsaicinoids by High Performance Liquid Chromatography in above-mentioned technique, in Shimadzu LC-20AHPLC system, ODS post (InersilODS-3,4.6 × 250mm, 5 μm), with 75%(v/v) methanol aqueous solution be moving phase, flow velocity is 1mL/min, and column temperature is room temperature, sample feeding amount is 20 μ L, detector is diode-array detector, and determined wavelength is 280nm, for liquid phase measure sample all through the membrane filtration of 0.45 μm.Technique of the present invention, the extraction yield of capsicine can reach 85-91%.
Compared with prior art, technical progress of the present invention is:
(1) technique of technology aqueous two-phase extraction capsicine of the present invention, easy and simple to handle, is suitable for suitability for industrialized production.
(2) process of aqueous two-phase extraction capsicum class material is carried out at normal temperatures, saved the consumption of the energy, reduced cost, decreased the destruction to capsicine molecular structure simultaneously.
(3) the technology of the present invention shortens extraction time, improves the extraction efficiency of capsicine.
(4) the technology of the present invention improves the extraction yield of capsicine, and greatly reduces the consumption of organic solvent.
(4) embodiment
Embodiment 1:
Under (1) 25 DEG C of condition, the solid carbonic acid potassium accounting for double-aqueous phase system total mass 25% is dissolved in pH be 2 Bloomsbury smooth-Robison's buffered soln in, adding analytical pure ethanol after dissolving completely makes the content of ethanol be 18% of double-aqueous phase system total mass, mixes rear one-tenth double-aqueous phase system.
(2) chilli extract getting the total mass 3% accounting for double-aqueous phase system joins in ethanol-salt of wormwood double-aqueous phase system, is placed in shaking table mechanical shaking extraction 30min.
(3) double water-phase is extracted the centrifugal 10min of system, take out be rich in capsicine ethanol in matrass, carry out concentrating under reduced pressure.
(4) decompressed concentrate obtained is placed in the dry 24h of vacuum drying oven and obtains solid capsicine.The capsicine dissolution of solid obtained is analyzed in 70% methyl alcohol the content of capsicine and the extraction yield calculating capsicine is 91%.
Embodiment 2:
Under (1) 25 DEG C of condition, the solid carbonic acid potassium accounting for double-aqueous phase system total mass 30% is dissolved in pH be 3 Bloomsbury smooth-Robison's buffered soln in, adding analytical pure ethanol after dissolving completely makes the content of ethanol be 25% of double-aqueous phase system total mass, mixes rear one-tenth double-aqueous phase system.
(2) chilli extract getting the total mass 4% accounting for double-aqueous phase system joins in ethanol-salt of wormwood double-aqueous phase system, is placed in shaking table mechanical shaking extraction 50min.
(3) double water-phase is extracted the centrifugal 10min of system, take out be rich in capsicine ethanol in matrass, carry out concentrating under reduced pressure.
(4) decompressed concentrate obtained is placed in the dry 24h of vacuum drying oven and obtains solid capsicine.The capsicine dissolution of solid obtained is analyzed in 70% methyl alcohol the content of capsicine and the extraction yield calculating capsicine is 89%.
Embodiment 3:
Under (1) 25 DEG C of condition, the solid carbonic acid potassium accounting for double-aqueous phase system total mass 20% is dissolved in pH be 2 Bloomsbury smooth-Robison's buffered soln in, adding analytical pure ethanol after dissolving completely makes the content of ethanol be 20% of double-aqueous phase system total mass, mixes rear one-tenth double-aqueous phase system.
(2) chilli extract getting the total mass 3% accounting for double-aqueous phase system joins in ethanol-salt of wormwood double-aqueous phase system, is placed in shaking table mechanical shaking extraction 60min.
(3) double water-phase is extracted the centrifugal 10min of system, take out be rich in capsicine ethanol in matrass, carry out concentrating under reduced pressure.
(4) decompressed concentrate obtained is placed in the dry 24h of vacuum drying oven and obtains solid capsicine.The capsicine dissolution of solid obtained is analyzed in 70% methyl alcohol the content of capsicine and the extraction yield calculating capsicine is 92.5%.
Embodiment 4:
Under (1) 25 DEG C of condition, the solid carbonic acid potassium accounting for double-aqueous phase system total mass 17.5% is dissolved in pH be 5 Bloomsbury smooth-Robison's buffered soln in, adding analytical pure ethanol after dissolving completely makes the content of ethanol be 23% of double-aqueous phase system total mass, mixes rear one-tenth double-aqueous phase system.
(2) chilli extract getting the total mass 6% accounting for double-aqueous phase system joins in ethanol-salt of wormwood double-aqueous phase system, is placed in shaking table mechanical shaking extraction 40min.
(3) double water-phase is extracted the centrifugal 10min of system, take out be rich in capsicine ethanol in matrass, carry out concentrating under reduced pressure.
(4) decompressed concentrate obtained is placed in the dry 24h of vacuum drying oven and obtains solid capsicine.The capsicine dissolution of solid obtained is analyzed in 70% methyl alcohol the content of capsicine and the extraction yield calculating capsicine is 86%.
What the double water-phase extraction method of embodiment and traditional basic solvent extraction method extracted capsicine is compared as follows shown in table:
。
Claims (3)
1. the method utilizing two-phase abstraction technique to extract capsicine from chilli extract, be raw material with chilli extract, it is characterized by, comprise the steps: (1) get salt of wormwood be dissolved in Bloomsbury smooth-Robison's buffered soln in, add ethanol, after mixing, obtain ethanol-salt of wormwood double-aqueous phase system; In ethanol-salt of wormwood double-aqueous phase system, the weight fraction of salt of wormwood is 17-30%, and the weight fraction of ethanol is 17-25%, and Bloomsbury is smooth-and the pH value of Robison's buffered soln is 2-5, and temperature is 25 DEG C; (2) chilli extract is joined in ethanol-salt of wormwood double-aqueous phase system, be placed in shaking table concussion and extract; (3) until double water-phase extract system centrifugal after become complete mutually, take out be rich in capsicine ethanol on phase, in matrass, carry out concentrating under reduced pressure; (4) concentrated solution drying is obtained solid capsicine.
2. the method utilizing two-phase abstraction technique to extract capsicine from chilli extract according to claim 1, it is characterized in that: in step (2), the addition of chilli extract accounts for the 3-6% of ethanol-salt of wormwood double-aqueous phase system weight, and concussion extraction time is 30-90min.
3. the method utilizing two-phase abstraction technique to extract capsicine from chilli extract according to claim 1, is characterized in that: in step (3), the vacuum tightness of concentrating under reduced pressure is 0.1MPa, and temperature is 30-45 DEG C.
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| CN201410287885.8A CN104058988B (en) | 2014-06-25 | 2014-06-25 | Utilize two-phase abstraction technique from chilli extract, extract the method for capsicine |
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| CN201410287885.8A CN104058988B (en) | 2014-06-25 | 2014-06-25 | Utilize two-phase abstraction technique from chilli extract, extract the method for capsicine |
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| CN105712898B (en) * | 2016-01-28 | 2018-05-01 | 罗建锟 | The method that natural capsicum element is extracted from capsicum |
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|---|---|---|---|---|
| CN1053803A (en) * | 1991-03-18 | 1991-08-14 | 贵阳市云岩区农副业生产基地 | The production method of natural chilli pigment |
| CN1059742A (en) * | 1990-09-11 | 1992-03-25 | 周建功 | Extract capsochrome and peppery plain processing method by capsicum |
| EP0540629B1 (en) * | 1990-07-20 | 1994-05-04 | L'oreal | Use of pyrimidine 3-oxyde derivatives to slow down hair fall and topical compositions implemented |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2719440B2 (en) * | 1990-11-15 | 1998-02-25 | 新紀産業 株式会社 | How to treat textiles |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0540629B1 (en) * | 1990-07-20 | 1994-05-04 | L'oreal | Use of pyrimidine 3-oxyde derivatives to slow down hair fall and topical compositions implemented |
| CN1059742A (en) * | 1990-09-11 | 1992-03-25 | 周建功 | Extract capsochrome and peppery plain processing method by capsicum |
| CN1053803A (en) * | 1991-03-18 | 1991-08-14 | 贵阳市云岩区农副业生产基地 | The production method of natural chilli pigment |
Non-Patent Citations (2)
| Title |
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| 双水相/三液相萃取分离天然产物有效成分;张华;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20100715(第7期);第28页倒数第1-2段，第29页第1段，第37页倒数第1段，第39页倒数第1段 * |
| 碱性乙醇法提取辣椒碱的工艺研究;张郁松;《食品研究与开发》;20090131;第30卷(第1期);第70-73页 * |
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