CN103772253A - Preparation method of xanthophyll - Google Patents
Preparation method of xanthophyll Download PDFInfo
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- CN103772253A CN103772253A CN201210398106.2A CN201210398106A CN103772253A CN 103772253 A CN103772253 A CN 103772253A CN 201210398106 A CN201210398106 A CN 201210398106A CN 103772253 A CN103772253 A CN 103772253A
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- preparation
- xenthophylls
- extraction
- soxhlet
- sherwood oil
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Abstract
The invention belongs to the field of natural pigment preparation, and more specifically relates to a preparation method of xanthophylls. The invention employs dried marigold flower particles as raw materials, and the preparation method comprises the following steps: (1) placing dried marigold flower particles in an extraction tube of a Soxhlet extractor; adding petroleum ether, aqueous solution of ethanol and potassium hydroxide in an extraction flask of the Soxhlet extractor in order; carrying out extraction-saponification under the conditions of heating, stirring and light avoiding; (2) filtering the mixture in the extraction flask of the Soxhlet extractor; collecting filter residues; washing filter residues with organic solvent until the filtrate is colorless; collecting filtrate; reducing pressure and condensing; standing the concentrate at low temperature for precipitating the xanthophyll product. The invention has the advantages of simplified process, simultaneous extraction and saponification of xanthophyll ester, substantially shortened preparation time of xanthophylls, low energy consumption and little environmental pollution; the preparation method accords with environmental protection requirements and is suitable for industrial scale production.
Description
Technical field
The invention belongs to natural pigment preparation field.Be specifically related to a kind of preparation method of xenthophylls.
Background technology
Xenthophylls is a kind of natural pigment, has the feature of lovely luster, strong coloring force, safety non-toxic, antioxidant property excellence, has been widely used in the production fields such as food, makeup, tobacco, animal and fowl fodder.Scientific research in recent years report xenthophylls causes that by oxidative damage macula retinae district the danger of age related macular degeneration (AMD) is relevant with reducing, and xenthophylls effectively prevention of arterial harden, cataract, also can suppress the generation of cancer.A large amount of xenthophylls is present in vegetables, flowers, fruit and some algae bio, wherein especially the highest with content in mary bush and Flower of Aztec Marigold.Xenthophylls in plant conventionally and the lipid acid such as tetradecanoic acid, lauric acid and palmitinic acid be combined into ester derivative, but lutein ester need change into free xenthophylls can be by body metabolism, therefore the lutein ester of preparing from the biology that contains xenthophylls needs saponification, generates free xenthophylls monomer.The technical process of preparing at present xenthophylls take dried marigold flower pellets as raw material as: dried marigold flower pellets → organic solvent extraction → extracting solution concentrated → lutein ester runic thing → saponification → saponified → purifying → xenthophylls product.There is the shortcomings such as consumption of organic solvent is large, complex process, length consuming time in existing xenthophylls preparation method.
Study morely about xenthophylls preparation method, below provide part document as a reference.
United States Patent (USP) 5382714,1995-1-17
United States Patent (USP) 6380442,2002-4-30
PCT patent application IN2005000016
Chinese patent 200410082365.X
Chinese patent 200510010041.X
Chinese patent 200510028396.1
Chinese patent 200710185292.0
Chinese patent 200810054840.0
Plant?Foods?Hum?Nutr,?1997,?50:163-169
Food?Chem,?1997,?58(3):?255-258
J?Agric?Food?Chem,?2002,?50:4491-4496。
Summary of the invention
The object of the invention is to overcome original xenthophylls preparation method's defect, provide a kind of take dried marigold flower pellets as raw material, and work simplification, cost are low, meet environmental requirement and be suitable for the preparation method of the xenthophylls of commercial scale production.
To achieve these goals, the present invention, take dried marigold flower pellets as raw material, comprises the steps:
(1) dried marigold flower pellets is placed in to the extraction tube of apparatus,Soxhlet's, in the extraction flask of apparatus,Soxhlet's, adds successively sherwood oil, aqueous ethanolic solution, potassium hydroxide, under the condition of heating, stirring, lucifuge, extract-saponification;
(2) mixture in the extraction flask of filtration apparatus,Soxhlet's, collect filter residue, colourless to filtrate with organic solvent washing filter residue, collect filtrate, underpressure distillation at 30 ~ 55 ℃, 60 ~ 85% of extraction organic solvent gross weight, be under the condition of-5 ~-10 ℃ in temperature by the liquid after concentrated, leave standstill 15 ~ 20 hours, collect the solid of separating out, vacuum-drying obtains xenthophylls product.
Wherein, the sherwood oil described in step (1) is that boiling range is the sherwood oil of 30 ~ 60 ℃, 1.2 ~ 1.5 times of the extraction tube volume that the consumption of sherwood oil is apparatus,Soxhlet's; The volumetric concentration of aqueous ethanolic solution is 80 ~ 90%, 5 ~ 10 times of the extraction tube volume that the consumption of aqueous ethanolic solution is apparatus,Soxhlet's; The consumption of potassium hydroxide is 0.003 ~ 0.006 gram of/gram of dried marigold flower pellets; Heating temperature is 55 ~ 65 ℃, and be 8 ~ 12 hours heat-up time.
Wherein, the organic solvent described in step (2) is ethyl acetate, acetone or tetrahydrofuran (THF).
Advantage of the present invention is as follows:
1. the extraction of work simplification, lutein ester and the saponification of lutein ester are carried out simultaneously, greatly shortened xenthophylls preparation time, be suitable for commercial scale production.
2. sherwood oil consumption is few and save lutein ester extract enrichment step, consume energy low, environmental pollution is little, meets environmental requirement.
3. the purity to 90% of xenthophylls product.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail:
A preparation method for xenthophylls, is characterized in that: take dried marigold flower pellets as raw material, comprise the steps:
(1) dried marigold flower pellets is placed in to the extraction tube of apparatus,Soxhlet's, in the extraction flask of apparatus,Soxhlet's, adds successively sherwood oil, ethanol, potassium hydroxide, under the condition of heating, stirring, lucifuge, extract-saponification;
(2) mixture in the extraction flask of filtration apparatus,Soxhlet's, collect filter residue, colourless to filtrate with organic solvent washing filter residue, collect filtrate, underpressure distillation at 30 ~ 55 ℃, 60 ~ 85% of extraction organic solvent gross weight, be under the condition of-5 ~-10 ℃ in temperature by the liquid after concentrated, leave standstill 15 ~ 20 hours, collect the solid of separating out, vacuum-drying obtains xenthophylls product.
Wherein, the sherwood oil described in step (1) is that boiling range is the sherwood oil of 30 ~ 60 ℃, 1.2 ~ 1.5 times of the extraction tube volume that the consumption of sherwood oil is apparatus,Soxhlet's; The volumetric concentration of aqueous ethanolic solution is 80 ~ 90%, 5 ~ 10 times of the extraction tube volume that the consumption of aqueous ethanolic solution is apparatus,Soxhlet's; The consumption of potassium hydroxide is 0.003 ~ 0.006 gram of/gram of dried marigold flower pellets; Heating temperature is 55 ~ 65 ℃, and be 8 ~ 12 hours heat-up time.
Wherein, the organic solvent described in step (2) is ethyl acetate, acetone or tetrahydrofuran (THF).
example 1
100 grams of dried marigold flower pellets are placed in to the extraction tube (volume is 150 milliliters) of apparatus,Soxhlet's, in the extraction flask of apparatus,Soxhlet's, adding successively 180 milliliters of boiling ranges is the sherwood oil of 30 ~ 60 ℃, the aqueous ethanolic solution that 1500 ml volumes concentration are 80%, 0.6 gram of potassium hydroxide, is extract-saponification 12 hours under 65 ℃, the condition of stirring, lucifuge in Heating temperature; After extraction-saponification finishes, mixture in the extraction flask of filtration apparatus,Soxhlet's, collects filter residue, colourless to filtrate with ethyl acetate washing filter residue, collect filtrate, underpressure distillation at 45 ℃, 60% of extraction organic solvent gross weight, is under the condition of-5 ℃ in temperature by the liquid after concentrated, leave standstill 20 hours, the solid that collection is separated out, vacuum-drying obtains 1.1 grams of xenthophylls products, and purity is 91.7%.
example 2
100 grams of dried marigold flower pellets are placed in to the extraction tube (volume is 150 milliliters) of apparatus,Soxhlet's, in the extraction flask of apparatus,Soxhlet's, adding successively 225 milliliters of boiling ranges is the sherwood oil of 30 ~ 60 ℃, the aqueous ethanolic solution that 750 ml volumes concentration are 90%, 0.3 gram of potassium hydroxide, is extract-saponification 8 hours under 55 ℃, the condition of stirring, lucifuge in Heating temperature; After extraction-saponification finishes, mixture in the extraction flask of filtration apparatus,Soxhlet's, collects filter residue, colourless to filtrate with washing with acetone filter residue, collect filtrate, underpressure distillation at 30 ℃, 80% of extraction organic solvent gross weight, is under the condition of-7 ℃ in temperature by the liquid after concentrated, leave standstill 15 hours, the solid that collection is separated out, vacuum-drying obtains 0.9 gram of xenthophylls product, and purity is 94.1%.
example 3
1000 grams of dried marigold flower pellets are placed in to the extraction tube (volume is 1500 milliliters) of apparatus,Soxhlet's, in the extraction flask of apparatus,Soxhlet's, adding successively 2000 milliliters of boiling ranges is the sherwood oil of 30 ~ 60 ℃, the aqueous ethanolic solution that 8000 ml volumes concentration are 85%, 5 grams of potassium hydroxide, is extract-saponification 10 hours under 60 ℃, the condition of stirring, lucifuge in Heating temperature; After extraction-saponification finishes, mixture in the extraction flask of filtration apparatus,Soxhlet's, collect filter residue, colourless to filtrate with tetrahydrofuran (THF) washing filter residue, collect filtrate, underpressure distillation at 40 ℃, 85% of extraction organic solvent gross weight is, under the condition of-10 ℃, to leave standstill 20 hours in temperature by the liquid after concentrated, the solid that collection is separated out, vacuum-drying obtains 11.9 grams of xenthophylls products.
Claims (6)
1. a preparation method for xenthophylls, is characterized in that: take dried marigold flower pellets as raw material, comprise the steps:
(1) dried marigold flower pellets is placed in to the extraction tube of apparatus,Soxhlet's, in the extraction flask of apparatus,Soxhlet's, adds successively sherwood oil, aqueous ethanolic solution, potassium hydroxide, under the condition of heating, stirring, lucifuge, extract-saponification;
(2) mixture in the extraction flask of filtration apparatus,Soxhlet's, collect filter residue, colourless to filtrate with organic solvent washing filter residue, collect filtrate, underpressure distillation at 30 ~ 55 ℃, 60 ~ 85% of extraction organic solvent gross weight, be under the condition of-5 ~-10 ℃ in temperature by the liquid after concentrated, leave standstill 15 ~ 20 hours, collect the solid of separating out, vacuum-drying obtains xenthophylls product.
2. according to the preparation method of xenthophylls claimed in claim 1, it is characterized in that: the sherwood oil described in step (1) is that boiling range is the sherwood oil of 30 ~ 60 ℃ 1.2 ~ 1.5 times of the extraction tube volume that the consumption of sherwood oil is apparatus,Soxhlet's.
3. according to the preparation method of xenthophylls claimed in claim 1, it is characterized in that: the volumetric concentration of the aqueous ethanolic solution described in step (1) is 80 ~ 90% 5 ~ 10 times of the extraction tube volume that the consumption of aqueous ethanolic solution is apparatus,Soxhlet's.
4. according to the preparation method of xenthophylls claimed in claim 1, it is characterized in that: the consumption of the potassium hydroxide described in step (1) is 0.003 ~ 0.006 gram of/gram of dried marigold flower pellets.
5. according to the preparation method of xenthophylls claimed in claim 1, it is characterized in that: the Heating temperature described in step (1) is 55 ~ 65 ℃, be 8 ~ 12 hours heat-up time.
6. according to the preparation method of xenthophylls claimed in claim 1, it is characterized in that: the organic solvent described in step (2) is ethyl acetate, acetone or tetrahydrofuran (THF).
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| CN201210398106.2A CN103772253B (en) | 2012-10-19 | 2012-10-19 | A kind of preparation method of xenthophylls |
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| CN201210398106.2A CN103772253B (en) | 2012-10-19 | 2012-10-19 | A kind of preparation method of xenthophylls |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104003962A (en) * | 2014-05-16 | 2014-08-27 | 集美大学 | Preparation method and application of alga xanthophyll |
| CN105085352A (en) * | 2015-09-22 | 2015-11-25 | 哈尔滨宝德生物技术股份有限公司 | Extracting method for converting high-content xanthophylls from marigolds |
| CN105646314A (en) * | 2015-12-30 | 2016-06-08 | 中国农业科学院郑州果树研究所 | Method for one-step extraction and saponification of marigold lutein |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1120565A (en) * | 1995-07-26 | 1996-04-17 | 青岛大学科技教育开发公司食品科学研究所 | Method for extracting lutein resin edible pigment from Tagetes erecta flower |
| US5648564A (en) * | 1995-12-21 | 1997-07-15 | Kemin Industries, Inc. | Process for the formation, isolation and purification of comestible xanthophyll crystals from plants |
| CN101139312A (en) * | 2007-05-08 | 2008-03-12 | 陈吉华 | Method for preparing free lutein having high saponification ratio |
| WO2009027850A2 (en) * | 2007-06-06 | 2009-03-05 | Multi-Tech Specialty Chemicals Co., Ltd. | Process for the preparation of xanthophyll crystals |
-
2012
- 2012-10-19 CN CN201210398106.2A patent/CN103772253B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1120565A (en) * | 1995-07-26 | 1996-04-17 | 青岛大学科技教育开发公司食品科学研究所 | Method for extracting lutein resin edible pigment from Tagetes erecta flower |
| US5648564A (en) * | 1995-12-21 | 1997-07-15 | Kemin Industries, Inc. | Process for the formation, isolation and purification of comestible xanthophyll crystals from plants |
| CN101139312A (en) * | 2007-05-08 | 2008-03-12 | 陈吉华 | Method for preparing free lutein having high saponification ratio |
| WO2009027850A2 (en) * | 2007-06-06 | 2009-03-05 | Multi-Tech Specialty Chemicals Co., Ltd. | Process for the preparation of xanthophyll crystals |
Non-Patent Citations (1)
| Title |
|---|
| 张多婷 等: "万寿菊中叶黄素的提取及分离工艺", 《食品与发酵工业》, vol. 36, no. 5, 31 May 2010 (2010-05-31) * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104003962A (en) * | 2014-05-16 | 2014-08-27 | 集美大学 | Preparation method and application of alga xanthophyll |
| CN104003962B (en) * | 2014-05-16 | 2016-08-24 | 集美大学 | A kind of preparation method and its usage of fucoxanthin |
| CN105085352A (en) * | 2015-09-22 | 2015-11-25 | 哈尔滨宝德生物技术股份有限公司 | Extracting method for converting high-content xanthophylls from marigolds |
| CN105646314A (en) * | 2015-12-30 | 2016-06-08 | 中国农业科学院郑州果树研究所 | Method for one-step extraction and saponification of marigold lutein |
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Granted publication date: 20151216 Termination date: 20161019 |