CN105368323B - A kind of preparation method of the capsicum oleoresin of colourless high Capsaicin content - Google Patents
A kind of preparation method of the capsicum oleoresin of colourless high Capsaicin content Download PDFInfo
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- CN105368323B CN105368323B CN201510935211.9A CN201510935211A CN105368323B CN 105368323 B CN105368323 B CN 105368323B CN 201510935211 A CN201510935211 A CN 201510935211A CN 105368323 B CN105368323 B CN 105368323B
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- capsicum oleoresin
- colourless
- capsaicin content
- mass
- oleoresin
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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 153
- 229960002504 capsaicin Drugs 0.000 title claims abstract description 95
- 239000001722 capsicum frutescens oleoresin Substances 0.000 title claims abstract description 72
- 229940050948 capsicum oleoresin Drugs 0.000 title claims abstract description 72
- 235000017663 capsaicin Nutrition 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000011347 resin Substances 0.000 claims abstract description 24
- 229920005989 resin Polymers 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 239000003960 organic solvent Substances 0.000 claims abstract description 16
- 235000002566 Capsicum Nutrition 0.000 claims abstract description 12
- 238000001179 sorption measurement Methods 0.000 claims abstract description 8
- 239000012141 concentrate Substances 0.000 claims abstract description 5
- 239000003480 eluent Substances 0.000 claims abstract description 5
- 239000006002 Pepper Substances 0.000 claims abstract description 3
- 235000016761 Piper aduncum Nutrition 0.000 claims abstract description 3
- 235000017804 Piper guineense Nutrition 0.000 claims abstract description 3
- 235000008184 Piper nigrum Nutrition 0.000 claims abstract description 3
- 239000007791 liquid phase Substances 0.000 claims abstract description 3
- 244000203593 Piper nigrum Species 0.000 claims abstract 2
- 238000001514 detection method Methods 0.000 claims abstract 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 21
- 239000002250 absorbent Substances 0.000 claims description 13
- 230000002745 absorbent Effects 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 240000008574 Capsicum frutescens Species 0.000 claims description 11
- 230000001476 alcoholic effect Effects 0.000 claims description 11
- 239000000284 extract Substances 0.000 claims description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- 239000008601 oleoresin Substances 0.000 claims description 6
- 238000004440 column chromatography Methods 0.000 claims description 5
- 239000003208 petroleum Substances 0.000 claims description 3
- 239000003463 adsorbent Substances 0.000 claims description 2
- 239000012539 chromatography resin Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 12
- 238000010828 elution Methods 0.000 abstract 1
- 150000004676 glycans Chemical class 0.000 abstract 1
- 229920002521 macromolecule Polymers 0.000 abstract 1
- 229920001277 pectin Polymers 0.000 abstract 1
- 235000010987 pectin Nutrition 0.000 abstract 1
- 239000001814 pectin Substances 0.000 abstract 1
- 239000012071 phase Substances 0.000 abstract 1
- 229920001282 polysaccharide Polymers 0.000 abstract 1
- 239000005017 polysaccharide Substances 0.000 abstract 1
- 102000004169 proteins and genes Human genes 0.000 abstract 1
- 108090000623 proteins and genes Proteins 0.000 abstract 1
- 238000011084 recovery Methods 0.000 description 12
- 239000001390 capsicum minimum Substances 0.000 description 9
- 240000004160 Capsicum annuum Species 0.000 description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- 235000008534 Capsicum annuum var annuum Nutrition 0.000 description 4
- 240000008384 Capsicum annuum var. annuum Species 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- PLVBBQBJTBWTDY-XGNSBGGRSA-N Capsochrome Chemical class O1C2(C)CC(O)CC(C)(C)C2=CC1C(\C)=C/C=C/C=C(\C)/C=C\C=C(/C)\C=C/C=C(/C)\C=C\C(=O)C1(C)CC(O)CC1(C)C PLVBBQBJTBWTDY-XGNSBGGRSA-N 0.000 description 1
- 244000147058 Derris elliptica Species 0.000 description 1
- 241000722363 Piper Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- UREBWPXBXRYXRJ-UHFFFAOYSA-N ethyl acetate;methanol Chemical compound OC.CCOC(C)=O UREBWPXBXRYXRJ-UHFFFAOYSA-N 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000000199 molecular distillation Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000001054 red pigment 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
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Seasonings (AREA)
Abstract
The invention discloses a kind of preparation method of the capsicum oleoresin of colourless high Capsaicin content, its step includes：Using organic solvent extracting capsicum oleoresin,By the pepper polysaccharide in capsicum oleoresin,After the macromolecular substances such as pectin and protein remove,It is concentrated under reduced pressure,Concentrate is through macroporous resin adsorption,With the eluant, eluent stepwise elution of various concentrations,Efficient liquid phase tracing detection,Collect respectively,The eluent of concentration different phase various concentrations obtains the capsicum oleoresin of colourless high Capsaicin content,High performance liquid chromatograph measure is carried out by standard GB/T 28,314 2012,The mass content of the capsaicine of capsicum oleoresin prepared by the present invention is 93 97%,It is measured by standard GB/T 10,783 2008,The color value of capsicum oleoresin is up to 0.005 0.010 (E460nm),The present invention is easy to operate,Cost is cheap,Environment amenable method prepares the capsicum oleoresin of colourless high Capsaicin content.Obtained capsicum oleoresin has the characteristics that capsaicin content height, free from extraneous odour, colourless.
Description
Technical field
The present invention relates to a kind of additive, specifically one kind is widely used in field of medicaments, field of food, military neck
The additive in domain, agriculture field and feed addition field, a kind of preparation method of the capsicum oleoresin of colourless high Capsaicin content.
Background technology
Capsicum oleoresin is also known as chilli extract, is a kind of oily liquids obtained from extraction, concentration from capsicum, has capsicum
Intrinsic strong acid.Capsicum oleoresin can be seasoned, coloured in the food industry, fumet and body-building adjuvant etc.,
Can be as the raw material that other compounds or unitary agent are made.Capsicum oleoresin mainly contains capsochrome class material and capsaicine
Class material.
With the development of society, the continuous expansion of the application field of capsicum oleoresin, requirement of the people to capsicum oleoresin
Also constantly changing.The capsicum oleoresin of colourless high Capsaicin content is not only to prepare the raw material of natural capsicine, and prepares
The indispensable raw material of colourless water-soluble Capsaicin, at home and abroad supply falls short of demand.Patent CN101693854A uses overcritical and molecular distillation
The method being combined prepares colorless capsicum oil, but this method complex process, production cost are higher, be not easy to realize product
Industrialization.Patent CN103351955A carries out oxidative decoloration using hydrogen peroxide to chilli extract crude product, although having obtained colourless peppery
Green pepper essence, but the total capsaicin content of colourless capsicum oleoresin that this method is obtained using substantial amounts of hydrogen peroxide is only 10 %, limitation
Further the applying of colourless capsicum oleoresin.Hydrogen peroxide oxidation ability is strong, a large amount of to use, and is unfavorable for environmental protection.Patent
The production method of the water-based chilli extract of CN102715482A report decolourings, although being entered using macroreticular resin absorbing method to chilli extract crude product
Row decolourizes, but the obtained Capsaicin of capsicum oleoresin of this method decolourizes incomplete, still there is pigment residue, prepared by this method
The color value of capsicum oleoresin is 0.5-0.6, is not reaching to colourless requirement.
By experimental studies have found that, capsicum oleoresin capsaicin content be 66%, color value 0.01, be prepared into water-soluble
Property capsaicine 6.6%, can just reach colourless.
The content of the invention
It is an object of the invention to provide a kind of new method, a kind of preparation of the capsicum oleoresin of colourless high Capsaicin content
Method, it is easy to operate, that cost is cheap, with short production cycle, capsaicine obtains the method that rate is high, environmentally safe is colourless to prepare
The capsicum oleoresin of high Capsaicin content, so as to get capsicum oleoresin there is capsaicin content height, free from extraneous odour, colourless.
A kind of preparation method of the capsicum oleoresin of colourless high Capsaicin content of the present invention, comprises the following steps：
（1）By the capsicum oleoresin for extracting and being concentrated under reduced pressure through organic solvent with volume mass than V/W is 1-2 times 70%
Alcoholic solution dissolves, and wherein volume mass is ml/g than unit, in chromatographic column of the injection equipped with macroporous absorbent resin, standing adsorption 2-
4 h, the dry weight of polymeric adsorbent used are 4-6 times of concentrated pepper oleoresin weight after organic solvent processing；
（2）By step（1）In column chromatography mass concentration be 70% alcoholic solution elute, efficient liquid phase tracking and monitoring, point
Section collects concentrate eluant, and the last period obtains capsaicine mass content 78-79%, and color value is that the 0.03-0.04 high Capsaicin of decolouring contains
The capsicum oleoresin of amount, latter section obtains capsaicine mass content 96-97%, and color value is that 0.005-0.006 colourless high Capsaicin contains
The capsicum oleoresin of amount；
（3）By step（2）In column chromatography with mass concentration be 80% alcoholic solution be eluted to eluate without capsaicine after,
Concentrate eluant is collected, obtains capsaicine mass content 93-94%, color value is the peppery of 0.007-0.01 colourless high Capsaicin content
Green pepper oleoresin；
（4）By step（3）Column chromatography resin be eluted to it is colourless；Macroporous absorbent resin can adsorb use again.
Further scheme as the present invention：The step（1）In organic solvent can be selected methanol, acetone, acetic acid second
Any one in ester, petroleum ether, n-hexane.
Further scheme as the present invention：The step（1）In macroporous absorbent resin be AB-8 macroporous absorbent resins.
Further scheme as the present invention：The step（2）In mass concentration used be 70% alcoholic solution volume
（ml）For the quality of capsicum oleoresin（g）50-70 times measure.
Further scheme as the present invention：The step（3）In mass concentration used be 80% alcoholic solution volume
（ml）For the quality of capsicum oleoresin（g）20-25 times measure.
Further scheme as the present invention：The step（4）The volume of ethyl acetate used（ml）For chilli oil tree
The quality of fat（g）10-15 times measure, the flow of eluent is 0.5-1 times of column volume/h.
Further scheme as the present invention：The step（4）Middle macroporous absorbent resin, must be molten with ethyl acetate, acetone
Agent elutes, it is impossible to is petroleum ether, n-hexane solvent.
The beneficial effects of the present invention are：
Separation of the macroreticular resin of the present invention for natural pigment, alkaloid has preferable separating effect, right
It is particularly evident in the separating effect of capsaicine and capsicum red pigment；
Capsicum oleoresin obtained by the present invention is respectively the capsicum oleoresin of colourless high Capsaicin content and the high Capsaicin that decolourizes
The capsicum oleoresin of content.Wherein, the capsicum oleoresin capsaicine mass content of colourless high Capsaicin content is 93-97%, capsaicine
Yield is 81.1-81.9%, and color value is 0.005-0.01 (E460nm).The capsicum oleoresin capsicum quality for high Capsaicin content of decolourizing
Amount content is 78-79%, and capsaicine yield is 16.6-17.3%, and color value is 0.03-0.04 (E460nm).Total capsaicine rate of recovery
For 98.3-99.0%,
Macroporous absorbent resin physical and chemical stability is high, and mechanical strength is good, and regeneration is easy, and cost is cheap；Technique is simple, behaviour
Make simplicity, a step can reaches separation purpose, and solvent and resin can recycle, without the discharge of the three wastes, without environment
Pollution, suitable for large-scale industrial production.
The macroreticular resin chromatographic column that the present invention uses, be eluted to ethyl acetate or acetone it is colourless, with the % of mass concentration 70
Methanol ethyl acetate is replaced after, can also again sorption cycle use.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
In the embodiment of the present invention, a kind of preparation method of the capsicum oleoresin of colourless high Capsaicin content, specific preparation process
For：
Embodiment 1
The capsicum oleoresin 200g that organic solvent of learning from else's experience is extracted and is concentrated under reduced pressure, is entered by standard GB/T 10783-2008
Row measure, color value is 2.5 (E460nm), and high performance liquid chromatograph measure, capsaicine are carried out by standard GB/T 28314-2012
Content 66.5%, with 200mL, the methanol solution that mass concentration is 70% is dissolved, AB-8 of the injection equipped with dry weight 1200g
In the chromatographic column of resin, standing adsorption 2h, eluted with the methanol solution that 14L mass concentrations are 70%, flow 5L/h, so
Eluted afterwards with the methanol solution that 5L mass concentrations are 80%, flow 2.5L/h.Fractional Collections, which is concentrated under reduced pressure, reclaims 70%
Meoh eluate, the last period obtain decolourizing the capsicum oleoresin 29.5g of high Capsaicin content, enter by standard GB/T 28314-2012
Row high performance liquid chromatograph determines, and capsaicine mass content is 78.0%, is measured by standard GB/T 10783-2008, color
Valency is 0.04 (E460nm).Latter section obtains the capsicum oleoresin 65.0g of colourless high Capsaicin content, by standard GB/T 28314-
2012 carry out high performance liquid chromatograph measure, capsaicin content 97.0%, are measured by standard GB/T 10783-2008,
Color value is 0.005 (E460nm).The meoh eluate that the recovery mass concentration that is concentrated under reduced pressure is 80%, obtains colourless high Capsaicin content
Capsicum oleoresin 48.5g, carry out high performance liquid chromatograph measure by standard GB/T 28314-2012, capsaicin content is
93.1%, it is measured by standard GB/T 10783-2008, color value is 0.001 (E460nm).Always the capsaicine rate of recovery is
98.7%, wherein, the capsaicine yield of the capsicum oleoresin of colourless high Capsaicin content is 81.4%, the capsicum for high Capsaicin content of decolourizing
The capsaicine yield of oleoresin is 17.3%.
Embodiment 2
The capsicum oleoresin 40kg that organic solvent of learning from else's experience is extracted and is concentrated under reduced pressure, carried out by standard GB/T 10783-2008
Measure, color value is 2.5 (E460nm), carries out high performance liquid chromatograph measure by standard GB/T 28314-2012, capsaicine contains
Amount 66.5%, dissolved with the methanol solution that 80L mass concentrations are 70%, HPD-722 tree of the injection equipped with dry weight 200kg
In the chromatographic column of fat, standing adsorption 2h, with 2400L, the methanol solution that mass concentration is 70% is eluted, flow 800L/h,
Then 1000L is used, the methanol solution that mass concentration is 80% is eluted, flow 250L/h.Fractional Collections is concentrated under reduced pressure recovery
70% meoh eluate, the last period obtain decolourizing the capsicum oleoresin 5.82kg of high Capsaicin content, by standard GB/T 28314-
2012 carry out high performance liquid chromatograph measure, and capsaicine mass content is 78.5%, is surveyed by standard GB/T 10783-2008
Fixed, color value is 0.034 (E460nm).Latter section obtains the capsicum oleoresin 13.0kg of colourless high Capsaicin content, by national standard
GB28314-2012 carries out high performance liquid chromatograph measure, and capsaicine mass content is 96.8%, by standard GB/T 10783-
2008 are measured, and color value is 0.006 (E460nm).Be concentrated under reduced pressure recovery 80% meoh eluate, obtain colourless high Capsaicin and contain
The capsicum oleoresin 9.68kg of amount, high performance liquid chromatograph measure, capsaicine quality are carried out by standard GB/T 28314-2012
Content is 92.9%, is measured by standard GB/T 10783-2008, and color value is 0.009 (E460nm).Total capsaicine rate of recovery
For 98.3%, wherein, the capsaicine yield of the capsicum oleoresin of colourless high Capsaicin content is 81.1%, the peppery of high Capsaicin content of decolourizing
The capsaicine yield of green pepper oleoresin is 17.2%.
Embodiment 3
The capsicum oleoresin 1kg that organic solvent of learning from else's experience is extracted and is concentrated under reduced pressure, carried out by standard GB/T 10783-2008
Measure, color value is 2.5 (E460nm), and high performance liquid chromatograph measure, capsicum quality are carried out by standard GB/T 28314-2012
Content 66.5% is measured, is dissolved with the ethanol solution that 1L mass concentrations are 70%, AB-8 resin of the injection equipped with dry weight 4kg
Chromatographic column in, standing adsorption 2h, with 50L mass concentrations be 70% ethanol solution eluted, flow 20L/h, Ran Houyong
20L, the ethanol solution that mass concentration is 80% are eluted, flow 10L/h.Fractional Collections be concentrated under reduced pressure recovery 70% ethanol
Eluent, the last period obtain decolourizing the capsicum oleoresin 140.0g of high Capsaicin content, are carried out by standard GB/T 28314-2012
High performance liquid chromatograph determines, and capsaicine mass content is 79.0%, is measured by standard GB/T 10783-2008, color value
For 0.03 (E460nm).Latter section obtains the capsicum oleoresin 330.0g of colourless high Capsaicin content, by standard GB/T 28314-
2012 carry out high performance liquid chromatograph measure, and capsaicine mass content is 96.5%, is surveyed by standard GB/T 10783-2008
Fixed, color value is 0.005 (E460nm).Be concentrated under reduced pressure recovery 80% ethanol eluate, obtain the chilli oil of colourless high Capsaicin content
Resin 243.0g, high performance liquid chromatograph measure is carried out by standard GB/T 28314-2012, capsaicine mass content is
93.0%, it is measured by standard GB/T 10783-2008, color value is 0.007 (E460nm).Always the capsaicine rate of recovery is
98.5%, wherein, the capsaicine yield of the capsicum oleoresin of colourless high Capsaicin content is 81.9%, the capsicum for high Capsaicin content of decolourizing
The capsaicine yield of oleoresin is 16.6%.
Embodiment 4
The capsicum oleoresin 200kg that organic solvent of learning from else's experience is extracted and is concentrated under reduced pressure, is entered by standard GB/T 10783-2008
Row measure, color value is 2.5 (E460nm), and high performance liquid chromatograph measure, capsaicine are carried out by standard GB/T 28314-2012
Mass content 66.5%, dissolved with the ethanol solution that 300L mass concentrations are 70%, injection is equipped with dry weight 1000kg's
In the chromatographic column of HPD-722 resins, standing adsorption 2h, eluted with the ethanol solution that 10000L mass concentrations are 70%, flow
For 3000L/h, then eluted with the ethanol solution that 4000L mass concentrations are 80%, flow 1000L/h.Fractional Collections subtracts
Press the ethanol eluate of concentration and recovery 70%, the last period obtains decolourizing the capsicum oleoresin 29.2kg of high Capsaicin content, is marked by country
Quasi- GB28314-2012 carries out high performance liquid chromatograph measure, and capsaicine mass content is 78.0%, by standard GB/T 10783-
2008 are measured, and color value is 0.036 (E460nm).The capsicum oleoresin 65.7kg of latter section of colourless high Capsaicin content, by state
Family standard GB28314-2012 carries out high performance liquid chromatograph measure, and capsaicine mass content is 97.0%, by national standard
GB10783-2008 is measured, and color value is 0.005 (E460nm).Be concentrated under reduced pressure recovery 80% ethanol eluate, obtain colourless
The capsicum oleoresin 48.5kg of high Capsaicin content, high performance liquid chromatograph measure is carried out by standard GB/T 28314-2012, it is peppery
Green pepper element mass content is 93.1%, is measured by standard GB/T 10783-2008, color value is 0.01 (E460nm).Total capsicum
The plain rate of recovery is 99.0%, wherein, the capsaicine yield of the capsicum oleoresin of colourless high Capsaicin content is 81.9%, and decolourize high Capsaicin
The capsaicine yield of the capsicum oleoresin of content is 17.1%.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It is appreciated that other embodiment.
Claims (7)
1. a kind of preparation method of the capsicum oleoresin of colourless high Capsaicin content, it is characterised in that comprise the steps of：
（1）The capsicum oleoresin for extracting and being concentrated under reduced pressure through organic solvent is more molten than 70% alcohol that V/W is 1-2 times with volume mass
Liquid dissolves, and wherein volume mass is ml/g than unit, in chromatographic column of the injection equipped with macroporous absorbent resin, standing adsorption 2-4 h,
The dry weight of polymeric adsorbent used is 4-6 times of concentrated pepper oleoresin weight after organic solvent processing；
（2）By step（1）In column chromatography in macroporous absorbent resin mass concentration be 70% alcoholic solution elute, efficient liquid
Phase tracing detection, Fractional Collections concentrate eluant, the last period obtain capsaicine mass content 78-79%, color value 0.03-0.04
The high Capsaicin content of decolouring capsicum oleoresin, it is 96-97%, color value 0.005- that latter section, which obtains capsaicine mass content,
The capsicum oleoresin of 0.006 colourless high Capsaicin content；
（3）By step（2）In macroporous absorbent resin with mass concentration be 80% alcoholic solution liquid be eluted to eluate without capsaicine
Afterwards, concentrate eluant is collected, it is 93-94% to obtain capsaicine mass content, and color value is 0.007-0.01 colourless high Capsaicin content
Capsicum oleoresin；
（4）By step（3）Macroporous absorbent resin be eluted to it is colourless；Macroporous absorbent resin can adsorb use again.
A kind of 2. preparation method of the capsicum oleoresin of colourless high Capsaicin content according to claim 1, it is characterised in that
The step（1）In organic solvent from methanol, acetone, ethyl acetate, petroleum ether, any one in n-hexane.
A kind of 3. preparation method of the capsicum oleoresin of colourless high Capsaicin content according to claim 1, it is characterised in that
The step（1）In macroporous absorbent resin be AB-8 macroporous absorbent resins.
A kind of 4. preparation method of the capsicum oleoresin of colourless high Capsaicin content according to claim 1, it is characterised in that
The step（2）In mass concentration used be that the volume of 70% alcoholic solution is the chilli oil for extracting and being concentrated under reduced pressure through organic solvent
50-70 times of the quality of resin is measured, and mass concentration is that the volume unit of 70% alcoholic solution is ml, extracts and depressurizes through organic solvent
The mass unit of the capsicum oleoresin of concentration is g.
A kind of 5. preparation method of the capsicum oleoresin of colourless high Capsaicin content according to claim 1, it is characterised in that
The step（3）In the volume of alcoholic solution of mass concentration 80% used be the chilli oil that extracts and be concentrated under reduced pressure through organic solvent
20-25 times of the quality of resin is measured, and mass concentration is that the volume unit of 80% alcoholic solution is ml, extracts and depressurizes through organic solvent
The mass unit of the capsicum oleoresin of concentration is g.
A kind of 6. preparation method of the capsicum oleoresin of colourless high Capsaicin content according to claim 1, it is characterised in that
The step（4）Column chromatography resin with ethyl acetate or acetone be eluted to it is colourless.
A kind of 7. preparation method of the capsicum oleoresin of colourless high Capsaicin content according to claim 6, it is characterised in that
The step（4）The volume of ethyl acetate used is the quality for the capsicum oleoresin for extracting and being concentrated under reduced pressure through organic solvent
10-15 times is measured, and the flow of eluent is 0.5-1 times of column volume/h；The volume unit of ethyl acetate is ml, the matter of capsicum oleoresin
Measure g.
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Denomination of invention: Method for preparing colorless capsicum oleoresin with high capsaicin content Effective date of registration: 20200212 Granted publication date: 20180130 Pledgee: CITIC Futong Finance Leasing Co., Ltd. Kunming Branch Pledgor: Wenshan Yongrun Capsaicin Co., Ltd. Registration number: Y2020530000003 |