CN105331291A - Method for raising proportion of capsaicin monomer in capsicum oleoresin - Google Patents
Method for raising proportion of capsaicin monomer in capsicum oleoresin Download PDFInfo
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- CN105331291A CN105331291A CN201510935212.3A CN201510935212A CN105331291A CN 105331291 A CN105331291 A CN 105331291A CN 201510935212 A CN201510935212 A CN 201510935212A CN 105331291 A CN105331291 A CN 105331291A
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- Prior art keywords
- oleoresin capsicum
- capsaicine
- monomer
- capsaicin
- alcoholic solution
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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 147
- 229960002504 capsaicin Drugs 0.000 title claims abstract description 95
- 239000000178 monomer Substances 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 31
- 235000017663 capsaicin Nutrition 0.000 title abstract description 51
- 239000001722 capsicum frutescens oleoresin Substances 0.000 title abstract 7
- 229940050948 capsicum oleoresin Drugs 0.000 title abstract 7
- 239000011347 resin Substances 0.000 claims abstract description 33
- 229920005989 resin Polymers 0.000 claims abstract description 33
- 230000001476 alcoholic effect Effects 0.000 claims abstract description 20
- 239000003960 organic solvent Substances 0.000 claims abstract description 20
- 238000000638 solvent extraction Methods 0.000 claims abstract description 18
- XJQPQKLURWNAAH-UHFFFAOYSA-N dihydrocapsaicin Chemical compound COC1=CC(CNC(=O)CCCCCCC(C)C)=CC=C1O XJQPQKLURWNAAH-UHFFFAOYSA-N 0.000 claims abstract description 14
- RBCYRZPENADQGZ-UHFFFAOYSA-N dihydrocapsaicin Natural products COC1=CC(COC(=O)CCCCCCC(C)C)=CC=C1O RBCYRZPENADQGZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001179 sorption measurement Methods 0.000 claims abstract description 12
- 235000002566 Capsicum Nutrition 0.000 claims description 71
- 241000208293 Capsicum Species 0.000 claims description 70
- 239000001390 capsicum minimum Substances 0.000 claims description 69
- 239000008601 oleoresin Substances 0.000 claims description 65
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 29
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 28
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 21
- 239000003463 adsorbent Substances 0.000 claims description 19
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 238000004587 chromatography analysis Methods 0.000 claims description 8
- 238000004440 column chromatography Methods 0.000 claims description 7
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 4
- 239000005012 oleoresinous Substances 0.000 claims description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 2
- 239000006002 Pepper Substances 0.000 claims description 2
- 235000016761 Piper aduncum Nutrition 0.000 claims description 2
- 235000017804 Piper guineense Nutrition 0.000 claims description 2
- 244000203593 Piper nigrum Species 0.000 claims description 2
- 235000008184 Piper nigrum Nutrition 0.000 claims description 2
- 239000002904 solvent Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 238000010828 elution Methods 0.000 abstract description 4
- 239000010842 industrial wastewater Substances 0.000 abstract 1
- 239000002912 waste gas Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 15
- 238000011084 recovery Methods 0.000 description 9
- 238000001514 detection method Methods 0.000 description 5
- 239000007791 liquid phase Substances 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- VQEONGKQWIFHMN-UHFFFAOYSA-N Nordihydrocapsaicin Chemical compound COC1=CC(CNC(=O)CCCCCC(C)C)=CC=C1O VQEONGKQWIFHMN-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000010898 silica gel chromatography Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 240000008574 Capsicum frutescens Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- -1 carbon chain ester Chemical class 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09F—NATURAL RESINS; FRENCH POLISH; DRYING-OILS; OIL DRYING AGENTS, i.e. SICCATIVES; TURPENTINE
- C09F1/00—Obtaining purification, or chemical modification of natural resins, e.g. oleo-resins
- C09F1/02—Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a method for raising the proportion of capsaicin monomer in capsicum oleoresin. The method comprises the steps of dissolving the capsicum oleoresin obtained through organic solvent extraction and decompressed concentration with an alcoholic solution, injecting the capsicum oleoresin into a chromatographic column filled with macroporous adsorption resin, leaving the capsicum oleoresin standing still for being adsorbed for 2-4 hours, then using an alcoholic solution for elution, conducting decompressed concentration on an elution solution, and obtaining capsicum oleoresin free of peculiar smell, wherein the total capsaicin content is 90-91%, and the proportion of the capsaicin monomers reaches 80-85%; continuing with elution with the alcoholic solution till eluant contains no capsaicin, conducting decompressed concentration on the eluant, and obtaining capsicum oleoresin free of peculiar smell, wherein the total capsaicin content is 93-94%, and the proportion of dihydrocapsaicin monomer reaches 45-50%. The method is obvious in effect, simple in process and easy and convenient to operate for separating capsaicin and dihydrocapsaicin, the solvent and resin can be recycled, no emission of industrial wastewater, waste gases and residues is generated, and the method is suitable for large-scale industrialized production.
Description
Technical field
The present invention relates to separation and Extraction field, specifically a kind of method improving capsaicine monomer ratio in oleoresin capsicum.
Background technology
Capsaicine material in oleoresin capsicum is mainly capsaicine, Dihydrocapsaicin and nordihydrocapsaicin, and the ratio of capsaicine monomer shared by natural capsicum element is generally 55-62%, ratio shared in Dihydrocapsaicin monomer natural capsicum element is generally 25-30%.In order to improve the ratio of capsaicine monomer in oleoresin capsicum, synthesis capsicine adds in the middle of oleoresin capsicum by illegal businessman, improves the ratio of capsaicine monomer in oleoresin capsicum, thus disrupts the market, improve the competitive power of oneself with this.In conjunction with relevant report, improve capsaicine monomer ratio in oleoresin capsicum and mainly adopt high performance liquid chromatography, reversed-phase silica gel column chromatography method, solvent method and macroporous adsorbent resin column chromatography method.Although high performance liquid chromatography and reversed-phase silica gel column chromatography method can obtain the high oleoresin capsicum of capsaicine monomer ratio, their treatment capacity is little, long processing period, and production unit is expensive, is unfavorable for suitability for industrialized production.And solvent treatment method needs a large amount of toxic or inflammable and explosive solvent that uses, as sherwood oil, halogenated alkane and low carbon chain ester equal solvent, in scale operation, severe contamination is caused to environment, be unfavorable for industrial scale operation.Patent CN101619028 reports that macroreticular resin absorbing method prepares capsaicine monomer, but the capsaicin content of the enriched material of the method upper prop absorption is lower, be only the extraction using alcohol enriched material of the capsicum oil of capsaicin content 0.969% and the red chilly powder of capsaicin content 1.123%, there is no realistic meaning.And, prepare the ethanolic soln wash-out of nordihydrocapsaicin monomer mass concentration 20-40%, monomer content is 90-92%, prepare the ethanolic soln wash-out of capsaicine monomer mass concentration 40-70%, monomer content is 94-96%, prepare the ethanolic soln wash-out of Dihydrocapsaicin monomer mass concentration 70-95%, monomer content is 91-93%.Just not saying the feasibility of this patent, be all different with regard to experiment purpose.
Methods all above is all only limited to the preparation of the capsaicine monomer of sample level, is not applied to the ratio improving capsaicine monomer in oleoresin capsicum, particularly above method is applied to industrialization to improve the ratio of capsaicine monomer in oleoresin capsicum.In sum, for prior art Problems existing, propose easy and simple to handle, that cost is low, with short production cycle, capsaicine monomer ratio is high oleo-resinous novel preparation method, be raising capsicum plant resource utilization, expand the range of application of oleoresin capsicum, realize oleoresin capsicum large-scale industrialized production problem demanding prompt solution.
Summary of the invention
The object of the present invention is to provide that a kind of good separating effect, technique are simple, easy and simple to handle, the method for capsaicine monomer ratio in the raising oleoresin capsicum of three-waste free discharge, to solve the problem proposed in above-mentioned background technology.
For achieving the above object, the invention provides following technical scheme:
Improve a method for capsaicine monomer ratio in oleoresin capsicum, be made up of following steps:
A, by through organic solvent extraction and the alcoholic solution that the oleoresin capsicum mass concentration of concentrating under reduced pressure is 70% dissolve, inject and the chromatography column of macroporous adsorbent resin be housed, standing adsorption 2-4h; Wherein mass concentration is that the alcoholic solution of 70% is with organic solvent extraction and the volume mass of the oleoresin capsicum of concentrating under reduced pressure is 1-2 than V/W, unit is ml/g, and the dry weight of big pore adsorption resin is organic solvent extraction and the 3-6 of the oleoresin capsicum weight of concentrating under reduced pressure times;
B, by the macroporous adsorbent resin mass concentration in the column chromatography of step a be 70% alcoholic solution wash-out, by elute soln concentrating under reduced pressure recycling design, obtain the oleoresin capsicum that total capsaicine mass content is 90-91%, capsaicine monomer mass content is 80-85%, free from extraneous odour;
C, the alcoholic solution being 80% by the macroporous adsorbent resin mass concentration in the column chromatography of step b are eluted to elutant without after capsaicine, by elute soln concentrating under reduced pressure recycling design, obtain the oleoresin capsicum that total capsaicine mass content is 93-94%, Dihydrocapsaicin monomer mass content is 45-50%, free from extraneous odour;
D, the macroporous adsorbent resin ethyl acetate in the column chromatography of step c or acetone to be carried out being eluted to colourless, macroporous adsorbent resin can adsorb use again.
As the further scheme of the present invention: described macroporous adsorbent resin is AB-8 macroporous adsorbent resin, or the macroporous adsorbent resin that other polar phase is worked as.
As the further scheme of the present invention: in step a, the dry weight of big pore adsorption resin is 4-5 times of concentrated pepper oleo-resinous weight after organic solvent process.
As the further scheme of the present invention: in described step b, mass concentration used is that the volume of the alcoholic solution of 70% is organic solvent extraction and the 50-70 times amount of the quality of the oleoresin capsicum of concentrating under reduced pressure, unit is ml/g, in described step c, mass concentration used is that the volume of the alcoholic solution of 80% is organic solvent extraction and the quality 20-25 times amount of the oleoresin capsicum of concentrating under reduced pressure, unit is ml/g, ethyl acetate used in described steps d or the volume of acetone are organic solvent extraction and the quality 10-15 times amount of the oleoresin capsicum of concentrating under reduced pressure, unit is ml/g, the flow of elutriant is 0.5-1 times of column volume/h.
As the further scheme of the present invention: the alcoholic solution in described above step is the alcoholic solution of methyl alcohol, ethanol, Virahol or propylene glycol.
In described steps d, macroporous adsorbent resin adopts the solvent elution that ethyl acetate, acetone or polar phase are worked as, and can not be the solvent that sherwood oil, normal hexane or polar phase are worked as.
In above-mentioned raising oleoresin capsicum, the method for capsaicine monomer ratio obtains oleoresin capsicum.
Compared with prior art, the invention has the beneficial effects as follows:
1) macroporous adsorbent resin of the present invention has good separating effect for each composition in natural capsicum element, and the separating effect for capsaicin and Dihydrocapsaicin is particularly evident.
2) the present invention can prepare total capsaicine mass content is 90.2%, and capsaicine monomer mass content can reach the oleoresin capsicum of 80-85% and total capsaicine mass content is 93.2%, and Dihydrocapsaicin monomer mass content can reach the oleoresin capsicum of 45-50%.
3) macroporous adsorbent resin physical and chemical stability is high, and physical strength is good, and regeneration is easily, with low cost.Technique is simple, and easy and simple to handle, a step just can reach separation object, and solvent and resin can be recycled, and do not have the discharge of the three wastes, are applicable to large-scale industrial production.
4) the present invention use macroporous resin chromatography column, with ethyl acetate or acetone be eluted to colourless rear mass concentration be 70% alcoholic solution by ethyl acetate replacement after, again can adsorb use, long service life.
Embodiment
Below in conjunction with the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, learn from else's experience the oleoresin capsicum 20g of organic solvent extraction concentrating under reduced pressure, high performance liquid chromatograph mensuration is carried out by standard GB/T 28314-2012, the content of total capsaicine is 66.5%, the content of capsaicin monomer is 61.1%, dissolved with the methanol solution that 20mL mass concentration is 70%, inject the chromatography column that the AB-8 resin of dry weight 120g is housed, standing adsorption 2h, wash-out is carried out with methyl alcohol (1.4L) solution that mass concentration is 70%, flow is 0.5L/h, then wash-out is carried out with methyl alcohol (500mL) solution that mass concentration is 80%, flow is 250mL/h.High performance liquid phase tracing detection, split reduction concentration and recovery mass concentration is the meoh eluate of 70%, carries out high performance liquid chromatograph mensuration by standard GB/T 28314-2012, obtains oleoresin capsicum 0.68g successively, total capsaicin content is 19.4%, and the content of capsaicin monomer is 84.3%; Oleoresin capsicum 6.46g, total capsaicin content is 90.2%, and the content of capsaicin monomer is 80.2%; The total capsaicin content of oleoresin capsicum 2.55g is 96.7%, and the content of capsaicin monomer is 66.0%.Concentrating under reduced pressure reclaims the meoh eluate of mass concentration 80%, and carry out high performance liquid chromatograph mensuration by standard GB/T 28314-2012, obtain oleoresin capsicum 4.90g, total capsaicin content is 93.2%, and Dihydrocapsaicin monomer ratio is 45.6%.Total capsaicine rate of recovery: 97.7%.
Embodiment 2
In the embodiment of the present invention, learn from else's experience the oleoresin capsicum 40g of organic solvent extraction concentrating under reduced pressure, high performance liquid chromatograph mensuration is carried out by standard GB/T 28314-2012, the content of total capsaicine is 66.5%, the content of capsaicin monomer is 61.1%, dissolved with the methanol solution that 80mL mass concentration is 70%, inject the chromatography column that the HPD-722 resin of dry weight 200g is housed, standing adsorption 3h, wash-out is carried out with methyl alcohol (2.4L) solution of mass concentration 70%, flow is 0.6L/h, then methyl alcohol (1L) solution of mass concentration 80% is used to carry out wash-out, flow is 250mL/h.High performance liquid phase tracing detection, the meoh eluate of split reduction concentration and recovery mass concentration 70%, carries out high performance liquid chromatograph mensuration by standard GB/T 28314-2012, obtains oleoresin capsicum 1.35g successively, total capsaicin content is 19.5%, and the content of capsaicin monomer is 86.5%; Oleoresin capsicum 12.93g, total capsaicin content is 90.2%, and the content of capsaicin monomer is 82.5%; Oleoresin capsicum 5.12g, total capsaicin content is 96.68%, and the content of capsaicin monomer is 65.8%.Concentrating under reduced pressure reclaims the meoh eluate of mass concentration 80%, and carry out high performance liquid chromatograph mensuration by standard GB/T 28314-2012, obtain oleoresin capsicum 9.82g, total capsaicin content is 93.15%, and Dihydrocapsaicin monomer ratio is 46.7%.Total capsaicine rate of recovery: 97.8%.
Embodiment 3
In the embodiment of the present invention, learn from else's experience the oleoresin capsicum 100g of organic solvent extraction concentrating under reduced pressure, high performance liquid chromatograph mensuration is carried out by standard GB/T 28314-2012, the content of total capsaicine is 66.5%, the content of capsaicin monomer is 61.1%, dissolved with the ethanolic soln that 100m mass concentration is 70%, inject the chromatography column that the AB-8 resin of dry weight 400g is housed, standing adsorption 3h, wash-out is carried out with ethanol (5L) solution that mass concentration is 70%, flow is 2L/h, then wash-out is carried out with ethanol (2L) solution that mass concentration is 80%, flow is 1L/h.High performance liquid phase tracing detection, split reduction concentrates back the ethanol eluate that mass concentration is 70%, carries out high performance liquid chromatograph mensuration by standard GB/T 28314-2012, obtains oleoresin capsicum 3.39g successively, total capsaicin content is 19.4%, and the content of capsaicin monomer is 86.4%; Oleoresin capsicum 32.5g, total capsaicin content is 90.17%, and the content of capsaicin monomer is 83.7%; Oleoresin capsicum 12.78g, total capsaicin content is 96.7%, and the content of capsaicin monomer is 65.9%.It is the ethanol eluate of 80% that concentrating under reduced pressure reclaims mass concentration, and carry out high performance liquid chromatograph mensuration by standard GB/T 28314-2012, obtain oleoresin capsicum 24.48g, total capsaicin content is 93.14%, and Dihydrocapsaicin monomer ratio is 47.7%.The capsaicine rate of recovery: 98.0%.
Embodiment 4
In the embodiment of the present invention, learn from else's experience the oleoresin capsicum 200g of organic solvent extraction concentrating under reduced pressure, high performance liquid chromatograph mensuration is carried out by standard GB/T 28314-2012, the content of total capsaicine is 66.5%, the content of capsaicin monomer is 61.1%, dissolved with the ethanolic soln that 300mL mass concentration is 70%, inject the chromatography column that the HPD-722 resin of dry weight 1kg is housed, standing adsorption 4h, wash-out is carried out with ethanol (10L) solution that mass concentration is 70%, flow is 2L/h, then ethanol (4L) solution of mass concentration 80% is used to carry out wash-out, flow is 1L/h.High performance liquid phase tracing detection, split reduction concentration and recovery mass concentration is the ethanol eluate of 70%, carries out high performance liquid chromatograph mensuration by standard GB/T 28314-2012, obtains oleoresin capsicum 6.79g successively, total capsaicin content is 19.4%, and the content of capsaicin monomer is 87.3%; Oleoresin capsicum 64.7g, total capsaicin content is 90.2%, and the content of capsaicin monomer is 84.7%; Oleoresin capsicum 25.7g, total capsaicin content is 96.7%, and the content of capsaicin monomer is 66.0%.It is the ethanol eluate of 80% that concentrating under reduced pressure reclaims mass concentration, and carry out high performance liquid chromatograph mensuration by standard GB/T 28314-2012, obtain oleoresin capsicum 49.6g, total capsaicin content is 93.2%, and Dihydrocapsaicin monomer ratio is 49.0%.The capsaicine rate of recovery: 98.3%.
Embodiment 5
In the embodiment of the present invention, learn from else's experience the oleoresin capsicum 7kg of organic solvent extraction concentrating under reduced pressure, high performance liquid chromatograph mensuration is carried out by standard GB/T 28314-2012, the content of total capsaicine is 66.5%, the content of capsaicin monomer is 61.1%, dissolved with the ethanolic soln that 7L mass concentration is 70%, inject the chromatography column that the AB-8 resin of dry weight 30kg is housed, standing adsorption 4h, wash-out is carried out with ethanol (350L) solution that mass concentration is 70%, flow is 50L/h, then wash-out is carried out with ethanol (150L) solution that mass concentration is 80%, flow is 50L/h.High performance liquid phase tracing detection, split reduction concentration and recovery mass concentration is the ethanol eluate of 70%, carries out high performance liquid chromatograph mensuration by standard GB/T 28314-2012, obtains oleoresin capsicum 238.9g successively, total capsaicin content is 19.4%, and the content of capsaicin monomer is 86.3%; Oleoresin capsicum 2261.8g, total capsaicin content is 90.2%, and the content of capsaicin monomer is 85.0%; Oleoresin capsicum 892.5g, total capsaicin content is 96.7%, and the content of capsaicin monomer is 65.9%.It is the ethanol eluate of 80% that concentrating under reduced pressure reclaims mass concentration, and carry out high performance liquid chromatograph mensuration by standard GB/T 28314-2012, obtain oleoresin capsicum 1715.5g, total capsaicin content is 93.2%, and Dihydrocapsaicin monomer ratio is 49.7%.The capsaicine rate of recovery: 97.7%.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should by specification sheets integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (6)
1. improve a method for capsaicine monomer ratio in oleoresin capsicum, it is characterized in that, be made up of following steps:
A, by through organic solvent extraction and the alcoholic solution that the oleoresin capsicum mass concentration of concentrating under reduced pressure is 70% dissolve, inject and the chromatography column of macroporous adsorbent resin be housed, standing adsorption 2-4h; Wherein mass concentration is that the alcoholic solution of 70% is with organic solvent extraction and the volume mass of the oleoresin capsicum of concentrating under reduced pressure is 1-2 than V/W, unit is ml/g, and the dry weight of big pore adsorption resin is organic solvent extraction and the 3-6 of the oleoresin capsicum weight of concentrating under reduced pressure times;
B, by the macroporous adsorbent resin mass concentration in the column chromatography of step a be 70% alcoholic solution wash-out, by elute soln concentrating under reduced pressure recycling design, obtain the oleoresin capsicum that total capsaicine mass content is 90-91%, capsaicine monomer mass content is 80-85%, free from extraneous odour;
C, the alcoholic solution being 80% by the macroporous adsorbent resin mass concentration in the column chromatography of step b are eluted to elutant without after capsaicine, by elute soln concentrating under reduced pressure recycling design, obtain the oleoresin capsicum that total capsaicine mass content is 93-94%, Dihydrocapsaicin monomer mass content is 45-50%, free from extraneous odour;
D, the macroporous adsorbent resin ethyl acetate in the column chromatography of step c or acetone to be carried out being eluted to colourless, macroporous adsorbent resin can adsorb use again.
2. the method for capsaicine monomer ratio in raising oleoresin capsicum according to claim 1, it is characterized in that, described macroporous adsorbent resin is AB-8 macroporous adsorbent resin.
3. the method for capsaicine monomer ratio in raising oleoresin capsicum according to claim 1, is characterized in that, in step a the dry weight of big pore adsorption resin be the 4-5 of concentrated pepper oleo-resinous weight after organic solvent process doubly.
4. the method for capsaicine monomer ratio in raising oleoresin capsicum according to claim 1, it is characterized in that, in described step b, mass concentration used is that the volume of the alcoholic solution of 70% is organic solvent extraction and the 50-70 times amount of the quality of the oleoresin capsicum of concentrating under reduced pressure, unit is ml/g, in described step c, mass concentration used is that the volume of the alcoholic solution of 80% is organic solvent extraction and the quality 20-25 times amount of the oleoresin capsicum of concentrating under reduced pressure, unit is ml/g, ethyl acetate used in described steps d or the volume of acetone are organic solvent extraction and the quality 10-15 times amount of the oleoresin capsicum of concentrating under reduced pressure, unit is ml/g, the flow of elutriant is 0.5-1 times of column volume/h.
5. the method for capsaicine monomer ratio in raising oleoresin capsicum according to claim 1, it is characterized in that, described alcoholic solution is the alcoholic solution of methyl alcohol, ethanol, Virahol or propylene glycol.
6. one kind as arbitrary in claim 1-5 as described in the obtained oleoresin capsicum of the method prepared of method.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106966917A (en) * | 2017-03-08 | 2017-07-21 | 黄冈师范学院 | Extraction separation method, capsorubin, the capsaicine of raw material of hot pepper |
| CN111139135A (en) * | 2020-01-09 | 2020-05-12 | 武汉轻工大学 | Method for removing capsaicin and dihydrocapsaicin in vegetable oil |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101619028A (en) * | 2009-06-17 | 2010-01-06 | 张鹏 | Method for preparing capsicine monomer |
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2015
- 2015-12-15 CN CN201510935212.3A patent/CN105331291B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101619028A (en) * | 2009-06-17 | 2010-01-06 | 张鹏 | Method for preparing capsicine monomer |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106966917A (en) * | 2017-03-08 | 2017-07-21 | 黄冈师范学院 | Extraction separation method, capsorubin, the capsaicine of raw material of hot pepper |
| CN111139135A (en) * | 2020-01-09 | 2020-05-12 | 武汉轻工大学 | Method for removing capsaicin and dihydrocapsaicin in vegetable oil |
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Denomination of invention: Method for raising proportion of capsaicin monomer in capsicum oleoresin Effective date of registration: 20200117 Granted publication date: 20180713 Pledgee: CITIC Futong Finance Leasing Co., Ltd. Kunming Branch Pledgor: Yunnan Honglv Capsaicin Co., Ltd. Registration number: Y2020530000001 |