CN108813616A - A method of preparing lutein water-soluble microemulsion - Google Patents
A method of preparing lutein water-soluble microemulsion Download PDFInfo
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- CN108813616A CN108813616A CN201810732211.2A CN201810732211A CN108813616A CN 108813616 A CN108813616 A CN 108813616A CN 201810732211 A CN201810732211 A CN 201810732211A CN 108813616 A CN108813616 A CN 108813616A
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- water
- lutein
- saponification
- soluble
- oil
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- 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 title claims abstract description 107
- 239000001656 lutein Substances 0.000 title claims abstract description 104
- 235000012680 lutein Nutrition 0.000 title claims abstract description 104
- 229960005375 lutein Drugs 0.000 title claims abstract description 104
- 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 title claims abstract description 104
- 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 title claims abstract description 104
- 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 title claims abstract description 104
- 239000004530 micro-emulsion Substances 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000007127 saponification reaction Methods 0.000 claims abstract description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 239000000839 emulsion Substances 0.000 claims abstract description 28
- 239000003995 emulsifying agent Substances 0.000 claims description 40
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 238000005119 centrifugation Methods 0.000 claims description 18
- 239000012530 fluid Substances 0.000 claims description 18
- 239000003963 antioxidant agent Substances 0.000 claims description 16
- 230000003078 antioxidant effect Effects 0.000 claims description 16
- 235000006708 antioxidants Nutrition 0.000 claims description 16
- 239000003381 stabilizer Substances 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 15
- 229920000223 polyglycerol Polymers 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 235000010489 acacia gum Nutrition 0.000 claims description 11
- 239000001785 acacia senegal l. willd gum Substances 0.000 claims description 11
- 229920002907 Guar gum Polymers 0.000 claims description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 10
- 239000000665 guar gum Substances 0.000 claims description 10
- 235000010417 guar gum Nutrition 0.000 claims description 10
- 229960002154 guar gum Drugs 0.000 claims description 10
- 241000206575 Chondrus crispus Species 0.000 claims description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 8
- 244000269722 Thea sinensis Species 0.000 claims description 8
- 150000008442 polyphenolic compounds Chemical class 0.000 claims description 8
- 235000013824 polyphenols Nutrition 0.000 claims description 8
- 229920000136 polysorbate Polymers 0.000 claims description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 7
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 6
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 6
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 6
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 6
- 230000008859 change Effects 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 5
- 239000000263 2,3-dihydroxypropyl (Z)-octadec-9-enoate Substances 0.000 claims description 4
- RZRNAYUHWVFMIP-GDCKJWNLSA-N 3-oleoyl-sn-glycerol Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@H](O)CO RZRNAYUHWVFMIP-GDCKJWNLSA-N 0.000 claims description 4
- 239000006071 cream Substances 0.000 claims description 4
- 230000001804 emulsifying effect Effects 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- RZRNAYUHWVFMIP-UHFFFAOYSA-N monoelaidin Natural products CCCCCCCCC=CCCCCCCCC(=O)OCC(O)CO RZRNAYUHWVFMIP-UHFFFAOYSA-N 0.000 claims description 4
- GDSOZVZXVXTJMI-SNAWJCMRSA-N (e)-1-methylbut-1-ene-1,2,4-tricarboxylic acid Chemical compound OC(=O)C(/C)=C(C(O)=O)\CCC(O)=O GDSOZVZXVXTJMI-SNAWJCMRSA-N 0.000 claims 1
- CKQVRZJOMJRTOY-UHFFFAOYSA-N octadecanoic acid;propane-1,2,3-triol Chemical compound OCC(O)CO.CCCCCCCCCCCCCCCCCC(O)=O CKQVRZJOMJRTOY-UHFFFAOYSA-N 0.000 claims 1
- 235000013305 food Nutrition 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 16
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 14
- 230000006872 improvement Effects 0.000 description 9
- 238000004062 sedimentation Methods 0.000 description 9
- 235000010323 ascorbic acid Nutrition 0.000 description 7
- 229960005070 ascorbic acid Drugs 0.000 description 7
- 239000011668 ascorbic acid Substances 0.000 description 7
- 238000004945 emulsification Methods 0.000 description 7
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 235000015165 citric acid Nutrition 0.000 description 6
- 230000001376 precipitating effect Effects 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 235000013616 tea Nutrition 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 231100000252 nontoxic Toxicity 0.000 description 3
- 230000003000 nontoxic effect Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 235000016709 nutrition Nutrition 0.000 description 2
- 230000035764 nutrition Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- 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 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 244000241257 Cucumis melo Species 0.000 description 1
- 235000015510 Cucumis melo subsp melo Nutrition 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- FJJCIZWZNKZHII-UHFFFAOYSA-N [4,6-bis(cyanoamino)-1,3,5-triazin-2-yl]cyanamide Chemical compound N#CNC1=NC(NC#N)=NC(NC#N)=N1 FJJCIZWZNKZHII-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- VJHCJDRQFCCTHL-UHFFFAOYSA-N acetic acid 2,3,4,5,6-pentahydroxyhexanal Chemical compound CC(O)=O.OCC(O)C(O)C(O)C(O)C=O VJHCJDRQFCCTHL-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 1
- 235000021466 carotenoid Nutrition 0.000 description 1
- 150000001747 carotenoids Chemical class 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000004438 eyesight Effects 0.000 description 1
- 235000012465 frozen bakery product Nutrition 0.000 description 1
- 235000013611 frozen food Nutrition 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 125000005456 glyceride group Chemical group 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000000215 hyperchromic effect Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 235000015094 jam Nutrition 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 239000007762 w/o emulsion Substances 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 OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- 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 OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/015—Inorganic compounds
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/03—Organic compounds
- A23L29/035—Organic compounds containing oxygen as heteroatom
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/10—Foods or foodstuffs containing additives; Preparation or treatment thereof containing emulsifiers
-
- 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)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Botany (AREA)
- Mycology (AREA)
- Cosmetics (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a kind of methods for preparing lutein water-soluble microemulsion, belong to chemicals field, the common stage of reaction including carrying out emulsion reaction while saponification.The present invention can be improved the stability of lutein, improve its water solubility, extend application range of the lutein in food, entire simple production process, at low cost, suitable large-scale industrial production.
Description
Technical field
The present invention relates to microemulsion, especially a kind of water-soluble microemulsion belongs to chemicals field.
Background technique
Lutein also known as " Lutein " are a kind of natural goods being widely present in the plants such as vegetables, flowers, fruit
Matter belongs to " carotenoids class " race's substance.Lutein have the characteristics that lovely luster, strong coloring force, it is safe and non-toxic, rich in nutrition,
It is widely used in the fields such as food, cosmetics, feed.With the further investigation discovery to lutein pharmacology, lutein is one
Kind excellent antioxidant, protect eyesight and pre- anti-cancer and in terms of have exact effect.Lutein
As a kind of with hyperchromic and food, auxiliary pharmaceutical adjuvants of nutrition double effects, because of its unique bioactivity, in food processing
It is more and more paid close attention to in health medicine by people.
Lutein mainly exists in the form of lutein ester in plant, and lutein ester can not be direct by human body and birds
It is absorbed and utilized, it is necessary to which being saponified could use for free lutein.And lutein is oil-soluble mostly, the lutein of oily is not
Conducive to addition, digestion, absorption, property not soluble in water limits its application in food, especially water-based food such as
Application in beverage, jelly and jam based food, frozen food and bakery product class.Meanwhile lutein is vulnerable to light, oxygen, high temperature
The effects of and degrade, stability is poor.Therefore, the water solubility and stability for how improving lutein, expanding its use scope is this
Field technical staff's urgent problem.
The method of water-soluble lutein microemulsion is prepared mainly using cream after being first saponified by raw material of lutein extract at present
The mode of change, the preparation method recorded in patent document CN201210136504.7 are：Lutein extract saponification, which is made, to be had
Then water-soluble saponification lutein extract is added emulsifier and water, stirs under water bath condition, liquid lutein is made.The party
Method will be saponified and emulsification separately carries out, and technique is cumbersome, and production efficiency is low.It is only stirred, is not carried out equal when emulsifying simultaneously
Matter, emulsifying effectiveness is poor, can also will affect final containing suspended matters such as lutein crystals, if not being centrifuged off in lotion after emulsification
The homogeneity and stability of product.
Summary of the invention
The technical problem to be solved by the invention is to provide a kind of method for preparing lutein water-soluble microemulsion, Neng Gouti
The stability of high lutein improves its water solubility, extends application range of the lutein in food, entire simple production process,
It is at low cost, it is suitble to large-scale industrial production.
In order to solve the above technical problems, the technical scheme adopted by the invention is that：
A method of lutein water-soluble microemulsion being prepared, including carrying out being total to for emulsion reaction while saponification
The same stage of reaction.
Technical solution of the present invention further improvement lies in that：The time of the common stage of reaction is 1~4 hour, by soap
Change liquid and mix emulsion fluid to be added in the reaction vessel containing lutein extract simultaneously or successively, saponification liquor and mix emulsion fluid are successive
The time interval of addition was less than 1 hour.
Technical solution of the present invention further improvement lies in that：Reaction vessel Lutein before addition saponification liquor and emulsion
The content of medicinal extract is 300~400g/kg, and saponification liquor is the potassium hydroxide solution of mass fraction 60~70%, at 70~90 DEG C
Saponification liquor is added while stirring and is passed through inert gas.
Technical solution of the present invention further improvement lies in that：Mix emulsion fluid be dehydrated alcohol, oil-in-water emulsifiers and
Water-in-oil emulsifier, dehydrated alcohol, oil-in-water emulsifiers and water-in-oil emulsifier mass ratio are 5:1:0.5~1.
Technical solution of the present invention further improvement lies in that：Oil-in-water emulsifiers are in tween and polyglycerol monooleate
Any one or two kinds combination, water-in-oil emulsifier is this disk, polyglycerol stearate, Unigly GO 102S and single oil
Any one or the combination of several of them in acid glyceride.
Technical solution of the present invention further improvement lies in that：After the completion of saponification and emulsion reaction, homogeneous, centrifugation are carried out.
Technical solution of the present invention further improvement lies in that：Revolving speed is 2000~3000r/min when homogeneous, and homogenizing time is
10~20min.
Technical solution of the present invention further improvement lies in that：Revolving speed is 4000~5000r/min when centrifugation, and centrifugation time is
5~10min.
Technical solution of the present invention further improvement lies in that：Stabilizer and antioxidant are added in upper layer after centrifugation,
Matter obtains lutein water-soluble microemulsion.
Technical solution of the present invention further improvement lies in that：Stabilizer is Arabic gum, guar gum, carragheen and carboxymethyl
Any one or the combination of several of them in cellulose, antioxidant are any one in ascorbic acid, citric acid and tea polyphenols
Or several combination；The mass fraction of stabilizer is 10~20%, and additional amount is 0.5~2% of upper liquid quality after being centrifuged；It is anti-
The additional amount of oxidant is 0.2~1% of upper liquid quality after being centrifuged.
By adopting the above-described technical solution, the technological progress achieved by the present invention is：
A kind of method preparing lutein water-soluble microemulsion provided by the invention, can be improved the stability of lutein,
Improve its water solubility, extends application range of the lutein in food, it is entire simple production process, at low cost, it is suitble to extensive
Industrialized production.
The present invention includes that the common stage of reaction of emulsion reaction is carried out while saponification, will be newborn in saponification process
Agent is coated on lutein surface, increases the dispersity of free lutein, and the stability of the microemulsion made is more preferable.?
When lutein ester in lutein extract is saponified into free lutein, with the generation of lutein, just carried out with emulsifier
Emulsion reaction is emulsified when generating lutein, it is ensured that emulsification carries out completely, the obtained lutein microemulsion middle period
Flavine content height, good water solubility, property stable homogeneous, while shortening process flow, improve working efficiency.
The present invention has carried out homogeneous, centrifugation after saponification and emulsification.In saponification and emulsification, keep it mixed simply by stirring
It closes, undercompounding, lutein water-soluble microemulsion can be layered even generation precipitating after placing a period of time.It is being saponified and is emulsifying
After carry out homogeneous, can be reached by the shearing force of homogenizer high speed makes the well-mixed purpose of material, when homogeneous revolving speed be 2000
When~3000r/min, homogenizing time are 10~20min, the microemulsion stable homogeneous of formation has good dispersibility and dissolution
Property, lamination will not be generated after placement.In saponification and emulsification, understand some lutein and be precipitated with crystal form, suspends
In microemulsion, if do not removed, the homogeneity and stability of microemulsion will affect, therefore after homogeneous, homogenizing fluid is centrifuged, is removed
Remove lutein crystal therein, remaining microemulsion is then the water-soluble microemulsion of stable homogeneous, when centrifugal rotational speed be 4000~
5000r/min, when centrifugation time is 5~10min, obtained lutein water-soluble microemulsion stability is best.
Saponification liquor is slowly dropped into lutein extract by the present invention when being saponified, can prevent from being added due to saponification liquor speed it is fast and
Lutein extract is caused to carbonize.The content that lutein extract is controlled when saponification is 300~400g/kg, and saponification liquor is mass fraction
60~70% potassium hydroxide solution, it is ensured that lutein extract has good dispersibility, meets saponification needs, and saponification liquor is dense
Degree is too low, then lutein extract poor dispersion, influences the progress of saponification, and saponification is incomplete；Saponification liquor concentration is too high, then
It is saponified obtained lutein easily to decompose under strong alkali environment, so that lutein content declines, reduces saponification yield.Heating temperature is
70~90 DEG C, obtained lutein content is high, and saponification temperature is low, then saponification is incomplete；Saponification temperature is high, then lutein occurs high
Temperature oxidation causes content to reduce.Mixing time is 2~4h, and obtained lutein content is high, and saponification time is short, then is saponified endless
Entirely；Saponification time is long, then oxidative degradation and isomerization occur under alkaline condition for lutein causes content to reduce.While stirring
It is passed through inert gas, lutein can be prevented to be oxidized degradation.By to saponification liquor concentration, saponification temperature, mixing time (saponification
Time), the comprehensively control of logical inert gas, ensure that lutein extract saponification completely, saponification process Lutein is not oxidized,
Obtained lutein content is high.
Oil-in-water emulsifiers and water-in-oil emulsifier are used cooperatively by the present invention, with water-in-oil emulsifier by grease
It wraps up, is then emulsified again with oil-in-water emulsifiers, oil-soluble lutein is transformed into water-soluble lutein,
Change its dissolubility, when mass ratio be 5:1:When 0.5~1, it is ensured that lutein extract has good dispersibility, simultaneously
Emulsibility is preferable.When oil-in-water emulsifiers are the combination of any one or two kinds in tween and polyglycerol monooleate, shape
At microemulsion good water solubility.Water-in-oil emulsifier is that this disk, polyglycerol stearate, Unigly GO 102S and single oleic acid are sweet
When any one or the combination of several of them in grease, the microemulsion of formation is uniform, no suspension or precipitating.Pass through lower alcohol, Shui Bao
Oil type emulsifier and water-in-oil emulsifier are used cooperatively, obtained water-soluble microemulsion property stable homogeneous, and no precipitating produces
It is raw.If only using single emulsifier, obtained microemulsion water solubility is poor, has suspended matter, precipitating, and stability is poor.
Stabilizer and antioxidant is added in the present invention in lutein water-soluble microemulsion.Stabilizer is Arabic gum, melon
Any one or the combination of several of them in your glue, carragheen and carboxymethyl cellulose.Arabic gum is a kind of good hydrophilic gel
Body, it is easy to be dissolved in cold/hot water, Arabic gum molecule polar groups can form multimolecular film at oil/water interface, can reduce
Oil/water interfacial tension increases storage-stable, and Arabic gum source is sufficient, cheap, safe and non-toxic.Guar gum is in cold water
With good dispersibility is all had in hot water, will not conglomeration, have with anion, amphoteric ion and surfactant good
Compatibility.Carragheen has good water-retaining property, thickening property and emulsibility, can generate association with Arabic gum, guar gum isocolloid
Same-action improves the emulsibility and water-retaining property of colloid.Carboxymethyl cellulose can form highly viscous solution, there is adhesion, emulsification point
The characteristics such as scattered, water conservation, and it is safe and non-toxic.It, can when Arabic gum, guar gum, carragheen and carboxymethyl cellulose are applied in combination
Better play the effect of thick stabilization.When the mass fraction of stabilizer is 10~20%, additional amount is upper liquid matter after centrifugation
Amount 0.5~2% when, the lutein water-soluble microemulsion optimal stability that is prepared.Antioxidant is ascorbic acid, lemon
The combination of acid and any one or more of tea polyphenols, ascorbic acid, citric acid and tea polyphenols have stronger oxidation resistance,
And it is soluble easily in water, when the additional amount of antioxidant be centrifugation after upper liquid quality 0.2~1% when, it will be able to protect lutein
Water-soluble microemulsion is not oxidized during placement, in addition, ascorbic acid, citric acid and tea polyphenols are all from natural plants
The effective component extracted in extract, it is safe and healthy.
Lutein microemulsion good water solubility prepared by the present invention, no suspended substance, without precipitating, stable homogeneous and high conversion rate,
Particularly suitable in aqueous-based food.
Specific embodiment
Here is certain specific embodiments of the invention, to be described in further detail.
A method of lutein water-soluble microemulsion being prepared, including carrying out being total to for emulsion reaction while saponification
The same stage of reaction.
Preparation method includes the following steps：
A. it weighs：A certain amount of lutein extract is weighed, the content of lutein extract is 300~400g/kg.
B. mix emulsion fluid is prepared：By dehydrated alcohol, oil-in-water emulsifiers and water-in-oil emulsifier according to mass ratio
5:1:0.5~1 ratio is uniformly mixed.Oil-in-water emulsifiers are any one or two in tween and polyglycerol monooleate
The combination of kind, water-in-oil emulsifier are appointing in this disk, polyglycerol stearate, Unigly GO 102S and glyceryl monooleate
The combination for one or more of anticipating.
C. it is saponified and emulsifies：The reaction vessel containing lutein extract is added in saponification liquor and mix emulsion fluid simultaneously or successively
In, for the time interval that saponification liquor and mix emulsion fluid are successively added less than 1 hour, the time of the common stage of reaction was 1~4 small
When.Saponification liquor is added while stirring at 70~90 DEG C and is passed through inert gas, continuing stirring to reaction terminates.
Saponification liquor is the potassium hydroxide solution of mass fraction 60~70%；Mix emulsion fluid is dehydrated alcohol, oil-in-water type
Emulsifier and water-in-oil emulsifier, dehydrated alcohol, oil-in-water emulsifiers and water-in-oil emulsifier mass ratio are 5:1:0.5
~1；Oil-in-water emulsifiers are the combination of any one or two kinds in tween and polyglycerol monooleate, water-in-oil emulsion
Agent is any one or the combination of several of them in this disk, polyglycerol stearate, Unigly GO 102S and glyceryl monooleate.
D. homogeneous：Distilled water is added, is sufficiently mixed rear high shear homogeneous, the homogeneous 10 under 2000~3000r/min revolving speed
~20min.
E. it is centrifuged：Solution after homogeneous is centrifuged 5~10min under 4000~5000r/min revolving speed.
Plus stabilizer and antioxidant F.：Stabilizer is added in upper liquid after centrifugation and antioxidant, homogeneous obtain
Lutein water-soluble microemulsion.
Stabilizer is any one or the combination of several of them in Arabic gum, guar gum, carragheen and carboxymethyl cellulose,
Antioxidant is any one or the combination of several of them in ascorbic acid, citric acid and tea polyphenols；The mass fraction of stabilizer is
10~20%, additional amount is 0.5~2% of upper liquid quality after being centrifuged；The additional amount of antioxidant is upper liquid matter after centrifugation
The 0.2~1% of amount.
Embodiment 1
A method of lutein water-soluble microemulsion being prepared, including carrying out being total to for emulsion reaction while saponification
The same stage of reaction.
Preparation method includes the following steps：
A. it weighs：30g lutein extract is weighed, the content of lutein extract is 328.42g/kg.
B. mix emulsion fluid is prepared：By dehydrated alcohol, tween and this disk according to 5:1:0.5 mass ratio is configured to mixing cream
Change liquid.
C. it is saponified and emulsifies：Under stirring simultaneously by 66.7% potassium hydroxide solution 3g and mix emulsion fluid 45g
It is slowly dropped in lutein extract, is heated to 80 DEG C, be passed through nitrogen, stir 1h.
D. homogeneous：150g distilled water is added, is sufficiently mixed rear high shear homogeneous, the homogeneous under 2000r/min revolving speed
10min。
E. it is centrifuged：Solution after homogeneous is centrifuged 5min under 4000r/min revolving speed.
Plus stabilizer and antioxidant F.：It is 15% Arabic gum that 2.5g mass fraction is added in upper liquid after centrifugation
Solution and 0.45g ascorbic acid, high shear homogeneous 5min under 2000r/min revolving speed, obtain lutein water-soluble microemulsion.
Embodiment 2
A method of lutein water-soluble microemulsion being prepared, including carrying out being total to for emulsion reaction while saponification
The same stage of reaction.
Preparation method includes the following steps：
A. it weighs：30g lutein extract is weighed, the content of lutein extract is 398.42g/kg.
B. mix emulsion fluid is prepared：By dehydrated alcohol, oil-in-water emulsifiers and water-in-oil emulsifier according to mass ratio
5:1:1 ratio is configured to mix emulsion fluid.Wherein oil-in-water emulsifiers are polyglycerol monooleate, water-in-oil emulsifier
For polyglycerol stearate and Unigly GO 102S, (polyglycerol stearate and Unigly GO 102S mass ratio are 2:1).
C. it is saponified and emulsifies：60% potassium hydroxide solution 6g is slowly dropped to lutein extract under stirring
In, 70 DEG C are heated to, nitrogen is passed through, mix emulsion fluid 50g is added after 30 minutes, continues to stir 4h.
D. homogeneous：170g distilled water is added, is sufficiently mixed rear high shear homogeneous, the homogeneous under 3000r/min revolving speed
20min。
E. it is centrifuged：Solution after homogeneous is centrifuged 10min under 5000r/min revolving speed.
Plus stabilizer and antioxidant F.：The guar gum and card that 4g mass fraction is 10% are added in upper layer after centrifugation
Drawing glue mixed solution, (mass ratio of guar gum and carragheen is 1:2), 0.4g citric acid and 0.1g tea polyphenols, 2000r/min turn
The lower high shear homogeneous 5min of speed, obtains lutein water-soluble microemulsion.
Embodiment 3
A method of lutein water-soluble microemulsion being prepared, including carrying out being total to for emulsion reaction while saponification
The same stage of reaction.
Preparation method includes the following steps：
A. it weighs：30g lutein extract is weighed, the content of lutein extract is 308.42g/kg.
B. mix emulsion fluid is prepared：By dehydrated alcohol, oil-in-water emulsifiers and water-in-oil emulsifier according to mass ratio
5:1:0.7 ratio is configured to mix emulsion fluid.Wherein oil-in-water emulsifiers be tween and polyglycerol monooleate (tween and
Polyglycerol monooleate mass ratio is 1:2), water-in-oil emulsifier be this disk, polyglycerol stearate, Unigly GO 102S and
Glyceryl monooleate (mass ratio 2:1:1:1).
C. it is saponified and emulsifies：70% potassium hydroxide solution 2g is slowly dropped to lutein extract under stirring
In, 90 DEG C are heated to, nitrogen is passed through, mix emulsion fluid 50g is added after 50 minutes, continues to stir 2h.
D. homogeneous：140g distilled water is added, is sufficiently mixed rear high shear homogeneous, the homogeneous under 2500r/min revolving speed
15min。
E. it is centrifuged：Solution after homogeneous is centrifuged 8min under 4500r/min revolving speed.
Plus stabilizer and antioxidant F.：The Arab that 2.0g mass fraction degree is 20% is added in upper layer after centrifugation
Glue, guar gum, carragheen and carboxymethyl cellulose mixed solution (Arabic gum, guar gum, carragheen and carboxymethyl cellulose
Mass ratio is 1:2:2:1), 0.4g ascorbic acid, 0.1g citric acid and 0.1g tea polyphenols, high shear is equal under 2000r/min revolving speed
Matter 5min obtains lutein water-soluble microemulsion.
In order to preferably verify feasibility and superiority of the invention, inventor is by lutein obtained in Examples 1 to 3
Water-soluble microemulsion has carried out Detection of Stability, and testing result is as shown in following table 1~3.
(1) gravitational stability
Lutein water-soluble microemulsion 20mL obtained in Examples 1 to 3 is separately added into three test tubes, 4000r/min
It is centrifuged 5min, as a result as shown in table 1 below.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| First week | It is whole uniformly, without sedimentation, without floating | It is whole uniformly, without sedimentation, without floating | It is whole uniformly, without sedimentation, without floating |
| Second week | It is whole uniformly, without sedimentation, without floating | It is whole uniformly, without sedimentation, without floating | It is whole uniformly, without sedimentation, without floating |
| Third week | It is whole uniformly, without sedimentation, without floating | It is whole uniformly, without sedimentation, without floating | It is whole uniformly, without sedimentation, without floating |
| 4th week | It is whole to be precipitated uniformly, on a small quantity, without floating | It is whole to be precipitated uniformly, on a small quantity, without floating | It is whole to be precipitated uniformly, on a small quantity, without floating |
(2) thermal stability
Lutein water-soluble microemulsion obtained in Examples 1 to 3 is heated into 0h, 4h, 8h, 12h at 60 DEG C, detects it
A474Absorbance, as a result as shown in table 2 below.
Table 2
| 0h | 4h | 8h | 12h | |
| Embodiment 1 | 0.679 | 0.677 | 0.678 | 0.666 |
| Embodiment 2 | 0.698 | 0.696 | 0.692 | 0.688 |
| Embodiment 3 | 0.627 | 0.625 | 0.622 | 0.618 |
(3) photostability
By lutein water-soluble microemulsion obtained in Examples 1 to 3 irradiated respectively under direct sunlight 1h, 2h, 3h,
4h, 5h detect its A474Absorbance, as a result as shown in table 3 below.
Table 3
| 1h | 2h | 3h | 4h | 5h | |
| Embodiment 1 | 0.679 | 0.675 | 0.671 | 0.668 | 0.662 |
| Embodiment 2 | 0.698 | 0.695 | 0.689 | 0.686 | 0.682 |
| Embodiment 3 | 0.627 | 0.625 | 0.621 | 0.618 | 0.612 |
It can be seen that lutein water-soluble microemulsion placement prepared by the present invention according to result in table 1~3 to be centrifuged after three weeks
Without precipitation, within 2%, direct sunlight 5h is lost within 2.5% for 60 DEG C of heating 12h losses.The microemulsion is steady in gravity
Performance is good in terms of qualitative, thermal stability and photostability, places no suspended substance for a long time, without precipitating, is suitably applied all kinds of
In food and drug.
Claims (10)
1. a kind of method for preparing lutein water-soluble microemulsion, it is characterised in that：Cream is carried out while being included in saponification
Change the common stage of reaction of reaction.
2. a kind of method for preparing lutein water-soluble microemulsion according to claim 1, it is characterised in that：It is described common
The time of the stage of reaction is 1 ~ 4 hour, and the reaction containing lutein extract is added in saponification liquor and mix emulsion fluid simultaneously or successively
In container, the time interval that saponification liquor and mix emulsion fluid are successively added was less than 1 hour.
3. a kind of method for preparing lutein water-soluble microemulsion according to claim 2, it is characterised in that：Saponification is added
The content of reaction vessel Lutein medicinal extract is 300 ~ 400g/kg before liquid and emulsion, and saponification liquor is mass fraction 60 ~ 70%
Potassium hydroxide solution, saponification liquor is added while stirring at 70 ~ 90 DEG C and is passed through inert gas.
4. a kind of method for preparing lutein water-soluble microemulsion according to claim 2, it is characterised in that：Mixing and emulsifying
Liquid is dehydrated alcohol, oil-in-water emulsifiers and water-in-oil emulsifier, dehydrated alcohol, oil-in-water emulsifiers and water-in-oil type
Emulsifier mass ratio is 5:1:0.5~1.
5. a kind of method for preparing lutein water-soluble microemulsion according to claim 4, it is characterised in that：Oil-in-water type
Emulsifier is the combination of any one or two kinds in tween and polyglycerol monooleate, and water-in-oil emulsifier is this disk, gathers
Any one or the combination of several of them in stearine, Unigly GO 102S and glyceryl monooleate.
6. a kind of method for preparing lutein water-soluble microemulsion according to claim 1, it is characterised in that：Saponification and cream
Change after the reaction was completed, carries out homogeneous, centrifugation.
7. a kind of method for preparing lutein water-soluble microemulsion according to claim 6, it is characterised in that：Turn when homogeneous
Speed is 2000 ~ 3000r/min, and homogenizing time is 10 ~ 20min.
8. utilizing a kind of method for preparing lutein water-soluble microemulsion as claimed in claim 6, it is characterised in that：Turn when centrifugation
Speed is 4000 ~ 5000r/min, and centrifugation time is 5 ~ 10min.
9. a kind of method for preparing lutein water-soluble microemulsion according to claim 6, it is characterised in that：After centrifugation
Stabilizer and antioxidant, homogeneous are added in upper layer, obtains lutein water-soluble microemulsion.
10. a kind of method for preparing lutein water-soluble microemulsion according to claim 9, it is characterised in that：Stabilizer
For any one or the combination of several of them in Arabic gum, guar gum, carragheen and carboxymethyl cellulose, antioxidant is anti-bad
Any one or the combination of several of them in hematic acid, citric acid and tea polyphenols；The mass fraction of stabilizer is 10 ~ 20%, and additional amount is
The 0.5 ~ 2% of upper liquid quality after centrifugation；The additional amount of antioxidant is 0.2 ~ 1% of upper liquid quality after being centrifuged.
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