CN102040548A - Method for extracting beta-carotene and zeaxanthin from Chinese wolfberry skin - Google Patents
Method for extracting beta-carotene and zeaxanthin from Chinese wolfberry skin Download PDFInfo
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- CN102040548A CN102040548A CN2010105737745A CN201010573774A CN102040548A CN 102040548 A CN102040548 A CN 102040548A CN 2010105737745 A CN2010105737745 A CN 2010105737745A CN 201010573774 A CN201010573774 A CN 201010573774A CN 102040548 A CN102040548 A CN 102040548A
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- elutriant
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- zeaxanthin
- chinese wolfberry
- sherwood oil
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- 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 title claims abstract description 25
- 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 title claims abstract description 25
- 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 title claims abstract description 25
- 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 title claims abstract description 25
- 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 25
- 235000010930 zeaxanthin Nutrition 0.000 title claims abstract description 25
- 239000001775 zeaxanthin Substances 0.000 title claims abstract description 25
- 229940043269 zeaxanthin Drugs 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 17
- 235000015468 Lycium chinense Nutrition 0.000 title abstract description 9
- 244000241872 Lycium chinense Species 0.000 title abstract description 8
- OENHQHLEOONYIE-UKMVMLAPSA-N all-trans beta-carotene Natural products CC=1CCCC(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)CCCC1(C)C OENHQHLEOONYIE-UKMVMLAPSA-N 0.000 title abstract 3
- 235000013734 beta-carotene Nutrition 0.000 title abstract 3
- 239000011648 beta-carotene Substances 0.000 title abstract 3
- TUPZEYHYWIEDIH-WAIFQNFQSA-N beta-carotene 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=CC2=CCCCC2(C)C TUPZEYHYWIEDIH-WAIFQNFQSA-N 0.000 title abstract 3
- 229960002747 betacarotene Drugs 0.000 title abstract 3
- OENHQHLEOONYIE-JLTXGRSLSA-N β-Carotene Chemical compound CC=1CCCC(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\C1=C(C)CCCC1(C)C OENHQHLEOONYIE-JLTXGRSLSA-N 0.000 title abstract 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 239000012046 mixed solvent Substances 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000007127 saponification reaction Methods 0.000 claims abstract description 15
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 13
- 238000000605 extraction Methods 0.000 claims abstract description 10
- 239000000344 soap Substances 0.000 claims abstract description 9
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 7
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 7
- 235000006708 antioxidants Nutrition 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000284 extract Substances 0.000 claims description 52
- 239000007788 liquid Substances 0.000 claims description 30
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- 244000241838 Lycium barbarum Species 0.000 claims description 21
- 235000015459 Lycium barbarum Nutrition 0.000 claims description 21
- 239000002893 slag Substances 0.000 claims description 17
- KIDXYAWWICJAFK-UHFFFAOYSA-N O.[Na].OC Chemical compound O.[Na].OC KIDXYAWWICJAFK-UHFFFAOYSA-N 0.000 claims description 12
- 238000001514 detection method Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 8
- 239000007791 liquid phase Substances 0.000 claims description 7
- 238000001179 sorption measurement Methods 0.000 claims description 7
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 6
- 230000006837 decompression Effects 0.000 claims description 6
- 238000010828 elution Methods 0.000 claims description 6
- 239000000395 magnesium oxide Substances 0.000 claims description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 6
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N methyl alcohol Substances OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000012071 phase Substances 0.000 claims description 6
- 238000010298 pulverizing process Methods 0.000 claims description 6
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- 230000003260 anti-sepsis Effects 0.000 claims description 4
- 235000011389 fruit/vegetable juice Nutrition 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000003480 eluent Substances 0.000 abstract 2
- 239000003208 petroleum Substances 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- GRONZTPUWOOUFQ-UHFFFAOYSA-M sodium;methanol;hydroxide Chemical compound [OH-].[Na+].OC GRONZTPUWOOUFQ-UHFFFAOYSA-M 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000002699 waste material Substances 0.000 abstract 1
- 235000021466 carotenoid Nutrition 0.000 description 4
- 150000001747 carotenoids Chemical class 0.000 description 4
- 239000000049 pigment Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 2
- 201000001320 Atherosclerosis Diseases 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 241001464837 Viridiplantae Species 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000000989 food dye Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- -1 β-Hu Luobusu Chemical class 0.000 description 1
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- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for extracting beta-carotene and zeaxanthin from Chinese wolfberry skin. The method comprises the following steps: (1) extraction: drying and crashing Chinese wolfberry skin, adding mixed solvent, adding antioxidant, stirring, extracting and performing vacuum concentration on extracting solution under reduced pressure to obtain extractum; (2) saponification: adding petroleum ether to dissolve, adding sodium hydroxide-methanol solution, performing cold process for soap, layering with a separatory funnel and washing ether layer with water to remove sodium hydroxide; (3) purification; and (4) adopting high performance liquid chromatography for treatment, and drying the collected eluent 1 and eluent 2 respectively under reduced pressure to obtain extractum. In the invention, the waste Chinese wolfberry skin generated in the production processes of Chinese Wolfberry juice and Chinese Wolfberry wine can be fully used as the raw material, thus the pollution to the environment can be reduced; and the purity of beta-carotene is up to 10% and the purity of zeaxanthin is up to 65%.
Description
Technical field
The invention belongs to the extracting method of β-Hu Luobusu, zeaxanthin, particularly relate to a kind of method of from matrimony vine skin slag, extracting β-Hu Luobusu, zeaxanthin.
Background technology
β-Hu Luobusu, zeaxanthin belong to poly-penta 2 hydrocarbon compounds, belong to carotenoids, and modern pharmacology research thinks that carotenoid has the enhancing immunity function, prevents atherosclerosis and anticancer, the anti-ageing effect of waiting for a long time.
Structural formula is as follows
Structural formula one is that zeaxanthin, structural formula two are β-Hu Luobusu
Structural formula one
Structural formula two
In foodstuffs industry fast development, today with rapid changepl. never-ending changes and improvements, people have proposed new standard to the requirement of food dye.Though synthetic colour is bright in colour, good stability is cheap, because of synthetic toxicity problem, people is worried and fear; Meanwhile, natural green plant pigments safety non-toxic, and its distinctive nutritive value and physiologically active, be loved by the people, pigment in the matrimony vine is rich in abundant carotenoid, and therefore, wolfberry pigment is all having bright development prospect aspect foodstuffs industry and the medicines and health protection.
Matrimony vine juice and Lycium chinense wine are to be the product of raw material production with matrimony vine, in the process of producing these products, produce a large amount of byproduct residue---matrimony vine skin slag, abandoning these byproducts can pollute environment.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, a kind of method of extracting β-Hu Luobusu, zeaxanthin from matrimony vine skin slag is provided.
Technical scheme of the present invention is summarized as follows:
From matrimony vine skin slag, extract the method for β-Hu Luobusu, zeaxanthin, comprise the steps:
(1) extracts: matrimony vine skin slag drying, pulverizing, with the feed liquid mass ratio is that 1: 15~20 ratio adds mixed solvent and gets mixing liquid, the antioxidant 2 that adds mixing liquid quality 0.1%~0.3%, the anti-sepsis acid of 6-ditertbutylparacresol or 0.3%-0.5%, stirred 1~2 hour, extract twice, united extraction liquid is condensed into medicinal extract with described extracting solution vacuum decompression; Described mixed solvent is that volume ratio is 1: 1~4 hexanaphthene and acetone;
(2) saponification: in described medicinal extract, add sherwood oil, the mass ratio of described medicinal extract and sherwood oil is 1: 1~4, medicinal extract is all dissolved, add mass percent again and be 15%~40% sodium hydrate methanol solution, the mass ratio of described medicinal extract and described sodium hydrate methanol solution 1: 2~5 is placed on the cold soap of shady place 10~24 hours, the separating funnel layering, the ether layer washes with water, removes sodium hydroxide;
(3) purifying: magnesium oxide post on the ether layer after the saponification is carried out liquid phase adsorption separation, is that 1~4: 1 the sherwood oil and the mixed solvent of acetone carry out gradient elution with sherwood oil, volume ratio, elutriant 1 and elutriant 2;
(4) high performance liquid chromatography: chromatographic condition is C18 chromatographic column: 250mm * 4.6mm; Moving phase: acetonitrile-methyl alcohol 85: 15~80: 20; Flow velocity is 0.7~1.0ml/min; The detection wavelength is λ=450nm; Sample size is that 20 μ l column temperatures are 25 ℃; Measuring elutriant 1 through the HPLC Liquid Detection is that β-Hu Luobusu elutriant 2 is zeaxanthin, elutriant 1 and the elutriant of collecting 2 is carried out drying under reduced pressure respectively to medicinal extract, again oven dry.
Advantage of the present invention is:
It is raw material that the present invention can make full use of the depleted matrimony vine skin slag that produces in matrimony vine juice and the Lycium chinense wine production process, reduces its pollution to environment, and the β-Hu Luobusu purity of utilizing method of the present invention to extract can reach 10%, zeaxanthin purity can reach 65%.Carotenoid such as β-Hu Luobusu, zeaxanthin need be finished extraction separation in the short period of time to light, heat and air-sensitive, method of the present invention is extracted fast, has improved the extraction yield of β-Hu Luobusu, zeaxanthin.The elutriant 1 collected and elutriant 2 are carried out with drying under reduced pressure to medicinal extract, and oven dry promptly gets product
Embodiment:
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1
From matrimony vine skin slag, extract the method for β-Hu Luobusu, zeaxanthin, comprise the steps:
(1) with matrimony vine skin slag drying, pulverizing, with the feed liquid mass ratio is that 1: 18 ratio adds mixed solvent and gets mixing liquid, the antioxidant 2 that adds mixing liquid quality 0.1%, the 6-ditertbutylparacresol, stirred 1 hour, extract twice, united extraction liquid is condensed into medicinal extract with the extracting solution vacuum decompression; Mixed solvent is that volume ratio is 1: 2 hexanaphthene and an acetone;
(2) saponification: in medicinal extract, add sherwood oil, the mass ratio of medicinal extract and sherwood oil is 1: 2, medicinal extract is all dissolved, add mass percent again and be 20% sodium hydrate methanol solution, the mass ratio of medicinal extract and sodium hydrate methanol solution 1: 3 is placed on the cold soap of shady place 15 hours, the separating funnel layering, the ether layer washes with water, removes sodium hydroxide;
(3) purifying: magnesium oxide post on the ether layer after the saponification is carried out liquid phase adsorption separation, with sherwood oil, volume ratio be 1: 1,2: 1,3: 1,4: 1, sherwood oil and the mixed solvent of acetone carry out gradient elution, elutriant 1 and elutriant 2;
(4) high performance liquid chromatography: chromatographic condition is C18 chromatographic column: 250mm * 4.6mm; Moving phase: acetonitrile-methyl alcohol 85: 15; Flow velocity is 1.0ml/min; The detection wavelength is λ=450nm; Sample size is that 20 μ l column temperatures are 25 ℃; Measuring elutriant 1 through the HPLC Liquid Detection is that β-Hu Luobusu elutriant 2 is zeaxanthin, elutriant 1 and the elutriant of collecting 2 is carried out drying under reduced pressure respectively to medicinal extract, again oven dry.
Embodiment 2
From matrimony vine skin slag, extract the method for β-Hu Luobusu, zeaxanthin, comprise the steps:
(1) with matrimony vine skin slag drying, pulverizing, be that 1: 15 ratio adds mixed solvent and gets mixing liquid with the feed liquid mass ratio, add the anti-sepsis acid of antioxidant of mixing liquid quality 0.5%, stirred 2 hours, extract twice, united extraction liquid is condensed into medicinal extract with the extracting solution vacuum decompression; Mixed solvent is that volume ratio is 1: 3 hexanaphthene and an acetone;
(2) saponification: in medicinal extract, add sherwood oil, the mass ratio of medicinal extract and sherwood oil is 1: 3, medicinal extract is all dissolved, add mass percent again and be 30% sodium hydrate methanol solution, the mass ratio of medicinal extract and sodium hydrate methanol solution 1: 4 is placed on the cold soap of shady place 18 hours, the separating funnel layering, the ether layer washes with water, removes sodium hydroxide;
(3) purifying: magnesium oxide post on the ether layer after the saponification is carried out liquid phase adsorption separation, with sherwood oil, volume ratio be 1: 1,2: 1,3: 1,4: 1, sherwood oil and the mixed solvent of acetone carry out gradient elution, elutriant 1 and elutriant 2;
(4) high performance liquid chromatography: chromatographic condition is C18 chromatographic column: 250mm * 4.6mm; Moving phase: acetonitrile-methyl alcohol 80: 20; Flow velocity is 1.0ml/min; The detection wavelength is λ=450nm; Sample size is that 20 μ l column temperatures are 25 ℃; Measuring elutriant 1 through the HPLC Liquid Detection is that β-Hu Luobusu elutriant 2 is zeaxanthin, elutriant 1 and the elutriant of collecting 2 is carried out drying under reduced pressure respectively to medicinal extract, again oven dry.
Embodiment 3
From matrimony vine skin slag, extract the method for β-Hu Luobusu, zeaxanthin, comprise the steps:
(1) with matrimony vine skin slag drying, pulverizing, with the feed liquid mass ratio is that 1: 20 ratio adds mixed solvent and gets mixing liquid, the antioxidant 2 that adds mixing liquid quality 0.3%, the 6-ditertbutylparacresol, stirred 1 hour, extract twice, united extraction liquid is condensed into medicinal extract with the extracting solution vacuum decompression; Mixed solvent is that volume ratio is 1: 1 hexanaphthene and an acetone;
(2) saponification: in medicinal extract, add sherwood oil, the mass ratio of medicinal extract and sherwood oil is 1: 1, medicinal extract is all dissolved, add mass percent again and be 15% sodium hydrate methanol solution, the mass ratio of medicinal extract and sodium hydrate methanol solution 1: 5 is placed on the cold soap of shady place 10 hours, the separating funnel layering, the ether layer washes with water, removes sodium hydroxide;
(3) purifying: magnesium oxide post on the ether layer after the saponification is carried out liquid phase adsorption separation, with sherwood oil, volume ratio be 1: 1,2: 1,3: 1,4: 1, sherwood oil and the mixed solvent of acetone carry out gradient elution, elutriant 1 and elutriant 2;
(4) high performance liquid chromatography: chromatographic condition is C18 chromatographic column: 250mm * 4.6mm; Moving phase: acetonitrile-methyl alcohol 85: 15; Flow velocity is 0.8ml/min; The detection wavelength is λ=450nm; Sample size is that 20 μ l column temperatures are 25 ℃; Measuring elutriant 1 through the HPLC Liquid Detection is that β-Hu Luobusu elutriant 2 is zeaxanthin, elutriant 1 and the elutriant of collecting 2 is carried out drying under reduced pressure respectively to medicinal extract, again oven dry.
Embodiment 4
From matrimony vine skin slag, extract the method for β-Hu Luobusu, zeaxanthin, comprise the steps:
(1) with matrimony vine skin slag drying, pulverizing, be that 1: 19 ratio adds mixed solvent and gets mixing liquid with the feed liquid mass ratio, add the anti-sepsis acid of antioxidant of mixing liquid quality 0.3%, stirred 2 hours, extract twice, united extraction liquid is condensed into medicinal extract with the extracting solution vacuum decompression; Mixed solvent is that volume ratio is 1: 4 hexanaphthene and an acetone;
(2) saponification: in medicinal extract, add sherwood oil, the mass ratio of medicinal extract and sherwood oil is 1: 4, medicinal extract is all dissolved, add mass percent again and be 40% sodium hydrate methanol solution, the mass ratio of medicinal extract and sodium hydrate methanol solution 1: 2 is placed on the cold soap of shady place 24 hours, the separating funnel layering, the ether layer washes with water, removes sodium hydroxide;
(3) purifying: magnesium oxide post on the ether layer after the saponification is carried out liquid phase adsorption separation, with sherwood oil, volume ratio be 1: 1,2: 1,3: 1,4: 1, sherwood oil and the mixed solvent of acetone carry out gradient elution, elutriant 1 and elutriant 2;
(4) high performance liquid chromatography: chromatographic condition is C18 chromatographic column: 250mm * 4.6mm; Moving phase: acetonitrile-methyl alcohol 80: 20; Flow velocity is 0.9ml/min; The detection wavelength is λ=450nm; Sample size is that 20 μ l column temperatures are 25 ℃; Measuring elutriant 1 through the HPLC Liquid Detection is that β-Hu Luobusu elutriant 2 is zeaxanthin, elutriant 1 and the elutriant of collecting 2 is carried out drying under reduced pressure respectively to medicinal extract, again oven dry.
Embodiment 5
Step (2) saponification as different from Example 1: employing be not cold soap, but hot soap is 85 ℃ of water-baths heating 35min in temperature, other step and parameter are with embodiment 1.
Embodiment 6:
As different from Example 1 at step (3) purifying: silicagel column carries out liquid phase adsorption separation on the ether layer after the saponification, and other steps and parameter are with embodiment 1.
By comparing embodiment 1,2,3,4,5,6, four embodiment in front, effect is better, and extraction yield is big.β-Hu Luobusu purity can reach more than 10%, zeaxanthin purity can reach 65 above %.。
Claims (1)
1. from matrimony vine skin slag, extract the method for β-Hu Luobusu, zeaxanthin, it is characterized in that comprising the steps:
(1) extracts: matrimony vine skin slag drying, pulverizing, with the feed liquid mass ratio is that 1: 15~20 ratio adds mixed solvent and gets mixing liquid, the antioxidant 2 that adds mixing liquid quality 0.1%~0.3%, the anti-sepsis acid of 6-ditertbutylparacresol or 0.3%-0.5%, stirred 1~2 hour, extract twice, united extraction liquid is condensed into medicinal extract with described extracting solution vacuum decompression; Described mixed solvent is that volume ratio is 1: 1~4 hexanaphthene and acetone;
(2) saponification: in described medicinal extract, add sherwood oil, the mass ratio of described medicinal extract and sherwood oil is 1: 1~4, medicinal extract is all dissolved, add mass percent again and be 15%~40% sodium hydrate methanol solution, the mass ratio of described medicinal extract and described sodium hydrate methanol solution 1: 2~5 is placed on the cold soap of shady place 10~24 hours, the separating funnel layering, the ether layer washes with water, removes sodium hydroxide;
(3) purifying: magnesium oxide post on the ether layer after the saponification is carried out liquid phase adsorption separation, is that 1~4: 1 the sherwood oil and the mixed solvent of acetone carry out gradient elution with sherwood oil, volume ratio, elutriant 1 and elutriant 2;
(4) high performance liquid chromatography: chromatographic condition is C18 chromatographic column: 250mm * 4.6mm; Moving phase: acetonitrile-methyl alcohol 85: 15~80: 20; Flow velocity is 0.7~1.0ml/min; The detection wavelength is λ=450nm; Sample size is that 20 μ l column temperatures are 25 ℃; Measuring elutriant 1 through the HPLC Liquid Detection is that β-Hu Luobusu elutriant 2 is zeaxanthin, and elutriant 1 and the elutriant of collecting 2 carried out drying under reduced pressure respectively to medicinal extract.
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Cited By (9)
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CN102288716A (en) * | 2011-05-12 | 2011-12-21 | 云南农业大学 | Method for testing residual canthaxanthin in animal body |
CN102886153A (en) * | 2012-10-24 | 2013-01-23 | 周学义 | Method for extracting eyesight improving functional components in Chinese wolfberries and dregs thereof |
CN103130698A (en) * | 2011-12-01 | 2013-06-05 | 周学义 | Method extracting maize yellow from medlar and medlar dregs |
CN103149165A (en) * | 2013-01-28 | 2013-06-12 | 西北农林科技大学 | Orange cabbage carotenoid extracting and measuring method |
WO2013123618A1 (en) * | 2012-02-22 | 2013-08-29 | Dsm Ip Assets B.V. | Process for manufacture of extract containing zeaxanthin and/or its esters |
CN103504435A (en) * | 2013-10-13 | 2014-01-15 | 全亚平 | Zeaxanthin-rich eyesight-improving wolfberry beverage and production method thereof |
CN104803901A (en) * | 2014-01-27 | 2015-07-29 | 中国科学院大连化学物理研究所 | Method for preparing zeaxanthin through in situ enrichment |
CN106093264A (en) * | 2016-07-20 | 2016-11-09 | 福建省农业科学院作物研究所 | A kind of assay method of Fructus Fragariae Ananssae Xanthophyll Cycle Components |
CN107141841A (en) * | 2017-07-04 | 2017-09-08 | 江苏食品药品职业技术学院 | A kind of wolfberry pigment product and preparation method thereof |
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