CN1120565A - Method for extracting lutein resin edible pigment from Tagetes erecta flower - Google Patents
Method for extracting lutein resin edible pigment from Tagetes erecta flower Download PDFInfo
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- CN1120565A CN1120565A CN 95108231 CN95108231A CN1120565A CN 1120565 A CN1120565 A CN 1120565A CN 95108231 CN95108231 CN 95108231 CN 95108231 A CN95108231 A CN 95108231A CN 1120565 A CN1120565 A CN 1120565A
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- xenthophylls
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Abstract
The process for extracting lutein resin as edible pigment from marigold flower includes fermenting collected marigold flower, drying, breaking, extracting with petroleum ether and heating extracted liquid for vaporization to obtain semi-finished product, cooling the vapour to obtain regenerated petroleum ether, deodouring said semi-finished product, removing residual petroleum ether by alcohol, and partially saponifying by potassium hydroxide. Obtained product has high purity and pure and stable hue. The extracted residue is used as additive for feed.
Description
The present invention relates to a kind of method, be used for the tinting material of food, beverage, makeup from marigold flower extraction lutein resin food dye.
At present, at food, beverage, in the makeup, great majority adopt the tinting material of chemosynthesis, because the chemosynthesis pigment has certain toxicity and pays effect, therefore, the tinting material of chemosynthesis can be eliminated by pottery gradually, seek a kind of nuisanceless, useful HUMAN HEALTH is a current urgency problem to be solved, in view of this to tinting material, invented the extracting method of natural yellow pigment-lutein resin, according to the present Searches of Patent Literature, the extracting method of existing xenthophylls mostly adopts a pure alkaline process, the use of soda acid runs through whole process of production, for the corrosion of equipment, the pollution of environment, workman's protection, the safety of producing etc. all causes influence to a certain degree, existing simultaneously method is not carried out pre-treatment to raw material, and therefore, xenthophylls extraction yield and purity are obviously on the low side, cause the raw material resources waste, technology is complicated simultaneously, and the equipment input is many, the production cost height.
The objective of the invention is to overcome the shortcoming and deficiency that prior art exists, be that the raw material process is extracted the refining a kind of lutein resin food dye that extracts from marigold flower that obtains and a kind of natural phant is provided, thereby solve current food dye problem.
The objective of the invention is to realize by following technical proposal:
Extract the method for lutein resin food dye from marigold flower, it is characterized in that it is made up of a row step:
A) pluck marigold flower, carry out the lucifuge fermentation in the fermentation vat of packing into;
B) pulverize behind the drying and dehydrating then;
C) (b) comminuting matter is packed in the extractor, add the petroleum ether solvent extraction agent again, heat, stir, extract xenthophylls;
D) separate (c) material, obtain extracting solution and slag;
E) (d) isolating extracting solution heating evaporation is obtained the lutein resin work in-process, its steam is through the cooling Petroleum ether extraction agent that obtains regenerating;
F) again with the lutein resin work in-process in (e) item, under vacuum condition, in retort, stir stink, add ethanol and potassium hydroxide again and slough unrecovered oil ether, it is partly-hydrolysed that work in-process xenthophylls is carried out;
G) separate (f) material, obtain lutein resin food dye product;
H) examination and test of products packing.
Wherein lucifuge fermentation adding starter is a saleratus, its consumption is the 0.01-0.02% of marigold flower weight, fermentation time is 2-3 days, also can be not with saleratus, spontaneous fermentation, fermentation time is 3-15 days, and drying and dehydrating adopts continous way electric heater or continous way spiral rotary kiln and is aided with dry air or cryogenic vacuum continuous drying equipment; Grinding particle size is-20 orders; The processing condition of extracting xenthophylls are: Heating temperature is 40-60 ℃, and churning time is 1-2 hour; Separation and Extraction liquid adopts 120-340 purpose filter plant; The Petroleum ether extraction agent of extracting the xenthophylls adding is 3-5 a times of comminuting matter (doing) weight; The temperature of extracting solution heating evaporation is 45-70 ℃; The extracting solution evaporation also can be carried out under vacuum condition, and its vacuum tightness is 540-720mmHg, and the processing condition of lutein resin work in-process vacuum deodorization are vacuum tightness 540-720mmHg, churning time 1-2 hour, also can lead to CO
2Gas, slough unrecovered oil ether, the ethanol and the potassium hydroxide mixed solution that add, its alcohol concn is that 50% ethanol and potassium hydroxide ratio are 3: 1, add-on is the 40-60% of work in-process lutein resin weight, churning time is 1-2 hour, and adding potassium hydroxide, to make its saponification deg of half-finished saponification be that the slag of 50-70% present method can be made pig, chicken feed addictive.
Flower of Aztec Marigold is the herbaceous plant of introducing from Mexico, contains abundant xenthophylls during it is spent, and is reddish-brown through extracting the purified lutein resin, is yellow behind the dilution for many times, and normal temperature is the oily liquid state during heating down for semi-solid state.
Method of the present invention adopts the lucifuge fermentation, its objective is the xenthophylls that protection has generated, promote the conversion of xenthophylls simultaneously, realize the enrichment of xenthophylls, improve the product extraction yield and the product purity of lutein resin, the extraction of more favourable xenthophylls product makes in the residue the remaining rate of xenthophylls low, makes full use of resource; The sherwood oil that extraction agent adopts also claims solvent No. six, and it contains the normal hexane more than 70%, and polarity is very little, and lipid-soluble substance is had very big solvability, therefore to extracting xenthophylls effect is preferably arranged, and cost is low; Vacuum-evaporation and feeding CO
2Gas helps deodorization and removes residual solvent, and hydro-oxidation potash soap part work in-process can improve the stability of product.
Method of the present invention, the extraction yield of xenthophylls are 11.5%-14.5%, product purity 11-13.5%.
Owing to take technique scheme, make the technology of the present invention compared with the prior art, have following advantage and effect.
A) product have a natural plant pigment, look just, toning is stable;
B) product purity height, purposes are wide;
C) method is easy, and flow process is short, three-waste free discharge, and environmental protection condition is good.
This product shows through Qingdao Sanitation and Antiepidemie Station's detected result, meets export standard fully, and its leading indicator is:
Heavy metal content (in Pb)≤2ppm,
Molten Ji residual quantity≤25ppm,
Colour 〉=200,
Sanitary index; Bacteria content≤30/g, pathogenic bacteria: do not detect.
Embodiment 1,
With the marigold flower 110kg that plucks, pack in the fermentation vat, add yeast powder 0.01kg, under the lucifuge condition, fermented 2 days, use spiral rotary kiln drying and dehydrating then, obtain siccative 10kg, pulverize the back, pack into and seal in the extractor with domestic standard sieve sieve comminuting matter to 20 order, add sherwood oil and must carry agent 40kg, heat 40 ℃, stirred 2 hours, separate with 120 order filter plants then, obtain extracting solution 33kg, its slag is done pig, chicken feed addictive, again with the extracting solution heating evaporation, 45 ℃ of its temperature, its steam cooling sherwood oil product that obtains regenerating, the evaporation residuum is 1.45kg lutein resin work in-process, stirs 1 hour under the 720mmkg vacuum condition, sloughs stink, add 50% concentration ethanol and hydrochlorinate potassium mixed solution (by 3: 1) 0.87kg then, stirred 1 hour, and made the further stripping of its unrecovered oil ether, and make xenthophylls partly-hydrolysed, separate obtaining product at last, product purity is that 12.5% extraction yield is 14%.
Embodiment 2,
With the marigold flower 110kg that plucks, in the fermentation vat of packing into, add saleratus 0.02kg, under the lucifuge condition, fermented 3 days, use the continuous heater drying and dehydrating then, obtain siccative 10kgh, be crushed to 20 orders with pulverizer, pack in the sealing extractor, add sherwood oil 50kg, heat 50 ℃, stirred 1.5 hours, and separated with 200 order filter plants then, obtain extracting solution 43.5kg, its slag is made fodder additives, to extract and heat 60 ℃ night, be to evaporate under the 720mmHg condition in vacuum tightness, and steam obtains the sherwood oil of regenerating through cooling, the evaporation residuum is lutein resin work in-process 1.5kg, under the 640mmHg vacuum condition, stirred logical CO 1.5 hours
2The gas desolventizing is residual, and slough stink, ethanol-potassium hydroxide mixed solution (by 3: the 1) 0.75kg that adds 50% concentration then, stirred 1.5 hours, and made its unrecovered oil ether stripping, and make the method flavine partly-hydrolysed, saponification deg is 60%, separate obtaining the lutein resin product at last, product purity is 13.5%, extraction yield 14.5%.
Embodiment 3,
With the marigold flower 110kg that plucks, pack in the fermentation vat, add yeast powder 0.02kg, under the lucifuge condition, fermented 2.5 days, drying and dehydrating in the spiral rotary kiln then, obtain siccative 10kg, crush and screen, add sherwood oil 30kg in the extractor of packing into to-20 orders, be heated to 60 ℃, stirred 1 hour, and crossed filter plant with 340 purposes and separate, obtain extracting solution 24.5kg, its slag is done pig, chicken feed addictive, with 70 ℃ of evaporations of extracting solution heating, steam cooling obtains the sherwood oil of regenerating again, evaporation residuum lutein resin work in-process 1.25kg, under the 540mmkg vacuum condition, stirred 2 hours, and deviate from stink, add the ethanol and potassium hydroxide mixed solution (3: the 1) 0.5kg of 50% concentration then, make the further stripping of unrecovered oil ether, the xenthophylls work in-process are partly-hydrolysed, and saponification deg is 50%, obtains product through separation, its purity is 11.5%, extraction yield 12.5%.
Embodiment 4,
To pluck marigold flower 110kg, the fermentation vat of packing into, spontaneous fermentation is 7 days under the lucifuge condition, not with saleratus, presses the condition of embodiment 2 then and extracts the product purity 11.4% that obtains, extraction yield 12.5%
Embodiment 5,
With the marigold flower 110kg that plucks, in the fermentation vat of packing into,,, press the condition of embodiment 2 then and extract the product purity 11.5% that obtains, extraction yield 13.7% not with saleratus lucifuge condition spontaneous fermentation 15 days.
Claims (12)
1, extract the method for lutein resin food dye from marigold flower, it is characterized in that it is made up of the following step:
A) pluck marigold flower, carry out the lucifuge fermentation in the fermentation vat of packing into;
B) pulverize behind the drying and dehydrating then;
C) (b) comminuting matter is packed in the extractor, add the petroleum ether solvent extraction agent again, heat, stir, extract xenthophylls;
D) separate (c) material, obtain extracting solution and slag;
E) (d) isolating extracting solution heating evaporation is obtained the lutein resin work in-process, its steam is through the cooling Petroleum ether extraction agent that obtains regenerating;
F) again with the lutein resin work in-process in (e) item, under vacuum condition, in retort, stir stink, add ethanol and potassium hydroxide again and slough unrecovered oil ether, it is partly-hydrolysed that work in-process xenthophylls is carried out;
G) separate (f) material, obtain lutein resin food dye product;
H) examination and test of products packing.
2, method according to claim 1 is characterized in that it is saleratus that the lucifuge fermentation adds starter, and its consumption is the 0.01-0.02% of marigold flower weight, fermentation time 2-3 days.
3, method according to claim 1 is characterized in that the lucifuge fermentation is spontaneous fermentation, fermentation time 3-15 days.
4, method according to claim 1 is characterized in that drying and dehydrating adopts continous way electric heater or continous way spiral rotary kiln and is aided with dry air or cryogenic vacuum continuous drying equipment.
5, method according to claim 1 is characterized in that grinding particle size is-20 orders.
6, method according to claim 1, it is characterized in that the processing condition of extracting xenthophylls are: Heating temperature is 40-60 ℃, and churning time is 1-2 hour.
7, method according to claim 1 is characterized in that extracting Petroleum ether extraction agent that xenthophylls adds and is 3-5 times of comminuting matter (doing) weight.
8, method according to claim 1 is characterized in that separation and Extraction liquid adopts 120-340 purpose filter plant.
9, method according to claim 1, the temperature that it is characterized in that the extracting solution heating evaporation is 45-70 ℃.
10, method according to claim 1 is characterized in that extracting solution evaporation carries out under vacuum condition, its vacuum tightness is 540-720mmHg, and the processing condition of xenthophylls work in-process vacuum deodorization are: its vacuum tightness 540-720mmHg, churning time 1-2 hour.
11, method according to claim 1 is characterized in that the work in-process vacuum deodorization feeds CO
2Gas.
12, method according to claim 1 is characterized in that, sloughs ethanol and potassium hydroxide mixed solution that unrecovered oil ether adds, its alcohol concn is 50%, ethanol and potassium hydroxide ratio are 3: 1, and add-on is the 40-60% of work in-process weight, and churning time is 1-2 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95108231 CN1120565A (en) | 1995-07-26 | 1995-07-26 | Method for extracting lutein resin edible pigment from Tagetes erecta flower |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95108231 CN1120565A (en) | 1995-07-26 | 1995-07-26 | Method for extracting lutein resin edible pigment from Tagetes erecta flower |
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| CN1120565A true CN1120565A (en) | 1996-04-17 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 95108231 Pending CN1120565A (en) | 1995-07-26 | 1995-07-26 | Method for extracting lutein resin edible pigment from Tagetes erecta flower |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006114794A1 (en) * | 2005-04-25 | 2006-11-02 | Katra Phytochem Private Limited | Isolation and purification of carotenoids from marigold flowers |
| CN1297609C (en) * | 2002-02-03 | 2007-01-31 | 高宾生 | Calendula pigment extracted from marigold and its extraction process |
| CN100341989C (en) * | 2002-09-20 | 2007-10-10 | 理研维他命株式会社 | Method for purifying tagetes oil-containing resin |
| EP2008661A3 (en) * | 2007-05-03 | 2009-04-08 | Lucia Antonia Spannagel | Formulation based on marigold aloe and centellae |
| CN100490642C (en) * | 2006-05-25 | 2009-05-27 | 辽宁省农业科学院食品与加工研究所 | Fresh marigold flower lactic fermentation process |
| CN102020869A (en) * | 2010-12-08 | 2011-04-20 | 聊城大学 | Method for extracting uranidin from marigold flower |
| CN101413020B (en) * | 2007-10-17 | 2012-09-05 | 邹福林 | Novel process for extracting xanthophyll extract from Calendula officinalis |
| CN102702776A (en) * | 2012-01-19 | 2012-10-03 | 天津天康源生物技术有限公司 | Phytochrome deodorizing and refining method |
| CN101532045B (en) * | 2009-04-24 | 2013-03-27 | 西安华瑞生物工程有限公司 | Enzyme-process method for extracting lutein |
| CN103099835A (en) * | 2013-01-31 | 2013-05-15 | 邹福林 | Novel process for extracting xanthophyll extract from calendula (marigold) |
| US8481769B2 (en) | 2005-04-25 | 2013-07-09 | Katra Phytochem (India) Private Limited | Isolation and purification of cartenoids from marigold flowers |
| CN103772253A (en) * | 2012-10-19 | 2014-05-07 | 哈尔滨理工大学 | Preparation method of xanthophyll |
| 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 |
| CN110663953A (en) * | 2019-10-29 | 2020-01-10 | 内江金瑞莫生物科技有限公司 | Preparation process for polar dispersed lutein and astaxanthin obtained by utilizing lutein |
-
1995
- 1995-07-26 CN CN 95108231 patent/CN1120565A/en active Pending
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1297609C (en) * | 2002-02-03 | 2007-01-31 | 高宾生 | Calendula pigment extracted from marigold and its extraction process |
| CN100341989C (en) * | 2002-09-20 | 2007-10-10 | 理研维他命株式会社 | Method for purifying tagetes oil-containing resin |
| AU2005331246B2 (en) * | 2005-04-25 | 2011-04-21 | Katra Phytochem (India) Private Limited | Isolation and purification of carotenoids from Marigold flowers |
| US8481769B2 (en) | 2005-04-25 | 2013-07-09 | Katra Phytochem (India) Private Limited | Isolation and purification of cartenoids from marigold flowers |
| WO2006114794A1 (en) * | 2005-04-25 | 2006-11-02 | Katra Phytochem Private Limited | Isolation and purification of carotenoids from marigold flowers |
| US7622599B2 (en) | 2005-04-25 | 2009-11-24 | Katra Phytochem Private Limited | Isolation and purification of carotenoids from marigold flowers |
| CN100490642C (en) * | 2006-05-25 | 2009-05-27 | 辽宁省农业科学院食品与加工研究所 | Fresh marigold flower lactic fermentation process |
| EP2008661A3 (en) * | 2007-05-03 | 2009-04-08 | Lucia Antonia Spannagel | Formulation based on marigold aloe and centellae |
| CN101413020B (en) * | 2007-10-17 | 2012-09-05 | 邹福林 | Novel process for extracting xanthophyll extract from Calendula officinalis |
| CN101532045B (en) * | 2009-04-24 | 2013-03-27 | 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 |
| CN102702776A (en) * | 2012-01-19 | 2012-10-03 | 天津天康源生物技术有限公司 | Phytochrome deodorizing and refining method |
| CN103772253A (en) * | 2012-10-19 | 2014-05-07 | 哈尔滨理工大学 | Preparation method of xanthophyll |
| CN103772253B (en) * | 2012-10-19 | 2015-12-16 | 哈尔滨理工大学 | A kind of preparation method of xenthophylls |
| CN103099835A (en) * | 2013-01-31 | 2013-05-15 | 邹福林 | Novel process for extracting xanthophyll extract from calendula (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 |
| CN110663953A (en) * | 2019-10-29 | 2020-01-10 | 内江金瑞莫生物科技有限公司 | Preparation process for polar dispersed lutein and astaxanthin obtained by utilizing lutein |
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