CN1840686A - Process for preparing lutein fatty acid ester by enzyme degradation and solvent extraction method - Google Patents
Process for preparing lutein fatty acid ester by enzyme degradation and solvent extraction method Download PDFInfo
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- CN1840686A CN1840686A CN 200610037774 CN200610037774A CN1840686A CN 1840686 A CN1840686 A CN 1840686A CN 200610037774 CN200610037774 CN 200610037774 CN 200610037774 A CN200610037774 A CN 200610037774A CN 1840686 A CN1840686 A CN 1840686A
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- fatty acid
- acid ester
- lutein
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Abstract
The disclosed preparation method for lutein fatty acid ester comprises: adding enzyme into marigold for ensilage; heating and stirring to extract the target product with non-polar solvent, finally vacuum condensing. Unlike to prior art, this invention eliminates some procedures, needs mild condition, and improves product extraction rate. The product has wide application.
Description
One, technical field
The present invention relates to a kind of method that extracts fatty acid ester of lutein in the marigold flower, be exclusively used in and from marigold flower, prepare fatty acid ester of lutein.
Two, technical background
In recent years, along with the raising of people's living standard, people are more and more to the demand of natural active matter, about the extraction and the development and use of natural active matter seem particularly important.Xenthophylls is a kind of of carotenoid, also is one of the most effective hyperchromic additive in the carotenoid, is used for appearance luster and interior quality that animal and fowl fodder can improve animal products; Natural carotenol still is a kind of oxidation inhibitor of excellent performance, the effect of have cancellation singlet nitrogen, removing free radical, as foodstuff additive and protective foods, to preventing that human body from having good effect because of a series of diseases that organ senescence causes, as the visual deterioration that can prevent senile eyeball macula retinae to degenerate to cause with blind.
Flower of Aztec Marigold owing to its lutein content height, other carotenoid contents are few and be suitable for the big area popularizing planting becomes the desirable industrial raw material that separates xenthophylls.In marigold flower, xenthophylls mainly exists with stable fatty acid ester attitude, but not free state.The production method of general fatty acid ester of lutein adopts solvent method, method in the patent 02110437.9 of declaring as China University Of Qingdao, this method is extracted the marigold flower of harvesting after fermentation (ensiling), squeezing, drying, granulation, pulverizing with No. 6 solvent oils, extracting solution is through vacuum concentration, fills nitrogen again and removes residual solvent and get the fatty acid ester of lutein finished product.Extract fatty acid ester of lutein in this way, will be after fresh flower harvesting, ensiling, the squeezing through super-dry, granulation, disintegrating process, technological process is comparatively complicated.Experimental study shows will lose in the marigold flower 20～40% xenthophylls in the drying process, alltrans xenthophylls also has the part isomerization or generates epoxide.Simultaneously, the consumption of the conventional production methods energy consumption of fatty acid ester of lutein is more, production power is higher.
Three, summary of the invention
Technical problem the object of the present invention is to provide a kind of new method for producing of fatty acid ester of lutein, at the present production status of China's fatty acid ester of lutein, with the fresh Flos Tagetis Erectae is raw material, by adding enzyme liberating and solvent extraction bonded method in the ensilage, produce fatty acid ester of lutein, reduction technical process and power consumption.
Technical scheme
Present invention resides in the fresh Flos Tagetis Erectae ensilage and to add effectively degrading plant cell walls and be the method for raw material production fatty acid ester of lutein directly such as Carboxymethylcellulose enzyme with the back marigold flower of degrading.
Steps such as major technique technology of the present invention comprises marigold flower ensiling (interpolation enzyme), extraction, concentrate.After the fresh Flos Tagetis Erectae harvesting, spray (enzyme dosage is 0～1% of a fresh Flos Tagetis Erectae weight, with spraying after the less water dissolving again) with enzyme solution, after mixing, in 20～35 ℃ of following lucifuge ensilings 3～20 days; (non-polar solvent is 3～4 with degraded fresh Flos Tagetis Erectae ratio: 1) add non-polar solvent and extract repeatedly under condition of heating and stirring by weight proportion, the combining extraction liquid concentrating under reduced pressure, oily product inflated with nitrogen removes residual solvent and makes fatty acid ester of lutein.The enzyme that adds in the ensilage is solid-state or liquid cellulase or beta-glucanase; Can be raw material non-polar solvent extract fatty acid ester of lutein directly in the extraction with the marigold flower after the ensiling; Non-polar solvent is C
6～C
8Naphthenic hydrocarbon or ethers; Stirring velocity is 200～700rpm when wherein extracting, and extraction time is 3～4 times, and extraction time is followed successively by 3h～4h, 3h～2h, 2h～1h; Do not heat the mode (be advisable with the enzyme optimum temperature, 30～65 ℃, be preferably 50 ℃) of (room temperature) or heating when wherein extracting; Temperature is 25～45 ℃ during concentrating under reduced pressure, and vacuum tightness is 0.08～0.09MPa.
Beneficial effect method provided by the invention has following advantage:
(1) owing to the squeezing, drying, granulation, the disintegrating process step that have reduced in traditional fatty acid ester of lutein production, enzyme degradation and solvent extraction method of the present invention technical process is simple, and is convenient for production;
(2) have only ensiling, extraction, concentrated common unit operation in the enzyme degradation and solvent extraction method of the present invention, technological process is safe and reliable, obviously reduces production costs, and shortens production time and production cycle, and energy consumption is low;
(3) enzyme degradation and solvent extraction method of the present invention does not have drying process, does not have problem of oxidation in the course of processing, effectively guarantees extraction effect and quality product; Experimental study shows will lose 20～40% xenthophylls in the marigold flower drying process in the prior art, simultaneously, because thermal oxidation, alltrans xenthophylls also have the part isomery to turn to cis xenthophylls and oxidation generates epoxide, reduce xenthophylls extraction yield and quality product.
Four, embodiment
Extraction yield is the ratio of the fresh Flos Tagetis Erectae weight (g) of xenthophylls oily example weight (g) and degraded.
The content assaying method of fatty acid ester of lutein is with reference to method in the Chinese patent 02157804.4.The testing sample that precision takes by weighing about 0.1g is dissolved in normal hexane and makes 100ml solution.Use the normal hexane dilute sample, make gained solution absorbency scope between 0.3～0.7, and record the maximum absorption wavelength of above-mentioned diluting soln near 445nm with spectrophotometer.The content of fatty acid ester of lutein calculates with following formula:
Fatty acid ester of lutein percentage composition=((extent of dilution ÷ example weight) * extent of dilution) ÷ 1394 * 100
Annotate: the 1394th, the uptake factor at wavelength 445nm place
Embodiment 1 (no enzyme group)
Fresh Flos Tagetis Erectae is plucked the back 30 ℃ of following lucifuge ensilings 10 days; Get ensiling fresh Flos Tagetis Erectae 1000g, with the normal hexane is extraction agent, normal hexane joined in the extraction kettle with the degraded fresh flower in 3: 1 by weight proportion, in 50 ℃ of heating and stirring velocity is to extract repeatedly under the 400rpm condition 3 times, extraction time is followed successively by 3h, 2h, 1h, combining extraction liquid, and with extraction liquid at 40 ℃, vacuum tightness is the 0.085MPa concentrating under reduced pressure.Concentrated solution is removed residual solvent, feed nitrogen to reactor, continuously stirring vacuumizes, and makes in the fatty acid ester of lutein Determination of Residual Organic Solvents less than 100ppm.Make fatty acid ester of lutein and be scarlet, extraction yield is 1.75%, and fatty acid ester of lutein content is 9.56%.This product need be stored in the environment of low temperature, drying, lucifuge.
Embodiment 2 (adding the beta-glucanase group)
Get and pluck back fresh Flos Tagetis Erectae 1100g, liquid beta-glucanase (enzyme dosage be fresh Flos Tagetis Erectae weight 0.5%) 5.5g is dissolved in the 50ml water, is sprayed on the fresh Flos Tagetis Erectae after mixing, enzyme and fresh flower stirring thorough mixing is even, 30 ℃ of following lucifuge ensilings 10 days; Get degraded fresh Flos Tagetis Erectae 1000g, with the normal hexane is extraction agent, normal hexane joined in the extraction kettle with the degraded fresh flower in 3: 1 by weight proportion, in 50 ℃ of heating and stirring velocity is to extract repeatedly under the 400rpm condition 3 times, extraction time is followed successively by 3h, 2h, 1h, combining extraction liquid, and with extraction liquid at 40 ℃, vacuum tightness is the 0.085MPa concentrating under reduced pressure.Charge into nitrogen in the reactor concentrated solution, continuously stirring vacuumizes, and makes in the fatty acid ester of lutein Determination of Residual Organic Solvents less than 100ppm.Make fatty acid ester of lutein and be dark garnet, extraction yield is 1.82%, and fatty acid ester of lutein content is 18.52%.This product need be stored in the environment of low temperature, drying, lucifuge.
Embodiment 3 (adding the cellulase group)
Get and pluck back fresh Flos Tagetis Erectae 1100g, liquid cellulase (enzyme dosage be fresh Flos Tagetis Erectae weight 0.5%) 5.5g is dissolved in the 50ml water, is sprayed on the fresh Flos Tagetis Erectae after mixing, enzyme and fresh flower stirring thorough mixing is even, 30 ℃ of following lucifuge ensilings 10 days; Get degraded fresh Flos Tagetis Erectae 1000g, with the normal hexane is extraction agent, normal hexane joined in the extraction kettle with the degraded fresh flower in 3: 1 by weight proportion, in 50 ℃ of heating and stirring velocity is to extract repeatedly under the 400rpm condition 3 times, extraction time is followed successively by 3h, 2h, 1h, combining extraction liquid, and with extraction liquid at 40 ℃, vacuum tightness is the 0.085MPa concentrating under reduced pressure.Charge into nitrogen to the reactor concentrated solution, continuously stirring vacuumizes, and makes in the fatty acid ester of lutein Determination of Residual Organic Solvents less than 100ppm.Make fatty acid ester of lutein and be dark garnet, extraction yield is 1.80%, and fatty acid ester of lutein content is 18.38%.This product need be stored in the environment of low temperature, drying, lucifuge.
Embodiment 4 (adding the beta-glucanase group)
Get and pluck back fresh Flos Tagetis Erectae 1100g, liquid beta-glucanase (enzyme dosage be fresh Flos Tagetis Erectae weight 0.5%) 5.5g is dissolved in the 50ml water, is sprayed on the fresh Flos Tagetis Erectae after mixing, enzyme and fresh flower stirring thorough mixing is even, 30 ℃ of following lucifuge ensilings 10 days; Get ensiling fresh Flos Tagetis Erectae 1000g, with sherwood oil (30～60 ℃ of boiling ranges) is extraction agent, sherwood oil joined in the extraction kettle with the degraded fresh flower in 3: 1 by weight proportion, in 50 ℃ of heating and stirring velocity is to extract repeatedly under the 400rpm condition 3 times, extraction time is followed successively by 3h, 2h, 1h, combining extraction liquid, and with extraction liquid at 20 ℃, vacuum tightness is the 0.085MPa concentrating under reduced pressure.Concentrated solution is removed residual solvent, feed nitrogen to reactor, continuously stirring vacuumizes, and makes in the fatty acid ester of lutein Determination of Residual Organic Solvents less than 100ppm.Make fatty acid ester of lutein and be scarlet, extraction yield is 1.88%, and fatty acid ester of lutein content is 18.64%.This product need be stored in the environment of low temperature, drying, lucifuge.
According to above embodiment, adopt non-polar solvent C
6～C
8Naphthenic hydrocarbon or ethers replace above-mentioned normal hexane or sherwood oil to extract fatty acid ester of lutein the marigold flower after ensiling, are that those skilled in the art can accomplish.
Claims (10)
1. utilize enzyme liberating-solvent extration to prepare the method for fatty acid ester of lutein, it is characterized in that it comprises the following steps:
(a) fresh Flos Tagetis Erectae is plucked back sprinkling enzyme solution, and enzyme solution is solid-state or liquid cellulase or beta-glucanase, and addition is 0～1% of a fresh Flos Tagetis Erectae weight, with spraying after the water dissolution again; After mixing, carry out the lucifuge ensiling;
(b) adopt non-polar solvent C
6～C
8Naphthenic hydrocarbon or ethers extract fatty acid ester of lutein the marigold flower after ensiling, non-polar solvent is 3～4: 1 with the ratio weight ratio of degraded marigold flower;
(c) vacuum concentration reclaims non-polar solvent and gets fatty acid ester of lutein oily product.
2. the method for claim 1, wherein temperature is 20～35 ℃ in (a) ensilage, the time is 3～20 days.
3. method as claimed in claim 1 or 2, stirring velocity was 200～700rpm when wherein (b) extracted, and extraction time is 3～4 times, and extraction time is followed successively by 3h～4h, 3h～2h, 2h～1h.
4. method as claimed in claim 1 or 2, room temperature or be heated to 30～65 ℃ when wherein (b) extracts.
5. method as claimed in claim 3, room temperature or be heated to 30～65 ℃ when wherein (b) extracts.
6. method as claimed in claim 1 or 2, wherein temperature is 20～45 ℃ during (c) concentrating under reduced pressure, vacuum tightness is 0.08～0.09MPa.
7. method as claimed in claim 3, wherein temperature is 20～45 ℃ during (c) concentrating under reduced pressure, vacuum tightness is 0.08～0.09MPa.
8. method as claimed in claim 4, wherein temperature is 20～45 ℃ during (c) concentrating under reduced pressure, vacuum tightness is 0.08～0.09MPa.
9. method as claimed in claim 5, wherein temperature is 20～45 ℃ during (c) concentrating under reduced pressure, vacuum tightness is 0.08～0.09MPa.
10. method as claimed in claim 1 or 2, wherein (b) non-polar solvent C
6～C
8Naphthenic hydrocarbon or ethers refer to normal hexane or sherwood oil.
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| CN 200610037774 CN1840686A (en) | 2006-01-13 | 2006-01-13 | Process for preparing lutein fatty acid ester by enzyme degradation and solvent extraction method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101235409B (en) * | 2007-01-30 | 2011-07-20 | 北京禹光生物科学研究中心有限公司 | Preparation of crystal lutein by hydrolysis with enzyme |
| 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 |
| CN103975069A (en) * | 2011-12-05 | 2014-08-06 | 赢创工业集团股份有限公司 | Method for oxidizing alkanes using an alkb alkane 1-monooxygenase |
| CN106190555A (en) * | 2016-07-22 | 2016-12-07 | 湖北中烟工业有限责任公司 | A kind of preparation method and applications of cigarette Flos Tagetis Erectae spice |
| CN107988077A (en) * | 2017-11-17 | 2018-05-04 | 云南博浩生物科技集团股份有限公司 | A kind of fresh marigold flower cell membrane wall-breaking method |
-
2006
- 2006-01-13 CN CN 200610037774 patent/CN1840686A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101235409B (en) * | 2007-01-30 | 2011-07-20 | 北京禹光生物科学研究中心有限公司 | Preparation of crystal lutein by hydrolysis with enzyme |
| 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 |
| CN103975069A (en) * | 2011-12-05 | 2014-08-06 | 赢创工业集团股份有限公司 | Method for oxidizing alkanes using an alkb alkane 1-monooxygenase |
| CN103975069B (en) * | 2011-12-05 | 2021-09-07 | 赢创运营有限公司 | Method for oxidizing alkanes by using AlkB alkane 1-monooxygenase |
| CN106190555A (en) * | 2016-07-22 | 2016-12-07 | 湖北中烟工业有限责任公司 | A kind of preparation method and applications of cigarette Flos Tagetis Erectae spice |
| CN107988077A (en) * | 2017-11-17 | 2018-05-04 | 云南博浩生物科技集团股份有限公司 | A kind of fresh marigold flower cell membrane wall-breaking method |
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