CN108294312A - A kind of low solvent residue xanthophyll-oil preparation method - Google Patents
A kind of low solvent residue xanthophyll-oil preparation method Download PDFInfo
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- CN108294312A CN108294312A CN201810210578.8A CN201810210578A CN108294312A CN 108294312 A CN108294312 A CN 108294312A CN 201810210578 A CN201810210578 A CN 201810210578A CN 108294312 A CN108294312 A CN 108294312A
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- China
- Prior art keywords
- residual
- xanthophyll
- solvent residue
- low solvent
- oil preparation
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- 239000002904 solvent Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 45
- KBPHJBAIARWVSC-XQIHNALSSA-N trans-lutein 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=CC2C(=CC(O)CC2(C)C)C KBPHJBAIARWVSC-XQIHNALSSA-N 0.000 claims abstract description 34
- 235000012680 lutein Nutrition 0.000 claims abstract description 33
- KBPHJBAIARWVSC-RGZFRNHPSA-N lutein 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=C\C=C(/C)\C=C\[C@H]1C(C)=C[C@H](O)CC1(C)C KBPHJBAIARWVSC-RGZFRNHPSA-N 0.000 claims abstract description 33
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 29
- 239000001656 lutein Substances 0.000 claims abstract description 29
- 229960005375 lutein Drugs 0.000 claims abstract description 29
- ORAKUVXRZWMARG-WZLJTJAWSA-N lutein Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CCCC1(C)C)C=CC=C(/C)C=CC2C(=CC(O)CC2(C)C)C ORAKUVXRZWMARG-WZLJTJAWSA-N 0.000 claims abstract description 29
- FJHBOVDFOQMZRV-XQIHNALSSA-N xanthophyll 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=CC2C=C(C)C(O)CC2(C)C FJHBOVDFOQMZRV-XQIHNALSSA-N 0.000 claims abstract description 29
- 239000001273 butane Substances 0.000 claims abstract description 24
- 239000013078 crystal Substances 0.000 claims abstract description 24
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims abstract description 24
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims abstract description 24
- 241000628997 Flos Species 0.000 claims abstract description 23
- 235000019441 ethanol Nutrition 0.000 claims abstract description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000007127 saponification reaction Methods 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- 235000019871 vegetable fat Nutrition 0.000 claims abstract description 7
- 238000000605 extraction Methods 0.000 claims abstract description 6
- 235000005881 Calendula officinalis Nutrition 0.000 claims abstract description 5
- 240000000785 Tagetes erecta Species 0.000 claims abstract description 5
- 239000000084 colloidal system Substances 0.000 claims abstract description 3
- 239000012467 final product Substances 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 30
- 239000003921 oil Substances 0.000 claims description 25
- 238000002156 mixing Methods 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 5
- 240000008042 Zea mays Species 0.000 claims description 4
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 4
- 235000005713 safflower oil Nutrition 0.000 claims description 4
- 239000003813 safflower oil Substances 0.000 claims description 4
- 235000019486 Sunflower oil Nutrition 0.000 claims description 3
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 claims description 3
- 235000009973 maize Nutrition 0.000 claims description 3
- 239000002600 sunflower oil Substances 0.000 claims description 3
- 241000196324 Embryophyta Species 0.000 claims description 2
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 2
- 239000004519 grease Substances 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 11
- 235000013373 food additive Nutrition 0.000 abstract description 3
- 239000002778 food additive Substances 0.000 abstract description 3
- 230000036541 health Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 73
- 238000001514 detection method Methods 0.000 description 7
- 238000001914 filtration Methods 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 5
- 238000004128 high performance liquid chromatography Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- KKAJSJJFBSOMGS-UHFFFAOYSA-N 3,6-diamino-10-methylacridinium chloride Chemical compound [Cl-].C1=C(N)C=C2[N+](C)=C(C=C(N)C=C3)C3=CC2=C1 KKAJSJJFBSOMGS-UHFFFAOYSA-N 0.000 description 2
- 235000019485 Safflower oil Nutrition 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 2
- 235000019198 oils Nutrition 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 239000007901 soft capsule Substances 0.000 description 2
- JKQXZKUSFCKOGQ-JLGXGRJMSA-N (3R,3'R)-beta,beta-carotene-3,3'-diol 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=CC1=C(C)C[C@@H](O)CC1(C)C JKQXZKUSFCKOGQ-JLGXGRJMSA-N 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 208000035719 Maculopathy Diseases 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- JKQXZKUSFCKOGQ-LQFQNGICSA-N Z-zeaxanthin Natural products C([C@H](O)CC=1C)C(C)(C)C=1C=CC(C)=CC=CC(C)=CC=CC=C(C)C=CC=C(C)C=CC1=C(C)C[C@@H](O)CC1(C)C JKQXZKUSFCKOGQ-LQFQNGICSA-N 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- QOPRSMDTRDMBNK-RNUUUQFGSA-N Zeaxanthin Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CCC(O)C1(C)C)C=CC=C(/C)C=CC2=C(C)CC(O)CC2(C)C QOPRSMDTRDMBNK-RNUUUQFGSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- JKQXZKUSFCKOGQ-LOFNIBRQSA-N all-trans-Zeaxanthin 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=CC2=C(C)CC(O)CC2(C)C JKQXZKUSFCKOGQ-LOFNIBRQSA-N 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 208000003464 asthenopia Diseases 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 235000021466 carotenoid Nutrition 0.000 description 1
- 150000001747 carotenoids Chemical class 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 208000002780 macular degeneration Diseases 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012053 oil suspension Substances 0.000 description 1
- 230000001151 other effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 235000010930 zeaxanthin Nutrition 0.000 description 1
- 239000001775 zeaxanthin Substances 0.000 description 1
- 229940043269 zeaxanthin Drugs 0.000 description 1
Classifications
-
- 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
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- 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
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/115—Fatty acids or derivatives thereof; Fats or oils
-
- 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/12—Ketones
- A61K31/122—Ketones having the oxygen directly attached to a ring, e.g. quinones, vitamin K1, anthralin
-
- 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
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Polymers & Plastics (AREA)
- Food Science & Technology (AREA)
- Engineering & Computer Science (AREA)
- Nutrition Science (AREA)
- Mycology (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Epidemiology (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Pharmacology & Pharmacy (AREA)
- Medicinal Chemistry (AREA)
- Botany (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Medicines Containing Plant Substances (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A kind of low solvent residue xanthophyll-oil preparation method, belongs to food additives preparing technical field.It is characterized by comprising the following steps：A, Flos Tagetis Erectae extract is obtained with liquefied butane extraction marigold under pressurized conditions；B, the carrying agent of the Flos Tagetis Erectae extract quality 1% ~ 10% obtained by step A is added, then carries out vacuumizing for the first time de- residual；Vacuumize for the first time it is de- it is residual after be passed through nitrogen restore normal pressure and add after the carrying agent of the Flos Tagetis Erectae extract quality 1% ~ 5% obtained by step A vacuumized for the second time it is de- residual；C, potassium hydroxide solution is added and carries out saponification, then is diluted with ethyl alcohol, washing, is dried to obtain lutein crystal；D, lutein crystal is mixed with vegetable fat, and colloid mill is ground to obtain the final product.The method of the present invention is simple, easily operated, is suitble to large-scale production, and prepared xanthophyll-oil dissolvent residual is low, is suitble to make health product raw material.
Description
Technical field
A kind of low solvent residue xanthophyll-oil preparation method, belongs to food additives preparing technical field.
Background technology
Lutein belongs to isoprenoid, is a kind of oxygen containing carotenoid, is primarily present in marigold flower and corn etc.
In plant.Lutein and zeaxanthin are isomers, and lutein is the primary pigments of human eye macular area, it can prevent always
Eye-blurred caused by year property maculopathy alleviates visual fatigue and other effects, and human body itself cannot synthesize, and can only be taken the photograph from the external world
It takes.Lutein or a kind of powerful antioxidant can protect machine by Anti-oxidation behaviors such as singlet-oxygen quenching, removing free radicals
Body cell also has the physiological functions such as antitumaous effect, prevention of cardiovascular disease and prevention.
Lutein is used as food additives, mainly lutein is fabricated to after oil suspension the leaf for making soft capsule, but present
Flavine crystal makes raw material Flos Tagetis Erectae extract and is mainly extracted with hexane, and n-hexane residual is higher in product, although follow-up
It carries out taking off the processes processing such as residual in process, but n-hexane remains in 50mg/kg or so in final xanthophyll-oil, limits leaf Huang
The application of vegetable oil.The present invention is mainly the n-hexane residual content reduced in xanthophyll-oil, and method is simple and practicable, is suitble to scale
Production.
Invention content
The technical problem to be solved by the present invention is to：Overcome the deficiencies of the prior art and provide it is a kind of it is simple and practicable, without n-hexane
Remaining low solvent residue xanthophyll-oil preparation method.
The technical solution adopted by the present invention to solve the technical problems is：The low solvent residue xanthophyll-oil preparation method,
It is characterized by comprising the following steps：
A, Flos Tagetis Erectae extract is obtained with liquefied butane extraction marigold under pressurized conditions；
B, the carrying agent of the Flos Tagetis Erectae extract quality 1% ~ 10% obtained by step A is added, then carries out vacuumizing for the first time de- residual；
Vacuumize for the first time it is de- it is residual after be passed through nitrogen and restore normal pressure and add Flos Tagetis Erectae extract quality 1% ~ 5% obtained by step A
It is vacuumized for the second time after carrying agent de- residual；
C, potassium hydroxide solution is added and carries out saponification, then is diluted with ethyl alcohol, washing, is dried to obtain lutein crystal；
D, lutein crystal is mixed with vegetable fat, and colloid mill is ground to obtain the final product.
The present invention provides a kind of preparation methods without molten residual xanthophyll-oil.Mainly solution is extracted marigold with n-hexane and is carried
Take n-hexane dissolvent residual in object that cannot completely remove clean problem.Solvent butane boiling point used in the present invention is -0.5 DEG C,
It is volatile, it, will not also can not be as the extractant of this field under normal conditions because butane is gas under normal conditions.The present invention's
Inventor, which uses, is liquefied butane in a manner of pressurization, and dissolvent residual is more easy in the Flos Tagetis Erectae extract extracted with butane
It removes, and can preferably ensure extraction efficiency, n-hexane（Butane is in terms of n-hexane）Dissolvent residual is less than 1000mg/kg, and to leaf
Flavine destructiveness is small, and carrying agent, which is added, can help the removal of butane, realizes de- residual in the process molten in Flos Tagetis Erectae extract
Agent butane all removes.In saponification process, ethyl alcohol dilute filtration is added, n-hexane will not be brought into, is contained by dry crystal ethyl alcohol
Amount is less than 0.1%, adds the vegetable fat without n-hexane, you can obtain without molten residual（N-hexane, butane）Lutein
Oil.
Preferably, the carrying agent is the arbitrary proportion mixture of one or both of ethyl alcohol, ethyl acetate.Invention
The preferred carrying agent that people provides can more thoroughly remove dissolvent residual.
Preferably, the carrying agent is ethyl alcohol and ethyl acetate in mass ratio 3 ~ 5：1 mixture.What inventor provided
Preferred carrying agent can thoroughly remove dissolvent residual within the shorter time with less dosage.
Preferably, the first time vacuumize it is de- residual and vacuumize for the second time it is de- it is residual take off residual tank in carry out, it is described
It takes off residual tank and carries gate stirrer.It is de- it is residual during can high-speed stirred, can be with less carrying agent dosage when shorter
Interior thorough removal dissolvent residual.
Preferably, the operation temperature when first time vacuumizes de- residual is 60 DEG C~65 DEG C, and pressure is -0.095MPa
~-0.100MPa takes off residual time 2h ~ 6h.Preferred treatment temperature and pressure can more be gone with less carrying agent dosage
Except dissolvent residual.
Preferably, described to vacuumize de- residual addition for the second time and carry agent, operation temperature is 65 DEG C~70 DEG C, pressure is-
0.095MPa~-0.100MPa takes off residual time 2h ~ 8h.Preferred treatment temperature and pressure can be with less carrying agent dosages
Thoroughly removal dissolvent residual.
Preferably, it is the Flos Tagetis Erectae extract quality obtained by step A to vacuumize the de- residual preceding addition for carrying agent for the first time
4.5%~7%。
Preferably, it is the Flos Tagetis Erectae extract quality obtained by step A to vacuumize the de- residual preceding addition for carrying agent for the second time
2%~3%。
Preferably, the vegetable fat is using in sunflower oil made from squeezing process, maize germ oil, safflower oil
A kind of or arbitrary two or more mixture.Preferred vegetable fat is made using squeezing process, is not had in grease remaining
Dissolve out solvent.
Compared with prior art, of the invention a kind of to be without advantageous effect possessed by molten residual xanthophyll-oil preparation method：
Solvent butane boiling point used in the present invention is -0.5 DEG C, volatile.More with dissolvent residual in the Flos Tagetis Erectae extract of butane extraction
Easily removal, n-hexane（Butane is in terms of n-hexane）Dissolvent residual is less than 1000mg/kg, and small to lutein destructiveness, and addition is taken
The removal of butane can be helped with agent, realized de- residual in the process all removals of the solvent butane in Flos Tagetis Erectae extract.Saponification
In the process, ethyl alcohol dilute filtration is added, n-hexane will not be brought into, is less than 0.1% by dry crystal ethanol content, then add
Enter to be free of the vegetable fat of n-hexane, you can obtain without molten residual（N-hexane, butane）Xanthophyll-oil.In products obtained therefrom of the present invention
N-hexane（Butane is in terms of n-hexane）Alkane residual is extremely low, this preparation method resulting product fineness can reach Nano grade, be convenient for
Absorption of human body can be used in food, medicine and health products, can also be used to the core material for making soft capsule.This method elapsed time
Short, easy to operate, product quality is stablized, and is suitble to large-scale industrial production.
Specific implementation mode
With reference to specific embodiment, the present invention will be further described, and wherein embodiment 1 is most preferably to implement, in embodiment
Butane residual is in terms of n-hexane residual.N-hexane detection method is measured by GB26405-2011 " the A.5 measurement of n-hexane ".
The residual quantity of n-hexane is with the mass fraction of n-hexanew 3Meter, numerical value with milligrams per kilogram（mg/kg）It indicates.
Embodiment 1
It is vertical it to be put into 1 with the Flos Tagetis Erectae extract double centner of liquefied butane extraction content 16% under the pressurized conditions more than 380kPa
In the frame type stirring reaction kettle of square rice, detection n-hexane remains 500mg/kg, and ethyl alcohol and ethyl acetate in mass ratio 4 is added：1
Mixing carries 5.5 kilograms of agent, and 62 DEG C of vacuum -0.097MPa take off residual 2 hours, continuously add 2.5 kilograms of ethyl alcohol, and be passed through nitrogen,
68 DEG C of vacuum -0.096MPa take off residual 2 hours, and n-hexane residual does not detect.Take de- residual rear product that 50% potassium hydroxide is added
42 kilograms of aqueous solution, 72 DEG C carry out saponification 3 hours, continuously add 50%（V/V）500 kilograms of ethyl alcohol is diluted filtering, crystal 45
DEG C dry 6 hours, 15.4 kilograms of 89% lutein crystal is obtained, trans-lutein ratio 93.4% takes 15 kilograms of crystal and 46,000
Gram squeezing safflower oil mixing high-pressure homogeneous arrives xanthophyll-oil.Detect lutein content（UV）22.33%, lutein content
（HPLC）20.57%, n-hexane residual does not detect.
Embodiment 2
The Flos Tagetis Erectae extract double centner that content 15.8% is extracted with liquefied butane under the pressurized conditions more than 380kPa is put into 1
In the frame type stirring reaction kettle of cubic meter, detection n-hexane remains 600mg/kg, and ethyl alcohol and ethyl acetate in mass ratio 3 is added：1
Mixing carry 7 kilograms of agent, 60 DEG C of vacuum -0.098MPa take off residual 4 hours, continuously add ethyl alcohol and ethyl acetate in mass ratio 1：
1 mixing carries 3 kilograms of agent, and is passed through nitrogen, and 65 DEG C of vacuum 0.095MPa take off residual 3 hours, and n-hexane residual does not detect.It takes
42 kilograms of 50% potassium hydroxide aqueous solution is added in de- residual rear product, and 72 DEG C carry out saponification 3 hours, continuously add 50%（V/V）
500 kilograms of ethyl alcohol is diluted filtering, and the drying 6 hours of 45 DEG C of crystal obtains 15.6 kilograms of 87% lutein crystal, and trans- leaf is yellow
Plain ratio 93.0% takes 15 kilograms of crystal and 46 kilograms to squeeze maize germ oils mixing, high-pressure homogeneous arrive xanthophyll-oil.Detection
Lutein content（UV）22.2%, lutein content（HPLC）20.60%, n-hexane residual does not detect.
Embodiment 3
The Flos Tagetis Erectae extract double centner that content 16.3% is extracted with liquefied butane under pressurized conditions is put into 1 cubic metre of frame
In stirred autoclave, detection n-hexane remains 200mg/kg, and ethyl alcohol and ethyl acetate in mass ratio 5 is added：1 mixing carries agent
4.5 kilograms, 65 DEG C of vacuum -0.095MPa take off residual 3 hours, continuously add 2 kilograms of ethyl acetate, and be passed through nitrogen, 70 DEG C of vacuum -
0.100MPa takes off residual 3 hours, and n-hexane residual does not detect.Take de- residual rear product that 50% potassium hydroxide aqueous solution 42 is added
Kilogram, 72 DEG C carry out saponification 3 hours, continuously add 50%（V/V）500 kilograms of ethyl alcohol is diluted filtering, 45 DEG C of dryings 6 of crystal
Hour, 15.6 kilograms of 87% lutein crystal is obtained, trans-lutein ratio 92.9% takes 15 kilograms of crystal and 46 kilograms of squeezings red
Caul-fat mixing high-pressure homogeneous arrives xanthophyll-oil.Detect lutein content（UV）22.3%, lutein content（HPLC）20.58%,
N-hexane residual does not detect.
Embodiment 4
The Flos Tagetis Erectae extract double centner that content 16.5% is extracted with liquefied butane under the pressurized conditions more than 380kPa is put into 1
In the frame type stirring reaction kettle of cubic meter, detection n-hexane remains 700mg/kg, and 10 kilograms of ethyl alcohol, 62 DEG C of vacuum-are added
0.100MPa takes off residual 4 hours, continuously adds ethyl alcohol and ethyl acetate in mass ratio 10：1 mixing carries 1 kilogram of agent, and is passed through
Nitrogen, 68 DEG C of vacuum -0.096MPa take off residual 4 hours, and n-hexane residual does not detect.Take de- residual rear product that 50% hydrogen is added
42 kilograms of aqueous solutions of potassium is aoxidized, 72 DEG C carry out saponification 3 hours, continuously add 50%（V/V）500 kilograms of ethyl alcohol is diluted filtering,
The drying 6 hours of 45 DEG C of crystal, obtains 15.5 kilograms of 87% lutein crystal, and trans-lutein ratio 92.8% takes 15 kilograms of crystal
With 46 kilograms of squeezing sunflower oils mixing, high-pressure homogeneous arrive xanthophyll-oil.Detect lutein content（UV）22.2%, lutein contains
Amount（HPLC）20.56%, n-hexane residual does not detect.
Embodiment 5
The Flos Tagetis Erectae extract double centner that content 15.5% is extracted with liquefied butane under the pressurized conditions more than 380kPa is put into 1
In the frame type stirring reaction kettle of cubic meter, detection n-hexane remains 300mg/kg, and 92% ethanol water 1,000 of mass fraction is added
Gram, 62 DEG C of vacuum -0.097MPa take off residual 6 hours, continuously add 6 kilograms of 92% ethanol water of mass fraction, and be passed through nitrogen,
68 DEG C of vacuum -0.096MPa take off residual 8 hours, and n-hexane residual does not detect.Take de- residual rear product that 50% potassium hydroxide is added
42 kilograms of aqueous solution, 72 DEG C carry out saponification 3 hours, continuously add 50%（V/V）500 kilograms of ethyl alcohol is diluted filtering, crystal 45
DEG C dry 6 hours, 15.8 kilograms of 86% lutein crystal is obtained, trans-lutein ratio 92.8% takes 15 kilograms of crystal and 46,000
Gram squeezing safflower oil mixing high-pressure homogeneous arrives xanthophyll-oil.Detect lutein content（UV）22.1%, lutein content
（HPLC）20.35%, n-hexane residual does not detect.
The above described is only a preferred embodiment of the present invention, being not that the invention has other forms of limitations, appoint
What those skilled in the art changed or be modified as possibly also with the technology contents of the disclosure above equivalent variations etc.
Imitate embodiment.But it is every without departing from technical solution of the present invention content, according to the technical essence of the invention to above example institute
Any simple modification, equivalent variations and the remodeling made, still fall within the protection domain of technical solution of the present invention.
Claims (9)
1. a kind of low solvent residue xanthophyll-oil preparation method, which is characterized in that include the following steps：
A, Flos Tagetis Erectae extract is obtained with liquefied butane extraction marigold under pressurized conditions；
B, the carrying agent of the Flos Tagetis Erectae extract quality 1% ~ 10% obtained by step A is added, then carries out vacuumizing for the first time de- residual；
Vacuumize for the first time it is de- it is residual after be passed through nitrogen and restore normal pressure and add Flos Tagetis Erectae extract quality 1% ~ 5% obtained by step A
It is vacuumized for the second time after carrying agent de- residual；
C, potassium hydroxide solution is added and carries out saponification, then is diluted with ethyl alcohol, washing, is dried to obtain lutein crystal；
D, lutein crystal is mixed with vegetable fat, and colloid mill is ground to obtain the final product.
2. a kind of low solvent residue xanthophyll-oil preparation method according to claim 1, it is characterised in that：The carrying
Agent is the arbitrary proportion mixture of one or both of ethyl alcohol, ethyl acetate.
3. a kind of low solvent residue xanthophyll-oil preparation method according to claim 1, it is characterised in that：The carrying
Agent is ethyl alcohol and ethyl acetate in mass ratio 3 ~ 5：1 mixture.
4. a kind of low solvent residue xanthophyll-oil preparation method according to claim 1, it is characterised in that：Described first
It is secondary vacuumize it is de- residual and vacuumize for the second time it is de- it is residual carry out taking off in residual tank, it is described to take off residual tank and carry gate stirrer.
5. a kind of low solvent residue xanthophyll-oil preparation method according to claim 1, it is characterised in that：Described first
Secondary operation temperature when vacuumizing de- residual is 60 DEG C~65 DEG C, and pressure is -0.095MPa~-0.100MPa, take off residual time 2h ~
6h。
6. a kind of low solvent residue xanthophyll-oil preparation method according to claim 1, it is characterised in that：Described second
Secondary to vacuumize de- residual addition carrying agent, operation temperature is 65 DEG C~70 DEG C, and pressure is -0.095MPa~-0.100MPa, when taking off residual
Between 2h ~ 8h.
7. a kind of low solvent residue xanthophyll-oil preparation method according to claim 1, it is characterised in that：It takes out for the first time true
The de- residual preceding addition for carrying agent of sky is the Flos Tagetis Erectae extract quality 4.5% ~ 7% obtained by step A.
8. a kind of low solvent residue xanthophyll-oil preparation method according to claim 1, it is characterised in that：Second of pumping is true
The de- residual preceding addition for carrying agent of sky is the Flos Tagetis Erectae extract quality 2% ~ 3% obtained by step A.
9. a kind of low solvent residue xanthophyll-oil preparation method according to claim 1, it is characterised in that：The plant
Grease be using in sunflower oil made from squeezing process, maize germ oil, safflower oil one kind or arbitrary two or more mixing
Object.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113797182A (en) * | 2021-10-14 | 2021-12-17 | 云南博瑞生物科技有限公司 | Method for preparing lutein oil suspension |
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