CN1160418C - Supercritical carbon dioxide process for extracting lutein from marigold flower - Google Patents
Supercritical carbon dioxide process for extracting lutein from marigold flower Download PDFInfo
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- CN1160418C CN1160418C CNB021030421A CN02103042A CN1160418C CN 1160418 C CN1160418 C CN 1160418C CN B021030421 A CNB021030421 A CN B021030421A CN 02103042 A CN02103042 A CN 02103042A CN 1160418 C CN1160418 C CN 1160418C
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- marigold flower
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- xenthophylls
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The present invention relates to a method for extracting lutein from marigold flowers with supercritical carbon dioxide. Marigold fresh flowers are fermented, dried and pulverized to be used as raw material; supercritical carbon dioxide is used, ethanol is used as an entrainer, and marigold flower extractum is extracted; the marigold flower extractum is saponified with potassium hydroxide, and lutein resin of a water solubility natural edible pigment is obtained. The present invention has the advantages of simple technology, low energy consumption, environmental protection, high purity of products, good colour tone, good heat resistance, good light resistance and stable color.
Description
Technical field:
The invention belongs to a kind of method of extracting xenthophylls, relate in particular to a kind of method of producing the edible natural yellow pigment with supercritical co from marigold flower extraction xenthophylls.
Background technology:
In the tinting material that industries such as food, beverage, makeup are used, the tinting material of chemosynthesis occupies very big proportion, but because it has certain toxicity and side effect is eliminated just gradually.At present multiple nontoxic, nuisanceless, the natural colorant of useful HUMAN HEALTH is developed by people just gradually.Xenthophylls (Lutein) more and more is subject to people's attention with its lovely luster, strong coloring force, safety non-toxic, advantage such as being rich in nutrition, is widely used in various fields such as food, makeup, medicine, tobacco, bird feed.Xenthophylls mainly contains lutein and forms luteinic molecular formula: C
40H
56O
2, molecular weight is 568.85.Water insoluble, be dissolved in some organic solvent, as trichloromethane, normal hexane, sherwood oil etc.Xenthophylls is more stable under slant acidity solution, the low light level and low temperature, and unstable under the meta-alkalescence condition, under weak acid, weak base condition, it is reversible change that color takes place, next destroyed in highly basic, high light or hot conditions.Xenthophylls extensively is present in the natural pigment in vegetables, flowers, fruit and some algae bio.Xenthophylls belongs to " carotenoid " family material, is the main ingredient that constitutes plant pigmentss such as corn, vegetables, fruit, flowers.According to the study, xenthophylls content in flowers such as deep green leaf vegetables such as wild cabbage, kale, spinach and mary bush, Flower of Aztec Marigold is the highest, and especially its lutein content of marigold flower reaches 6-12g/kg.Marigold flower is planted in China on a large scale as the raw material that extracts xenthophylls, opens up the planting base of a plurality of up to ten thousand mu of scales.
From marigold flower, extract the method for xenthophylls at present, mostly adopt solvent method to extract.Its product yield is low, purity difference, peculiar smell and dissolvent residual height are arranged, and has had a strong impact on product quality, causes raw material, the wasting of resources.
Summary of the invention:
The object of the present invention is to provide a kind of nontoxic, purity is high, yield is high xenthophylls edible natural pigment.
Method provided by the invention is to be raw material with fermentation, marigold flower dry, after pulverizing, do entrainment agent with postcritical carbonic acid gas with ethanol and extract marigold flower medicinal extract, marigold flower medicinal extract is obtained the water-soluble lutein natural food colour with the potassium hydroxide saponification.Its concrete steps comprise:
(1) with the fresh Flos Tagetis Erectae of plucking, the fermenting cellar lucifuge of packing into fermentation;
(2) marigold flower that ferments is dry under the condition of temperature≤60 ℃ lucifuge;
(3) crushed after being dried is to the 10-40 order;
(4) material of the Fen Suiing extractor of packing into, feeding with ethanol from the extractor bottom is the carbon dioxide gas of entrainment agent, at 20-40MPa, under the 30-60 ℃ of condition, supercritical extraction 1-10 hour;
(5) from the effusive carbon dioxide gas in extractor top, be 30-65 ℃ in separation temperature, carry out decompression separation, obtain extracting solution;
(6) extracting solution is 45-70 ℃ in temperature, and vacuum tightness is underpressure distillation under the condition of 540-720mmHg, obtains marigold flower medicinal extract;
(7) be the 30-50wt% potassium hydroxide-ethanol solution with concentration, be 30-65 ℃ in temperature marigold flower medicinal extract carried out saponification 20-60 minute, obtain xenthophylls.
Aforesaid fermentation is spontaneous fermentation, fermentation time 3-15 days, and also can add saleratus and accelerate fermentation, its consumption is the 0.01-0.02% of marigold flower weight, fermentation time 2-3 days.
Aforesaid dry employing continous way electric heater or continous way spiral rotary kiln also is aided with dry air or cryogenic vacuum.
Aforesaid entrainment agent inlet amount is 2～8wt% of carbonic acid gas.
The present invention has following advantage:
(1) product extraction yield height; The product purity height, nontoxic, noresidue.
(2) product have color and luster just, characteristic such as stable, the pure natural of toning.
(3) technology is simple, and energy consumption is low, environmental friendliness.
Embodiment:
Embodiment 1:
(1) with the fresh Flos Tagetis Erectae of plucking, the fermenting cellar lucifuge of packing into spontaneous fermentation 12 days; With the marigold flower that ferments under the condition of temperature≤60 ℃ lucifuge with continous way spiral rotary kiln and be aided with the dry air drying; The exsiccant marigold flower is crushed to 30 orders;
(2) the marigold flower material 400g that pulverizes is packed into extractor is with the supercritical CO of purity 99%
2,, get extracting solution 79g pressure 30Mpa, 45 ℃ of extractings of temperature 5 hours;
(3) with supercritical CO
265 ℃ of temperature, vacuum tightness 540mmHg underpressure distillation 30 minutes gets marigold flower medicinal extract 32g to extracting solution with rotatory evaporator;
(4) with medicinal extract with 50% potassium hydroxide-ethanol solution 50 ℃ of saponification of temperature 50 minutes;
(5) separation obtains the water-soluble lutein natural food colour.Its purity 19%, look valency 275.
Embodiment 2:
(1) with the fresh Flos Tagetis Erectae 0.02% adding saleratus of plucking by weight, the fermenting cellar lucifuge of packing into fermentation 3 days; With the marigold flower low-temperature vacuum drying under the condition of temperature≤60 ℃ lucifuge that ferments; The exsiccant marigold flower is crushed to 30 orders;
(2) the marigold flower material 400g that pulverizes is packed into extractor is with the supercritical CO of purity 99%
2,, get extracting solution 90g pressure 32Mpa, 45 ℃ of extractings of temperature 5 hours;
(3) with supercritical CO
265 ℃ of temperature, vacuum tightness 540mmHg underpressure distillation 30 minutes gets marigold flower medicinal extract 36g to extracting solution with rotatory evaporator;
(4) with medicinal extract with 50% potassium hydroxide-ethanol solution 50 ℃ of saponification of temperature 60 minutes;
(5) separation obtains the water-soluble lutein natural food colour.Its purity 22%, look valency 321.
Embodiment 3:
(1) with the fresh Flos Tagetis Erectae of plucking, the fermenting cellar lucifuge of packing into spontaneous fermentation 12 days; With the marigold flower that ferments under the condition of temperature≤60 ℃ lucifuge with continous way spiral rotary kiln and be aided with the dry air drying; The exsiccant marigold flower is crushed to 30 orders;
(2) the marigold flower material 400g that pulverizes is packed into extractor is with the supercritical CO of purity 99%
2,, get extracting solution 80g pressure 28Mpa, 45 ℃ of extractings of temperature 5 hours;
(3) with supercritical CO
265 ℃ of temperature, vacuum tightness 540mmHg underpressure distillation 30 minutes gets marigold flower medicinal extract 30g to extracting solution with rotatory evaporator;
(4) with medicinal extract with 50% potassium hydroxide-ethanol solution 50 ℃ of saponification of temperature 50 minutes;
(5) separation obtains the water-soluble lutein natural food colour.Its purity 18%, look valency 262.
Embodiment 4:
(1) with the fresh Flos Tagetis Erectae 0.02% adding saleratus of plucking by weight, the fermenting cellar lucifuge of packing into fermentation 3 days; With the marigold flower low-temperature vacuum drying under the condition of temperature≤60 ℃ lucifuge that ferments; The exsiccant marigold flower is crushed to 30 orders;
(2) the marigold flower material 400g that pulverizes is packed into extractor is with the supercritical CO of purity 99%
2,, get extracting solution 74g pressure 26Mpa, 45 ℃ of extractings of temperature 5 hours;
(3) with supercritical CO
265 ℃ of temperature, vacuum tightness 540mmHg underpressure distillation 30 minutes gets marigold flower medicinal extract 28g to extracting solution with rotatory evaporator;
(4) with medicinal extract with 50% potassium hydroxide-ethanol solution 50 ℃ of saponification of temperature 50 minutes.
(5) separation obtains the water-soluble lutein natural food colour.Its purity 17%, look valency 212.
Claims (4)
1. one kind is extracted the method for xenthophylls with supercritical co from marigold flower, it is characterized in that the preparation method comprises the steps:
(1) with the fresh Flos Tagetis Erectae of plucking, the fermenting cellar lucifuge of packing into fermentation;
(2) marigold flower that ferments is dry under the condition of temperature≤60 ℃ lucifuge;
(3) crushed after being dried is to the 10-40 order;
(4) material of the Fen Suiing extractor of packing into, feeding with ethanol from the extractor bottom is the carbon dioxide gas of entrainment agent, at 20-40MPa, under the 30-60 ℃ of condition, supercritical extraction 1-10 hour;
(5) from the effusive carbon dioxide gas in extractor top, be 30-65 ℃ in separation temperature, carry out decompression separation, obtain extracting solution;
(6) extracting solution is 45-70 ℃ in temperature, and vacuum tightness is underpressure distillation under the condition of 540-720mmHg, obtains marigold flower medicinal extract;
(7) be the 30-50wt% potassium hydroxide-ethanol solution with concentration, be 30-65 ℃ in temperature marigold flower medicinal extract carried out saponification 20-60 minute, obtain xenthophylls.
2. a kind of method of extracting xenthophylls with supercritical co from marigold flower as claimed in claim 1, it is characterized in that described fermentation is spontaneous fermentation, fermentation time 3-15 days or adding saleratus quickening fermentation, its consumption is the 0.01-0.02% of marigold flower weight, fermentation time 2-3 days.
3. as claimed in claim 1 a kind of with the method for supercritical co from marigold flower extraction xenthophylls, it is characterized in that described dry employing continous way electric heater or continous way spiral rotary kiln and be aided with dry air or cryogenic vacuum.
4. as claimed in claim 1 a kind of with the method for supercritical co from marigold flower extraction xenthophylls, it is characterized in that described entrainment agent inlet amount is 2～8wt% of carbonic acid gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021030421A CN1160418C (en) | 2002-02-06 | 2002-02-06 | Supercritical carbon dioxide process for extracting lutein from marigold flower |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021030421A CN1160418C (en) | 2002-02-06 | 2002-02-06 | Supercritical carbon dioxide process for extracting lutein from marigold flower |
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| CN1364831A CN1364831A (en) | 2002-08-21 |
| CN1160418C true CN1160418C (en) | 2004-08-04 |
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| CNB021030421A Expired - Fee Related CN1160418C (en) | 2002-02-06 | 2002-02-06 | Supercritical carbon dioxide process for extracting lutein from marigold flower |
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Families Citing this family (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1400509B1 (en) * | 2002-09-20 | 2007-04-11 | Riken Vitamin Co., Ltd. | A method for the purification of marigold oleoresin |
| CN100429297C (en) * | 2006-01-10 | 2008-10-29 | 中国农业大学 | Marigold lutein supercritical CO2 extraction method |
| CN101693683B (en) * | 2009-09-26 | 2012-06-27 | 邯郸市中进天然色素有限公司 | Method for preparing high-purity lutein extract from common lutein extract |
| CN102010357A (en) * | 2010-10-25 | 2011-04-13 | 青岛赛特香料有限公司 | Method for refining lutein by supercritical extraction |
| JP2014529607A (en) * | 2011-08-26 | 2014-11-13 | ピーティーティー グローバル ケミカル パブリック カンパニー リミテッド | Method for extracting lutein / xanthophyll from natural substances and highly purified lutein / xanthophyll obtained by this method |
| CN103058904B (en) * | 2012-12-13 | 2016-03-30 | 大兴安岭林格贝寒带生物科技股份有限公司 | A kind of novel method of enriching and purifying Flower of Aztec Marigold Lutein |
| CN104230776A (en) * | 2013-06-09 | 2014-12-24 | 中国科学院大连化学物理研究所 | Method for preparing natural zeaxanthine by combination of enzymatic hydrolysis and supercritical extraction |
| CN103478840B (en) * | 2013-09-27 | 2015-06-10 | 滁州市滁菊研究所 | Chrysanthemum beverage |
| CN105232774A (en) * | 2015-10-28 | 2016-01-13 | 青海尤尼克生物技术有限公司 | Lycium barbarum pigment extract and preparation method thereof |
| CN105327001A (en) * | 2015-10-28 | 2016-02-17 | 青海尤尼克生物技术有限公司 | Lycium ruthenicum Murr. pigment extract and preparation method thereof |
| 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 |
| CN105754723A (en) * | 2016-05-28 | 2016-07-13 | 黄宇松 | Method for extracting chrysanthemum essential oil |
| CN106307492B (en) * | 2016-08-19 | 2019-08-30 | 华侨大学 | A kind of yeast microcapsules of lutein and preparation method thereof |
| CN106883160A (en) * | 2017-02-23 | 2017-06-23 | 童玉扁 | A kind of method that carrotene is extracted from spinach |
| CN107242565A (en) * | 2017-05-27 | 2017-10-13 | 新疆红帆生物科技有限公司 | Marigold is health food xanthophyll soft capsule of raw material and preparation method thereof |
| CN107954911A (en) * | 2017-11-23 | 2018-04-24 | 广州市辉乐医药科技有限公司 | A kind of marigold extracts lutein preparation process |
| CN109662233A (en) * | 2018-12-20 | 2019-04-23 | 株洲千金药业股份有限公司 | A kind of sweet drinking particle of brown sugar and preparation method thereof |
| CN115028613B (en) * | 2022-06-27 | 2024-03-22 | 山东天音生物科技有限公司 | Method for extracting lutein ester and quercitin from marigold flowers |
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- 2002-02-06 CN CNB021030421A patent/CN1160418C/en not_active Expired - Fee Related
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Granted publication date: 20040804 Termination date: 20170206 |