CN101020917A - Process of preparing lutein with marigold - Google Patents
Process of preparing lutein with marigold Download PDFInfo
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- CN101020917A CN101020917A CN 200710001006 CN200710001006A CN101020917A CN 101020917 A CN101020917 A CN 101020917A CN 200710001006 CN200710001006 CN 200710001006 CN 200710001006 A CN200710001006 A CN 200710001006A CN 101020917 A CN101020917 A CN 101020917A
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- xenthophylls
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Abstract
The process of preparing lutein with marigold features that marigold is leached with isopropanol in a sealed rotary leaching apparatus to obtain lutein ester, and through subsequent vacuum falling film evaporation to recover solvent and saponifying the leached lutein with composite alkali liquor in a saponifying reactor, saponified lutein is prepared. The said process has the features of reduced residue of harmful matter, reduced lutein loss, lowered production cost and low reaction temperature.
Description
Technical field:
The present invention relates to a kind of preparation method of xenthophylls, especially adopt Flower of Aztec Marigold to produce the method for xenthophylls.
Background technology:
Extracting lutein factice from marigold flower is the thing in nearly ten years as fodder additives, foodstuff additive and health care food production raw material, its development rapidly, it has progressively replaced synthetic yellow pigment with the advantage on performance and the price.Originally, people use the equipment that extracts edible oil and extract xenthophylls, extract and concentration process temperature height, make the yield of xenthophylls and quality not high.1996, begin to extract xenthophylls in China with the pot type extractor, added vacuum system in the concentration process, reduced course of processing temperature, improved the quality of product; In exhaust gas recovery system, increased freezing recovery system, reduced solvent consumption, reduced pollution environment; But its shortcoming is the pot type extractor can not realize continuous production, and industrial scale is little, realize very difficulty of mass-producing.2002, begin test and adopt the rotary extractor of small-sized continuous countercurrent, continous way running, the closed production problem of total system have been solved, and, freezing recovery system concentrated in conjunction with vacuum and low temperature, obtained certain effect, but existed industrial scale little, the xenthophylls yield is low, ton raw material consumption quantity of solvent is big, the low problem of the content of antiform lutein in the xenthophylls.
At present, extracting from marigold flower at home and abroad in the processing method of xenthophylls that great majority adopt normal hexanes again and contain normal hexane 70% is that No. 6 main solvent oils are extracting solvent, therefore, leaching back residual a large amount of benzene, phenol, alkanes substance in lutein ester, this class material is deleterious to human body, also need take measures aborning to remove, as: increase vaporizer, prolong the evaporation time discharge of being gasified, so just increased production cost, being heated for a long time to make the lutein ester rate of loss increase.
Summary of the invention:
Little in order to solve existing Xanthophyll extraction process industrial scale, the xenthophylls yield is low, the problem of residual a large amount of objectionable impuritiess, the invention provides a kind of method that adopts Flower of Aztec Marigold to produce xenthophylls, this method has reduced the residual quantity of nuisance, the xenthophylls rate of loss is reduced, have production cost, the characteristics that temperature of reaction is low of reducing.
The technical solution adopted in the present invention is:
(1) Flower of Aztec Marigold is plucked, get its flower, airtight then lucifuge fermentation, use 5 ‰ Mierocrystalline celluloses, starch, fermented 110-120 hour, leavening temperature 25-30 ℃, the chrysanthemum after the fermentation is again through super-dry, 115-125 ℃ of dry initial temperature, 60 ℃ of dry back damp-heat air temperature, dry back moisture≤12%, dried chrysanthemum are again through the granulation of ring mould granulator, particle diameter is 3-5mm, grain length 12-15mm;
(2) above-mentioned particle is put into the flat-turn leacher of airtight rotation, adopting alcohols is the interior leaching solvent of leacher, lutein ester in the leaching chrysanthemum particle, leach solvent and be 1.8-2.0: 1 with the particle weight ratio, extraction time 2-3 hour, extraction temperature 50-52 ℃, be negative pressure state in the leacher, vacuum tightness is 50-100mmHg;
(3) mixing liquid that obtains containing lutein ester after the leaching and leach solvent through the vacuum-evaporation of lifting film, will leach solvent gasification cooling and reclaim, and obtaining content is the 12-20% lutein ester;
(4) be that 50% xenthophylls drops into reactor saponification jar with weight percent, drop into 35% alkali lye, 3% ethanol then, speed with 80 commentaries on classics/min stirs, be heated to 60 ℃, reacted 5 hours, and added 2% antioxidant, 10% glycerol then, be cooled to 35 ℃ after the heating, continue to stir 100 minutes afterreactions again and finish, obtain saponification xenthophylls.
Leaching solvent in the above-mentioned said leacher can be selected Virahol for use; Antioxidant can be selected vitamin-E for use; The used alkali lye of saponification can be selected the compound alkali lye of water glass-sodium hydroxide for use.
The invention has the beneficial effects as follows: because this method adopts Virahol to extract xenthophylls, reduced the residual quantity of nuisance, do not needed gasification to discharge the hazard residue thing, then shortened the production time greatly, reduced production cost simultaneously; Adopt the compound alkali lye of water glass-sodium hydroxide that xenthophylls is carried out saponification, it is little to have the xenthophylls rate of loss, the characteristics that temperature of reaction is low.
Embodiment:
Be described further below in conjunction with embodiment, but not as a limitation of the invention.
This method invention comprises the steps: that (one) plucks Flower of Aztec Marigold, gets its flower (being called for short " chrysanthemum "), airtight then lucifuge fermentation, use 5 ‰ Mierocrystalline celluloses, starch, fermented 110-120 hour, leavening temperature 25-30 ℃, the chrysanthemum after the fermentation is again through super-dry, 115-125 ℃ of dry initial temperature, 60 ℃ of dry back damp-heat air temperature, dry back moisture≤12%, dried chrysanthemum are again through the granulation of ring mould granulator, particle diameter is 3-5mm, grain length 12-15mm;
(2) above-mentioned particle is put into the flat-turn leacher of airtight rotation, and have alcohols to leach solvent in the leacher, leach solvent and can select Virahol for use, the leaching solvent is used for leaching the lutein ester in the chrysanthemum particle, leach solvent and be 1.8-2.0 with the particle weight ratio: 1, extraction time 2-3 hour, extraction temperature 50-52 ℃, be negative pressure state in the leacher, vacuum tightness is 50-100mmHg;
(3) mixing liquid that obtains containing lutein ester after the leaching and leach solvent through the vacuum-evaporation of lifting film, will leach solvent gasification cooling and reclaim, and obtaining content is the 12-20% lutein ester;
(4) be that 50% xenthophylls drops into reactor saponification jar with weight percent, its reactor saponification jar can adopt and have liquidometer, airtight, the chuck heating, but the stainless cylinder of steel of extracting vacuum, drop into 35% alkali lye then, 3% ethanol, speed with 80 commentaries on classics/min stirs, be heated to 60 ℃, reacted 5 hours, add 2% antioxidant then, wherein antioxidant can be selected vitamin-E for use, 10% glycerol, be cooled to 35 ℃ after the heating, continue to stir 100 minutes afterreactions again and finish, obtain saponification xenthophylls, wherein, the used alkali lye of saponification can be selected the compound alkali lye of water glass-sodium hydroxide for use, its alkali lye mesosilicic acid sodium, sodium hydroxide respectively accounts for 4% of alkali lye gross weight.
Embodiment 1: with 100 tons, the marigold particles raw material of specification 3-5mm, powder content 9%, moisture content 10% extracts lutein ester by flat form circumgyrated extractor, 50 ℃ of extraction temperatures, extraction time 140 minutes.Leach the saturated liquid that the back forms, respectively through 60 order net filtrations, the vane separator separates, 180 order net filtrations, washing, three grades of precipitate and separate enter lifting film vacuum isopropanol recovering system, at first saturated solution is squeezed into pump and had vacuum pressure 0.045Mpa, 70 ℃ of vaporization temperatures, 42 ℃ of medium temperatures, the climbing-film evaporator evaporation that hot water circulation jar temperature is 80 ℃, gas phase reclaims by condensation, liquid phase enters dual evaporation, gas phase reclaims by condensation, liquid phase enters vacuum tightness 0.09Mpa, the falling liquid film rectifying tower circulation that temperature is 50 ℃ concentrates 30 minutes, and the medicinal extract after concentrating is squeezed in the saponification jar standby.When the rewinding of saponification jar starts stirring to rated value, after adding antioxidant vitamin E, mixed alkali liquor according to quantity successively, 60 ℃ of heating, Heating temperatures, 300 minutes reaction times, and then add ethanol, glycerol according to quantity, Heating temperature is reduced to 35 ℃, stirs 100 minutes afterreactions and finishes, and stockyard is gone in barrelling.This production goes out 22.15 tons of products altogether, and lutein content 75g/kg-80g/kg in the product detects the dissolvent residual 15ppm in the product according to the vegetables oil method for detecting residue in 4.8 standards among the GB/T5009.37-2003.
Embodiment 2: with 120.8 tons, the marigold particles raw material of specification 3-5mm, powder content 8%, moisture content 12% rotates leacher continuously by platform-type adverse current and extracts lutein ester, 52 ℃ of extraction temperatures, extraction time 180 minutes.Leach the saturated solution that the back forms, respectively through 60 order net filtrations, the vane separator separates, 180 order net filtrations, washing, enter lifting film vacuum solvent recovering system after three grades of precipitate and separate, at first saturated solution is squeezed into and had vacuum tightness 0.05Mpa with pump, 69 ℃ of vaporization temperatures, 40 ℃ of medium temperatures, the climbing-film evaporator evaporation that hot water circulation jar temperature is 78 ℃, gas phase reclaims by condensation, liquid phase enters the secondary climbing-film evaporation, gas phase reclaims by condensation, liquid phase enters vacuum tightness 0.092Mpa, the falling liquid film rectifying tower circulation that temperature is 49.5 ℃ concentrates 31 minutes, and it is standby that concentrated back medicinal extract is squeezed into the saponification jar.When the rewinding of saponification jar starts stirring to rated value, after adding antioxidant vitamin E, mixed alkali liquor according to quantity successively, 60 ℃ of heating, Heating temperatures, 300 minutes reaction times, and then add ethanol, glycerol according to quantity, Heating temperature is reduced to 35 ℃, stirs 100 minutes afterreactions and finishes, and stockyard is gone in barrelling.This production goes out 26.85 tons of products altogether, and lutein content 77g/kg-81g/kg in the product detects the residual 16ppm of the solvent in the product according to the vegetables oil method for detecting residue in 4.8 standards among the GB/T5009.37-2003.
Table 1 numerical value contrast table
In every effect data from table 1 as can be seen, the product that this explained hereafter goes out is better than the level of the world, domestic like product, it is big to use this technology to have industrial scale, xenthophylls yield, saponification degree height, solvent-oil ratio is little, and dissolvent residual is low, transconfiguration content height in the xenthophylls, guaranteed the quality of product, reduced cost.
Claims (4)
1, adopt Flower of Aztec Marigold to produce the method for xenthophylls, it is characterized in that: it comprises the following steps:
(1) Flower of Aztec Marigold is plucked, get its flower, airtight then lucifuge fermentation, use 5 ‰ Mierocrystalline celluloses, starch, fermented 110-120 hour, leavening temperature 25-30 ℃, the chrysanthemum after the fermentation is again through super-dry, 115-125 ℃ of dry initial temperature, 60 ℃ of dry back damp-heat air temperature, dry back moisture≤12%, dried chrysanthemum are again through the granulation of ring mould granulator, particle diameter is 3-5mm, grain length 12-15mm;
(2) above-mentioned particle is put into the flat-turn leacher of airtight rotation, adopting alcohols is the interior leaching solvent of leacher, lutein ester in the leaching chrysanthemum particle, leach solvent and be 1.8-2.0: 1 with the particle weight ratio, extraction time 2-3 hour, extraction temperature 50-52 ℃, be negative pressure state in the leacher, vacuum tightness is 50-100mmHg;
(3) mixing liquid that obtains containing lutein ester after the leaching and leach solvent through the vacuum-evaporation of lifting film, will leach solvent gasification cooling and reclaim, and obtaining content is the yellow rope ester of 12-20% leaf;
(4) be that 50% xenthophylls drops into reactor saponification jar with weight percent, drop into 35% alkali lye, 3% ethanol then, speed with 80 commentaries on classics/min stirs, be heated to 60 ℃, reacted 5 hours, and added 2% antioxidant, 10% glycerol then, be cooled to 35 ℃ after the heating, continue to stir 100 minutes afterreactions again and finish, obtain saponification xenthophylls.
2, employing Flower of Aztec Marigold according to claim 1 is produced the method for xenthophylls, and it is characterized in that: the leaching solvent in the leacher can be selected Virahol for use.
3, employing Flower of Aztec Marigold according to claim 1 is produced the method for xenthophylls, and it is characterized in that: antioxidant can be selected vitamin-E for use.
4, employing Flower of Aztec Marigold according to claim 1 is produced the method for xenthophylls, and it is characterized in that: the used alkali lye of saponification can be selected the compound alkali lye of water glass-sodium hydroxide for use.
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| CN 200710001006 CN101020917A (en) | 2007-01-19 | 2007-01-19 | Process of preparing lutein with marigold |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101532045A (en) * | 2009-04-24 | 2009-09-16 | 西安华瑞生物工程有限公司 | Enzyme-process method for extracting lutein |
| CN102020869A (en) * | 2010-12-08 | 2011-04-20 | 聊城大学 | Method for extracting uranidin from marigold flower |
| CN102090511A (en) * | 2011-01-07 | 2011-06-15 | 福州金佰慧生物技术有限公司 | Feed additive containing natural lutein and preparation method thereof |
| CN101514177B (en) * | 2009-03-13 | 2013-04-03 | 湖北丽生堂生物科技有限公司 | Method for extracting lutein from marigold particles |
| CN103304463A (en) * | 2013-06-18 | 2013-09-18 | 哈尔滨宝德生物技术开发有限公司 | Method for preparing lutein from marigold particles |
| CN103588691A (en) * | 2013-11-28 | 2014-02-19 | 刘同宽 | Lutein extraction and treatment process |
| CN103626686A (en) * | 2013-12-09 | 2014-03-12 | 新疆特瑞生物科技有限公司 | Method for extracting lutein ester from marigold |
| 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 |
| 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 |
| CN109400512A (en) * | 2018-11-15 | 2019-03-01 | 北京联合大学 | It is a kind of for improving the fresh marigold flower inorganic agent of carotenoid extraction efficiency |
| CN114957071A (en) * | 2021-02-25 | 2022-08-30 | 内蒙古昶辉生物科技股份有限公司 | Method for preparing lutein by marigold ointment |
| CN114957073A (en) * | 2021-02-25 | 2022-08-30 | 内蒙古昶辉生物科技股份有限公司 | Method for preparing lutein ester from marigold ointment and lutein ester |
-
2007
- 2007-01-19 CN CN 200710001006 patent/CN101020917A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101514177B (en) * | 2009-03-13 | 2013-04-03 | 湖北丽生堂生物科技有限公司 | Method for extracting lutein from marigold particles |
| CN101532045A (en) * | 2009-04-24 | 2009-09-16 | 西安华瑞生物工程有限公司 | Enzyme-process method for extracting lutein |
| CN102020869A (en) * | 2010-12-08 | 2011-04-20 | 聊城大学 | Method for extracting uranidin from marigold flower |
| CN102020869B (en) * | 2010-12-08 | 2013-12-25 | 聊城大学 | Method for extracting uranidin from marigold flower |
| CN102090511A (en) * | 2011-01-07 | 2011-06-15 | 福州金佰慧生物技术有限公司 | Feed additive containing natural lutein and preparation method thereof |
| CN103304463A (en) * | 2013-06-18 | 2013-09-18 | 哈尔滨宝德生物技术开发有限公司 | Method for preparing lutein from marigold particles |
| CN103588691A (en) * | 2013-11-28 | 2014-02-19 | 刘同宽 | Lutein extraction and treatment process |
| CN103588691B (en) * | 2013-11-28 | 2015-07-15 | 刘同宽 | Lutein extraction and treatment process |
| CN103626686A (en) * | 2013-12-09 | 2014-03-12 | 新疆特瑞生物科技有限公司 | Method for extracting lutein ester from marigold |
| 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 |
| 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 |
| CN109400512A (en) * | 2018-11-15 | 2019-03-01 | 北京联合大学 | It is a kind of for improving the fresh marigold flower inorganic agent of carotenoid extraction efficiency |
| CN109400512B (en) * | 2018-11-15 | 2021-05-25 | 北京联合大学 | Tagetes fresh flower treating agent for improving carotenoid extraction efficiency |
| CN114957071A (en) * | 2021-02-25 | 2022-08-30 | 内蒙古昶辉生物科技股份有限公司 | Method for preparing lutein by marigold ointment |
| CN114957073A (en) * | 2021-02-25 | 2022-08-30 | 内蒙古昶辉生物科技股份有限公司 | Method for preparing lutein ester from marigold ointment and lutein ester |
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Open date: 20070822 |