CN108034279B - A method of separating chilli extract and capsanthin in red Capsaicin - Google Patents
A method of separating chilli extract and capsanthin in red Capsaicin Download PDFInfo
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- CN108034279B CN108034279B CN201711402705.6A CN201711402705A CN108034279B CN 108034279 B CN108034279 B CN 108034279B CN 201711402705 A CN201711402705 A CN 201711402705A CN 108034279 B CN108034279 B CN 108034279B
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- capsanthin
- chilli extract
- separating
- red capsaicin
- red
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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 126
- 235000017663 capsaicin Nutrition 0.000 title claims abstract description 64
- 229960002504 capsaicin Drugs 0.000 title claims abstract description 63
- VYIRVAXUEZSDNC-TXDLOWMYSA-N (3R,3'S,5'R)-3,3'-dihydroxy-beta-kappa-caroten-6'-one Chemical compound C([C@H](O)CC=1C)C(C)(C)C=1/C=C/C(/C)=C/C=C/C(/C)=C/C=C/C=C(C)C=CC=C(C)C=CC(=O)[C@]1(C)C[C@@H](O)CC1(C)C VYIRVAXUEZSDNC-TXDLOWMYSA-N 0.000 title claims abstract description 58
- VYIRVAXUEZSDNC-LOFNIBRQSA-N Capsanthyn Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CC(O)CC1(C)C)C=CC=C(/C)C=CC(=O)C2(C)CC(O)CC2(C)C VYIRVAXUEZSDNC-LOFNIBRQSA-N 0.000 title claims abstract description 58
- WRANYHFEXGNSND-LOFNIBRQSA-N capsanthin Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CC(O)CC1(C)C)C=CC=C(/C)C=CC(=O)C2(C)CCC(O)C2(C)C WRANYHFEXGNSND-LOFNIBRQSA-N 0.000 title claims abstract description 58
- 235000018889 capsanthin Nutrition 0.000 title claims abstract description 58
- 239000001688 paprika extract Substances 0.000 title claims abstract description 58
- 235000012658 paprika extract Nutrition 0.000 title claims abstract description 58
- 239000000284 extract Substances 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 40
- 240000004160 Capsicum annuum Species 0.000 title abstract description 49
- 239000002904 solvent Substances 0.000 claims abstract description 53
- 239000002244 precipitate Substances 0.000 claims abstract description 34
- 239000006228 supernatant Substances 0.000 claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 25
- 238000005119 centrifugation Methods 0.000 claims abstract description 20
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 105
- 239000000243 solution Substances 0.000 claims description 29
- 240000008574 Capsicum frutescens Species 0.000 claims description 20
- 239000010409 thin film Substances 0.000 claims description 15
- 235000002566 Capsicum Nutrition 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 239000001390 capsicum minimum Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 239000010408 film Substances 0.000 claims description 9
- 238000001556 precipitation Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 230000009194 climbing Effects 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 4
- 241000208293 Capsicum Species 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 28
- 239000000047 product Substances 0.000 abstract description 24
- 238000000926 separation method Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 7
- 238000000605 extraction Methods 0.000 abstract description 7
- 239000000419 plant extract Substances 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 9
- 238000001704 evaporation Methods 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- 239000001054 red pigment Substances 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 235000008534 Capsicum annuum var annuum Nutrition 0.000 description 2
- 239000006002 Pepper Substances 0.000 description 2
- 241000722363 Piper Species 0.000 description 2
- 235000016761 Piper aduncum Nutrition 0.000 description 2
- 235000017804 Piper guineense Nutrition 0.000 description 2
- 235000008184 Piper nigrum Nutrition 0.000 description 2
- 239000001722 capsicum frutescens oleoresin Substances 0.000 description 2
- 229940050948 capsicum oleoresin Drugs 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 235000013373 food additive Nutrition 0.000 description 2
- 239000002778 food additive Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 240000008384 Capsicum annuum var. annuum Species 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000000476 body water Anatomy 0.000 description 1
- 239000001511 capsicum annuum Substances 0.000 description 1
- 235000021466 carotenoid Nutrition 0.000 description 1
- 150000001747 carotenoids Chemical class 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 235000019462 natural additive Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000009657 tetraterpenes Nutrition 0.000 description 1
- 150000003535 tetraterpenes Chemical class 0.000 description 1
- 229960002415 trichloroethylene Drugs 0.000 description 1
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 239000002699 waste material Substances 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
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/10—Natural spices, flavouring agents or condiments; Extracts thereof
- A23L27/11—Natural spices, flavouring agents or condiments; Extracts thereof obtained by solvent extraction
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/40—Colouring or decolouring of foods
- A23L5/42—Addition of dyes or pigments, e.g. in combination with optical brighteners
- A23L5/43—Addition of dyes or pigments, e.g. in combination with optical brighteners using naturally occurring organic dyes or pigments, their artificial duplicates or their derivatives
- A23L5/44—Addition of dyes or pigments, e.g. in combination with optical brighteners using naturally occurring organic dyes or pigments, their artificial duplicates or their derivatives using carotenoids or xanthophylls
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
Abstract
The invention discloses a kind of methods for separating chilli extract and capsanthin in red Capsaicin, belong to the separation and Extraction of natural plant extracts, comprise the following processes: I, is centrifuged after mixing red Capsaicin raw material with middle gradient solvent, separates light phase and heavy phase；Centrifugation obtains supernatant A and precipitate A after II, mixes light phase with low gradient solvent, and chilli extract is extracted from supernatant A；III, is centrifuged after mixing heavy phase with high gradient solvent, obtains supernatant B and precipitate B, capsanthin is extracted from precipitate B；The present invention can significantly improve chilli extract and capsanthin separating effect, improve product purity, yield and yield, reduce pollution and production cost, it is easy to operate, be suitble to industrialized production.
Description
Technical field
The present invention relates to red Capsaicins, and the concentration gradient separate work of chilli extract and capsanthin is extracted especially from red Capsaicin
Skill belongs to the separation and Extraction of natural plant extracts.
Background technique
Capsanthin is also known as capsicum red pigment, is a kind of orange red pigment of the tetraterpenes being present in mature paprika fruit,
Belong to carotenoids pigment, the red no acid of pure pepper.Capsicum red pigment by U.S. FAO, Britain, Japan, EEC, WHO and
The tissues such as the Chinese world are approval for the natural additive for foodstuff that unlimitedness uses, and international market is very well sold and in short supply.
Chilli extract is also known as capsicum oleoresin, is a kind of product obtained by extracting, being concentrated in capsicum, and pure pepper essence is colourless
Crystal has strong acid, is often used to production food seasoning, also can be used as medical ingredient, cosmetic material, biochemical agriculture
Medicine, chemical and biological weapons, biochemical special paint etc..
Red Capsaicin is with methylene chloride, trichloro ethylene, acetone equal solvent from chilli powder or the fruit of other capsicum plants
A kind of oiliness containing capsanthin, chilli extract, colloid obtained by dissolvent residual is removed after middle extraction to dissolve each other object.Red Capsaicin is de- through aquation
Red Capsaicin after obtaining degumming after glue or acetone treatment.It is usually adopted when separating capsanthin, chilli extract from the red Capsaicin after degumming
Conventional processing methods are that the red Capsaicin after degumming is direct with the solvent for being only capable of that chilli extract is made to dissolve and not dissolve capsanthin
The mode of hybrid extraction separates chilli extract, then obtains capsanthin through reduced pressure.
Solvent used in this entire production process of method is the same solvent of fixed concentration, but when industrialized production, vehicle
Between the solvent strength that evaporates of evaporators at different levels to have height to have low, most enterprises, which are generallyd use, carries out essence for low concentration solvent
It evaporates, obtains producing required consolidate in the mode for adding a certain proportion of pure solvent after intermediate concentration and high concentration solvent are mixed
Determine the solvent of concentration.Therefore, this production technology often results in separation and is not thorough, in obtained capsanthin due to containing chilli extract and
With acid, due to being unable to satisfy the requirement of high-quality product, depositing containing capsanthin and with red in obtained chilli extract
In the problem that impurity content is high, yield is lower, the market competitiveness is weaker, there is an urgent need to a kind of high yield, high yield pulp1, low pollutions
High-quality chilli extract and capsanthin production technology.
Summary of the invention
The technical problem to be solved by the invention is to provide a kind of method for separating chilli extract and capsanthin in red Capsaicin, energy
It enough significantly improves the separating effect of chilli extract and capsanthin, improve purity, yield and the yield of product, reduce pollution and be produced into
Originally, easy to operate, suitable industrialized production.
In order to solve the above technical problems, the technical scheme adopted by the invention is that:
A method of chilli extract and capsanthin in red Capsaicin are separated, is comprised the following processes:
I, is centrifuged after mixing red Capsaicin raw material with middle gradient solvent, separates light phase and heavy phase；
Centrifugation obtains supernatant A and precipitate A after II, mixes light phase with low gradient solvent, and capsicum is extracted from supernatant A
Essence；
III, is centrifuged after mixing heavy phase with high gradient solvent, obtains supernatant B and precipitate B, capsicum is extracted from precipitate B
It is red.
Technical solution of the present invention further improvement lies in that: the red Capsaicin raw material be degumming after red Capsaicin and precipitate A
With any one of supernatant B or two kinds of mixture.
Technical solution of the present invention further improvement lies in that: the middle gradient solvent be mass fraction 65~75% methanol
Solution, volume ratio when red Capsaicin raw material is mixed with middle gradient solvent are 1:1~5.
Technical solution of the present invention further improvement lies in that: methanol in the solution that light phase obtains after mixing with low gradient solvent
Mass fraction be 45~55%.
Technical solution of the present invention further improvement lies in that: the low gradient solvent be water, body when light phase is mixed with water
Product is than being 1.5~4.5:1.
Technical solution of the present invention further improvement lies in that: the high gradient solvent be mass fraction 85~95% methanol
Aqueous solution, volume ratio when heavy phase is mixed with high gradient solvent are 1:2~4.
Technical solution of the present invention further improvement lies in that: when centrifugation use explosion-proof type disk centrifugal separator, revolving speed 4000
~6000 revs/min.
Technical solution of the present invention further improvement lies in that: be combined by the realization of multiple-effect mixer, temperature when mixing
It is 35~55 DEG C, revolving speed is 940~980 revs/min.
Technical solution of the present invention further improvement lies in that: from supernatant A extract chilli extract when use climbing film evaporator
It connects with two thin film evaporators, obtains chilli extract after being evaporated in vacuo precipitation.
Technical solution of the present invention further improvement lies in that: steamed when extracting capsanthin from precipitate B using 2~4 films
Device series connection is sent out, obtains capsanthin after being evaporated in vacuo precipitation at vacuum degree >=-0.090Mpa.
By adopting the above-described technical solution, the technological progress achieved by the present invention is:
A kind of method separating chilli extract and capsanthin in red Capsaicin provided by the invention, can significantly improve chilli extract and
The separating effect of capsanthin, purity, yield and the yield for improving product, reduce pollution and production cost, it is easy to operate, be suitble to work
Industry metaplasia produces.
In technical process of the invention it is preferable to use solvent be methanol aqueous solution, compared to ethyl alcohol, acetone etc. other often
The effect of extracting of extractant, methanol aqueous solution is more preferable, can utmostly improve yield and product yield, realizes capsicum
Essence is kept completely separate with capsanthin, significantly improves product purity.Chilli extract in red Capsaicin raw material is soluble in methanol, and capsicum
It is red to be insoluble in methanol, it will appear layering after the red Capsaicin after degumming is mixed with methanol aqueous solution, upper layer light phase is mainly methanol
With chilli extract mixture, lower layer's heavy phase is mainly capsanthin.
The present invention carries out repeatedly mixing Centrifugical extraction, the solvent of various concentration using the solvent of various concentration and successively forms one
A gradient, gradient solvent in selection when first pass mixing Centrifugical extraction, middle gradient solvent concentration is preferably 65~75%, is mixed again
Close Centrifugical extraction chilli extract where light phase and capsanthin where heavy phase when, the concentration of solvent is reduced and is improved respectively, formation
The separation of Solvent Gradient concentration.The solvent of various concentration has different separating effects for separation capsanthin and chilli extract, and use is dense
Spending higher high gradient solvent, to can guarantee that capsicum red pigment sufficiently takes off peppery, and high gradient solvent strength is preferably 85~95%, is isolated
Capsanthin in be free of chilli extract；It can guarantee using the lower solvent of concentration without containing capsanthin in the chilli extract isolated, gently
Methanol concentration is preferably 45~55% after mutually mixing with low gradient solvent, is solved the problems, such as colored (capsanthin) of chilli extract, effectively
Separating effect is optimized, product quality and yield are improved.
The present invention uses explosion-proof type disk centrifugal separator (maximum processing capability is 10 sides/hour), revolving speed 4000 when being centrifuged
~6000 revs/min are able to achieve acceleration layering, improve production efficiency, keep separation more thorough.It is extracted and is centrifuged with low gradient solvent
The precipitate A separated afterwards and the supernatant B separated after high gradient solvent extraction centrifugation, which can be collected, is added to separation next time institute
In red Capsaicin after degumming, the waste of resource can be effectively avoided, the yield of product is further increased, reduces the dirt of environment
Dye.
And the solvent of various concentration that the present invention uses can be directly obtained by workshop evaporation equipments at different levels, be steamed wherein rising film
Hair device is used for recycling high gradient solvent, First thin film evaporator for gradient solvent in recycling, second thin film evaporator
In recycling low gradient solvent, without mixing, being adjusted to a kind of solvent of fixed concentration, by increasing pipeline, making liquid pump and control
Flow can be such that entire production process is carried out continuously, and realize the recycling of solvent, reduce environmental pollution, saving mass energy,
When consumption and re-treating process operation investment.
The product of production high yield pulp1, high yield, low impurity can be achieved in the present invention, and feasibility is strong in technique, production cost compared with
Low, step is simple, and environmental pollution is small, is suitble to industrialized production.
Specific embodiment
The present invention is described in further details below with reference to embodiment:
A method of separating chilli extract and capsanthin in red Capsaicin, it is characterised in that comprise the following processes:
I, removes dissolvent residual after extracting in chilli powder by organic solvent, then after aquation degumming or acetone treatment
Red Capsaicin after to degumming obtains in production cycle before can remixing addition certain proportion in the red Capsaicin after degumming
Precipitate A and supernatant B become red Capsaicin raw material.By volume by the methanol solution of red Capsaicin raw material and mass fraction 65~75%
It being mixed for 1:1~5, is combined by the realization of multiple-effect mixer, temperature is 35~55 DEG C when mixing, revolving speed is 940~
980 revs/min, then using explosion-proof type disk centrifugal separator be centrifuged, revolving speed be 4000~6000 revs/min, separation light phase with again
Phase；
II, mixes light phase with low gradient solvent by multiple-effect mixer, and temperature is 35~55 DEG C when mixing, revolving speed
It is 940~980 revs/min, low gradient solvent can be water or the lower methanol solution of concentration, when low gradient solvent is water,
Volume ratio when light phase is mixed with water is 1.5~4.5:1, and the mass fraction of methanol is 45~55% in the solution obtained after mixing,
It is then centrifuged for obtaining supernatant A and precipitate A, be then centrifuged using explosion-proof type disk centrifugal separator, revolving speed is 4000~6000 revs/min
Clock.Supernatant A goes successively to the process flow for producing chilli extract finished product, using climbing film evaporator and two thin film evaporators
Series connection obtains chilli extract after being evaporated in vacuo recycling methanol solution.Precipitate A can mix after separating with the red Capsaicin after degumming
As the red Capsaicin raw material of subsequent production, it is recycled.
The methanol aqueous solution of heavy phase and mass fraction 85~95% is that 1:2~4 pass through multiple-effect mixer by III, by volume
It is mixed, temperature is 35~55 DEG C when mixing, and revolving speed is 940~980 revs/min, and explosion-proof type disk centrifugal is used after mixing
Machine centrifugation, revolving speed are 4000~6000 revs/min, obtain supernatant B and precipitate B, precipitate B is gone successively to for producing capsanthin
The process flow of finished product is connected using 2~4 thin film evaporators, is obtained after precipitation is evaporated in vacuo at vacuum degree >=-0.090Mpa
To capsanthin.Supernatant B can mix the red Capsaicin raw material as subsequent production, quilt with the red Capsaicin after degumming after separating
Recycling and reusing.
Embodiment 1
4000kg color value is 205.3 by I, and the methanol solution of the red Capsaicin raw material and mass fraction 65% of peppery degree 0.22% is pressed
Volume ratio is 1:1 mixing, and temperature is 35 DEG C when mixing, and revolving speed is 960 revs/min, is then centrifuged for, and the revolving speed of centrifugation is 4000
Rev/min, separate light phase and heavy phase；
Light phase is that 1.5:1 is mixed with water by II, by volume, and temperature is 55 DEG C, and revolving speed is 960 revs/min, is then centrifuged for
Supernatant A and precipitate A are obtained, the revolving speed of centrifugation is 4000 revs/min.Supernatant A is gone successively to for producing chilli extract finished product
Process flow capsicum is obtained after being evaporated in vacuo recycling methanol solution using climbing film evaporator and the series connection of two thin film evaporators
Essence.Precipitate A can mix the red Capsaicin raw material as subsequent production with the red Capsaicin after degumming after separating, be recovered again sharp
With.
Heavy phase is that 1:2 is mixed with the methanol aqueous solution of mass fraction 85% by III, by volume, and temperature is 45 DEG C, and revolving speed is
960 revs/min, be centrifuged after mixing, the revolving speed of centrifugation is 4000 revs/min, obtain supernatant B and precipitate B, precipitate B continue into
Enter the process flow for producing capsanthin finished product, is connected using 2 thin film evaporators, it is true at vacuum degree >=-0.090Mpa
Capsanthin is obtained after sky evaporation precipitation.Supernatant B can be mixed after separating with the red Capsaicin after degumming is used as subsequent production
Red Capsaicin raw material, be recycled.
After production, capsanthin 3950kg, color value 205.84, peppery degree 0.00015%, color value yield 99.01% are obtained；
To chilli extract 50kg, color value 8.21, peppery degree 17.58；Whole process, color value yield 99.06%, peppery degree yield 99.95%.
Embodiment 2
12500kg color value is 189.6 by I, the methanol solution of red Capsaicin raw material and mass fraction 73% that peppery degree is 0.55%
It is mixed by volume for 1:2, temperature is 35 DEG C, and revolving speed is 940 revs/min, is then centrifuged for, and the revolving speed of centrifugation is 5000 revs/min
Clock separates light phase and heavy phase；
Light phase is that 4.5:1 is mixed with water by II, by volume, temperature be 35 DEG C, revolving speed be 940 revs/min, then from
For gains in depth of comprehension to supernatant A and precipitate A, the revolving speed of centrifugation is 5000 revs/min.Supernatant A go successively to for produce chilli extract at
The process flow of product is obtained peppery using climbing film evaporator and two thin film evaporator series connection after vacuum evaporation recycling methanol solution
Green pepper essence.Precipitate A can mix the red Capsaicin raw material after the degumming as subsequent production with the red Capsaicin after degumming after separating,
It is recycled.
Heavy phase is that 1:3.5 is mixed with the methanol aqueous solution of mass fraction 87% by III, by volume, and temperature is 35 DEG C, revolving speed
It is 940 revs/min, is centrifuged after mixing, the revolving speed of centrifugation is 5000 revs/min, obtains supernatant B and precipitate B, and precipitate B continues
Into the process flow for producing capsanthin finished product, connected using 3 thin film evaporators, at vacuum degree >=-0.090Mpa
Capsanthin is obtained after being evaporated in vacuo precipitation.Supernatant B can be mixed after separating with the red Capsaicin after degumming as subsequent life
The red Capsaicin raw material produced, is recycled.
After production, capsanthin 12356kg, color value 190.37, peppery degree 0.00011%, color value yield 99.25% are obtained；
Obtain chilli extract 144kg, color value 6.58, peppery degree 47.73%；Whole process, color value yield 99.29%, peppery degree yield 99.99%.
Embodiment 3
7500kg color value is 150.7 by I, the methanol solution of red Capsaicin raw material and mass fraction 70% that peppery degree is 0.48%
It is mixed by volume for 1:3, temperature is 55 DEG C, and revolving speed is 980 revs/min, is then centrifuged for, and the revolving speed of centrifugation is 6000 revs/min
Clock separates light phase and heavy phase；
II, which passes through light phase with the methanol solution that concentration is 5%, to be mixed, and temperature is 55 DEG C, and revolving speed is 980 revs/min, is obtained
The solution for being 45% to methanol quality score is then centrifuged for obtaining supernatant A and precipitate A, and the revolving speed of centrifugation is 6000 revs/min.
Supernatant A goes successively to the process flow for producing chilli extract finished product, using climbing film evaporator and two thin film evaporator strings
Connection obtains chilli extract after being evaporated in vacuo recycling methanol solution.Precipitate A can mix work with the red Capsaicin after degumming after separating
For the red Capsaicin raw material of subsequent production, it is recycled.
Heavy phase is that 1:3 is mixed with the methanol aqueous solution of mass fraction 90% by III, by volume, and temperature is 55 DEG C, and revolving speed is
980 revs/min, be centrifuged after mixing, the revolving speed of centrifugation is 6000 revs/min, obtain supernatant B and precipitate B, precipitate B continue into
Enter the process flow for producing capsanthin finished product, is connected using 4 thin film evaporators, it is true at vacuum degree >=-0.090Mpa
Capsanthin is obtained after sky evaporation precipitation.Supernatant B can be mixed after separating with the red Capsaicin after degumming is used as subsequent production
Red Capsaicin raw material, be recycled.
After production, capsanthin 7400kg, color value 151.04, peppery degree 0.00010%, color value yield 98.89% are obtained；
To chilli extract 100kg, color value 4.52, peppery degree 35.98%；Whole process, color value yield 98.93%, peppery degree yield 99.97%.
Embodiment 4
10000kg color value is 195.3 by I, and peppery degree is molten for the methanol of 0.75% red Capsaicin raw material and mass fraction 75%
Liquid is 1:5 mixing by volume, and temperature is 45 DEG C, and revolving speed is 970 revs/min, is then centrifuged for, the revolving speed of centrifugation is 4000 turns/
Minute, separate light phase and heavy phase；
II, mixes light phase with the methanol solution that concentration is 10%, and temperature is 45 DEG C, and revolving speed is 960 revs/min, obtains first
The solution that alcohol mass fraction is 55% is then centrifuged for obtaining supernatant A and precipitate A, and the revolving speed of centrifugation is 5000 revs/min.Supernatant
Liquid A goes successively to the process flow for producing chilli extract finished product, using climbing film evaporator and two thin film evaporator series connection, very
Chilli extract is obtained after sky evaporation recycling methanol solution.Precipitate A can mix conduct with the red Capsaicin after degumming after separating after
The red Capsaicin raw material of continuous production, is recycled.
Heavy phase is that 1:4 is mixed with the methanol aqueous solution of mass fraction 95% by III, by volume, and temperature is 45 DEG C, and revolving speed is
970 revs/min, be centrifuged after mixing, the revolving speed of centrifugation is 6000 revs/min, obtain supernatant B and precipitate B, precipitate B continue into
Enter the process flow for producing capsanthin finished product, is connected using 3 thin film evaporators, it is true at vacuum degree >=-0.090Mpa
Capsanthin is obtained after sky evaporation precipitation.Supernatant B can be mixed after separating with the red Capsaicin after degumming is used as subsequent production
Red Capsaicin raw material, be recycled.
After production, capsanthin 9800kg, color value 197.21, peppery degree 0.00008%, color value yield 98.96% are obtained；
To chilli extract 200kg, color value 3.91, peppery degree 37.49%；Whole process, color value yield 99.00%, peppery degree yield 99.98%.
Control group
Be 201.3 by 5000kg color value, peppery degree be 0.33% red Capsaicin raw material and 85% methanol aqueous solution by volume
1:3 is mixed by multiple-effect mixer, and temperature is 45 DEG C, and revolving speed is 960 revs/min, is centrifuged after mixing, and the revolving speed of centrifugation is 5000
Rev/min, obtain light phase and heavy phase.Will heavy phase with 85% methanol aqueous solution by volume 1:3 mix after be centrifuged, mixing and from
The condition of the heart is identical as above-mentioned steps, and the red finished product of lower sediment refining chilli is used after being repeated 5 times.Light phase is distilled, is distilled out
Solvent recycled, distill remaining sediment be chilli extract crude product, chilli extract finished product will be re-refined to obtain.
After production, capsanthin 4500kg, color value 216.18, peppery degree 0.015%, color value yield 96.65% are obtained；It obtains
Chilli extract 500kg, color value 41.87, peppery degree 3.17%；Whole process, color value yield 98.73%, peppery degree yield 99.85%.
The detection of the indices obtained when being produced from the process conditions according to Examples 1 to 4 and control group are practical
Data can be seen that the present invention can significantly improve the separating effect of chilli extract and capsanthin, improve the purity of product, yield and
Yield, wherein the detection method of color value is referring to " GB10783-2008 food additives capsanthin ", and peppery degree detection method is referring to " GB
28314-2012 food additives capsicum oleoresin ".
Claims (9)
1. a kind of method for separating chilli extract and capsanthin in red Capsaicin, it is characterised in that comprise the following processes: I, is by red Capsaicin
Raw material is centrifuged after mixing with middle gradient solvent, separates light phase and heavy phase；
Centrifugation obtains supernatant A and precipitate A after II, mixes light phase with low gradient solvent, and chilli extract is extracted from supernatant A；
III, is centrifuged after mixing heavy phase with high gradient solvent, obtains supernatant B and precipitate B, capsanthin is extracted from precipitate B；
Wherein, the middle gradient solvent is the methanol solution of mass fraction 65~75%；
Wherein, the mass fraction of methanol is 45~55% in the solution that the light phase obtains after mixing with low gradient solvent；
Wherein, the high gradient solvent is the methanol aqueous solution of mass fraction 85~95%.
2. a kind of method for separating chilli extract and capsanthin in red Capsaicin according to claim 1, it is characterised in that: described
Red Capsaicin raw material is the red Capsaicin and any one of precipitate A and supernatant B or two kinds of mixture after degumming.
3. a kind of method for separating chilli extract and capsanthin in red Capsaicin according to claim 1, it is characterised in that: described
Volume ratio when red Capsaicin raw material is mixed with middle gradient solvent is 1:1~5.
4. a kind of method for separating chilli extract and capsanthin in red Capsaicin according to claim 1, it is characterised in that: described
Low gradient solvent is water, and volume ratio when light phase is mixed with water is 1.5~4.5:1.
5. a kind of method for separating chilli extract and capsanthin in red Capsaicin according to claim 1, it is characterised in that: described
Volume ratio when heavy phase is mixed with high gradient solvent is 1:2~4.
6. a kind of method for separating chilli extract and capsanthin in red Capsaicin according to claim 1, it is characterised in that: centrifugation
Shi Caiyong explosion-proof type disk centrifugal separator, revolving speed are 4000~6000 revs/min.
7. a kind of method for separating chilli extract and capsanthin in red Capsaicin according to claim 1, it is characterised in that: mixing
It is to be realized by multiple-effect mixer, temperature is 35~55 DEG C when mixing, and revolving speed is 940~980 revs/min.
8. a kind of method for separating chilli extract and capsanthin in red Capsaicin according to claim 1, it is characterised in that: from upper
Using climbing film evaporator and two thin film evaporator series connection when extracting chilli extract in clear liquid A, capsicum is obtained after being evaporated in vacuo precipitation
Essence.
9. a kind of method for separating chilli extract and capsanthin in red Capsaicin according to claim 1, it is characterised in that: from heavy
Using 2~4 thin film evaporator series connection when extracting capsanthin in the B of shallow lake, after being evaporated in vacuo precipitation at vacuum degree >=-0.090Mpa
Obtain capsanthin.
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| CN101066120A (en) * | 2007-05-31 | 2007-11-07 | 河北晨光天然色素有限公司 | Efficient continuous spicy material eliminating process in capsanthin production |
| CN101531826A (en) * | 2009-04-17 | 2009-09-16 | 邯郸市东之星生物科技有限公司 | Method for extracting capsicum red pigment |
| CN101709153A (en) * | 2009-12-23 | 2010-05-19 | 崔俊良 | Method for removing piquancy of capsanthin |
| CN102140067A (en) * | 2011-01-31 | 2011-08-03 | 新疆隆平高科弘安天然色素有限公司 | Method for extracting and purifying high-purity capsaicine from capsicum oleoresin |
| CN102757665A (en) * | 2012-07-28 | 2012-10-31 | 吉林省金塔实业（集团）股份有限公司 | Degumming process of capsicum extract |
| CN104194389A (en) * | 2014-08-26 | 2014-12-10 | 晨光生物科技集团股份有限公司 | Method for extracting capsanthin and capsaicine by processing fresh chili |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101066120A (en) * | 2007-05-31 | 2007-11-07 | 河北晨光天然色素有限公司 | Efficient continuous spicy material eliminating process in capsanthin production |
| CN101531826A (en) * | 2009-04-17 | 2009-09-16 | 邯郸市东之星生物科技有限公司 | Method for extracting capsicum red pigment |
| CN101709153A (en) * | 2009-12-23 | 2010-05-19 | 崔俊良 | Method for removing piquancy of capsanthin |
| CN102140067A (en) * | 2011-01-31 | 2011-08-03 | 新疆隆平高科弘安天然色素有限公司 | Method for extracting and purifying high-purity capsaicine from capsicum oleoresin |
| CN102757665A (en) * | 2012-07-28 | 2012-10-31 | 吉林省金塔实业（集团）股份有限公司 | Degumming process of capsicum extract |
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