CN103636919A - Method for preparing textural phosphatide and phosphatidylcholine - Google Patents
Method for preparing textural phosphatide and phosphatidylcholine Download PDFInfo
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- CN103636919A CN103636919A CN201310602796.3A CN201310602796A CN103636919A CN 103636919 A CN103636919 A CN 103636919A CN 201310602796 A CN201310602796 A CN 201310602796A CN 103636919 A CN103636919 A CN 103636919A
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Abstract
The invention discloses a method for preparing textural phosphatide and phosphatidylcholine. The method comprises the following steps: mixing condensed phosphatide with unsaturated grease, then adding lipase to catalyze the phosphatide to carry out ester exchange reactions; inactivating the lipase after the reactions, removing the free aliphatic acid, condensing, drying so as to obtain powdered textural phosphatide crude product; subjecting the powdered textural phosphatide crude product to processes of extracting, decoloring, and condensing so as to obtain textural phosphatidylcholine paste, and freeze-drying so as to obtain powdered textural phosphatide finished product B. In the structure of the textural phosphatidylcholines prepared by the method, the saturated aliphatic acids in the 1st and 3rd positions of the phosphatide carry out ester exchange reactions at the same time, the saturated aliphatic acids are all replaced by unsaturated aliphatic acids; so the product is rich in nutrients and healthier for human body; moreover the reaction conditions are mild, so that the structure of finished product will not be destroyed, and the unsaturated bonds in the unsaturated aliphatic acids are well protected.
Description
Technical field
The present invention relates to a kind of method of producing matter structure helping digestion product, particularly a kind of method of producing matter structure phosphatide and lecithin.
Background technology
Phosphatide is the basic substance of the activity of sustaining life, and to activating cell, maintains metabolism, basic metabolism and hormonal balanced secretion, and immunity and the regeneration power of enhancing human body, can bring into play great effect.But 1,3 link of phosphatide is saturated fatty acid, and take in for a long time too much saturated fatty acid, can improve LDL-C content harmful in blood, and human body health is threatened.
Unrighted acid belongs to needed by human but can not self synthetic aliphatic acid, can keep the relative mobility of cell membrane, to guarantee the normal physiological function of cell; Can make cholesterol esterification, reduce Blood Cholesterol and content of triglyceride, reduce blood viscosity, this kind blood microcirculation; Improve the activity of brain cell, strengthen memory and thinking ability.
By using ester exchange, use unrighted acid by being linked at phosphatidase 11, the saturated fatty acid of 3 is replaced, realize the matter structure of phosphatide, can obtain multiple brand-new matter structure phosphatide and lecithin, the advantage of comprehensive two kinds of important nutrient, meets human body and is specially adapted to the demand that the elderly, pregnant woman, children must nutriments to these.
Conventionally adopt now chemical method to carry out ester exchange, obtain phosphatide and/or the unrighted acid of matter structure.Use chemical method, most 1 or 3 of only can occur in phosphatide of ester exchange substitution reaction, exchange rate is low, the product of producing, impurity is many, poor effect; Residual chemical substance in product, may have potential harm to human body.
Summary of the invention
The object of the present invention is to provide a kind of method of producing matter structure phosphatide and lecithin.
The technical solution used in the present invention is:
A method of producing matter structure phosphatide and lecithin, comprises the following steps;
1) by concentrated phosphatide or concentrated phosphatide and consaturated oil mixing, add lipase-catalyzed phosphatide ester exchange reaction;
2) after reaction finishes, by lipase deactivation, remove free fatty, concentrated, dryly obtain Powdered matter structure phosphatide crude product A;
3) powder matter structure phosphatide crude product A further extracted, decolour, concentratedly obtain paste matter structure lecithin, after freeze drying, obtain Powdered matter structure lecithin finished product B.
The invention has the beneficial effects as follows: the inventive method is prepared rhythm matter structure phosphatide, there is ester exchange in the saturated fatty acid on phosphatidase 11,3, all by unrighted acid, substituted simultaneously, nutritious, more healthy for human body; Reaction condition is gentle, can not destroy the structure of finished product, particularly can well protect the unsaturated bond in unrighted acid.
The specific embodiment
Below in conjunction with example, further illustrate the present invention.
Embodiment 1
1) first crude oil of soybean is filtered, then carry out hydration degum, collect jelly to stainless cylinder of steel, ratio in 1: 3 adds anhydrous propanone, temperature is controlled to 50 ℃ of stirrings and after 3 hours, supernatant is leached, adding in proportion anhydrous propanone to repeat to appeal step, obtain concentrated soybean phospholipid;
2) get concentrated soybean phospholipid and mix with CHA, EPA, add the Novozym435 lipase of phosphatide quality 20%, then add water to make the water content of reaction system to be 4%, 50 ℃, under pH=7.5, to react 60h and carry out ester exchange;
3) be warming up to 90 ℃ by enzyme-deactivating, unrighted acid free in system is washed away, 90kpa, 80 ℃ of thin film evaporation concentrate, and obtain liquid matter structure soybean lecithin, acquisition powder matter structure soybean lecithin crude product A after spraying is dry;
4) use purification by liquid extraction at 70 ℃ of 95% ethanol to obtain powder matter structure soybean lecithin, the large ovum Fabaceous Lecithin of the matter structure of purification is decoloured by active carbon carbon post and silicagel column successively, collect the matter structure soybean lecithin after decolouring, Vacuum Concentration 2h at 66kPa, 70 ℃, paste matter structure soybean lecithin carries out after freeze drying at-20 ℃, obtains powder matter structure soybean lecithin finished product B.
Embodiment 2
1) first crude oil of soybean is filtered, then carry out hydration degum, collect jelly to stainless cylinder of steel, ratio in 1: 3 adds anhydrous propanone, temperature is controlled to 50 ℃ of stirrings and after 3 hours, supernatant is leached, adding in proportion anhydrous propanone to repeat to appeal step, obtain concentrated soybean phospholipid;
2) get concentrated soybean phospholipid and mix with DHA, EPA, add the Novozym435 lipase of phosphatide quality 20%, then add water to make the water content of reaction system to be 4%, 55 ℃, under pH=8, to react 60h and carry out ester exchange;
3) be warming up to 90 ℃ by enzyme-deactivating, unrighted acid free in system is washed away, 90kpa, 80 ℃ of thin film evaporation concentrate, and obtain liquid matter structure soybean lecithin, acquisition powder matter structure soybean lecithin crude product A after spraying is dry;
4) use purification by liquid extraction at 70 ℃ of 95% ethanol to obtain powder matter structure soybean lecithin, the large ovum Fabaceous Lecithin of the matter structure of purification is decoloured by active carbon carbon post and silicagel column successively, collect the matter structure soybean lecithin after decolouring, Vacuum Concentration 2h at 66kPa, 70 ℃, paste matter structure soybean lecithin carries out after freeze drying at-20 ℃, obtains powder matter structure soybean lecithin finished product B.
Embodiment 3
1) first crude cotton seed oil is filtered, then carry out hydration degum, collect jelly to stainless cylinder of steel, ratio in 1: 3.5 adds anhydrous propanone, temperature is controlled to 55 ℃ of stirrings and after 3 hours, supernatant is leached, adding in proportion anhydrous propanone to repeat to appeal step, obtain cottonseed concentrated phosphatide;
2) get cottonseed concentrated phosphatide and mix with DFA, AA, add the Novozym435 lipase of phosphatide quality 22%, then add water to make the water content of reaction system to be 7%, 0 ℃, under pH=9.5, to react 55h and carry out ester exchange;
3) be warming up to 110 ℃ by enzyme-deactivating, unrighted acid free in system is washed away, at 90kpa, 80 ℃, thin film evaporation is concentrated, obtains liquid matter structure cottonseed phosphatide, obtains powder matter structure cottonseed phosphatide crude product A after spraying is dry;
4) use purification by liquid extraction at 75 ℃ of 95% ethanol to obtain powder matter structure cottonseed lecithin, the matter structure cottonseed lecithin of purification is decoloured by active carbon carbon post and silicagel column successively, collect the matter structure cottonseed lecithin after decolouring, at 67kPa, 70 ℃, Vacuum Concentration 2h obtains paste matter structure cottonseed lecithin, paste matter structure cottonseed lecithin carries out after freeze drying at-30 ℃, obtains powder matter structure cottonseed lecithin finished product B.
Embodiment 4
1) first sunflower seeds crude oil is filtered, then carry out hydration degum, collect jelly to stainless cylinder of steel, ratio in 1: 3 adds anhydrous propanone, temperature is controlled to 55 ℃ of stirrings and after 3 hours, supernatant is leached, adding in proportion anhydrous propanone to repeat to appeal step, obtain cottonseed concentrated phosphatide;
2) get sunflower seeds concentrated phosphatide and mix with DHA, EPA, add the LipozymeTLIM immobilized lipase of phosphatide quality 8%, 65 ℃, under pH=6.5, react 4h and carry out ester exchange;
3) be warming up to 100 ℃ by enzyme-deactivating, unrighted acid free in system is washed away, 88kpa, 80 ℃ of thin film evaporation concentrate, and obtain liquid matter structure sunflower seeds phosphatide, acquisition powder matter structure sunflower seeds phosphatide crude product A after spraying is dry;
4) use purification by liquid extraction powder matter structure sunflower seeds lecithin at 75 ℃ of 95% ethanol, the matter structure sunflower seeds lecithin of purification is decoloured by active carbon carbon post and silicagel column successively, collect the matter structure sunflower seeds lecithin after decolouring, Vacuum Concentration 2h at 68kPa, 65 ℃, paste matter structure sunflower seeds lecithin carries out after freeze drying at-30 ℃, obtains powder matter structure sunflower seeds lecithin finished product B.
Embodiment 5
1) get concentrated soybean phospholipid and mix with cod-liver oil, DPA, add the LipozymeTLIM immobilized lipase of phosphatide quality 10%, 80 ℃, under pH=9.0, react 6h and carry out ester exchange;
2) be warming up to 100 ℃ by enzyme-deactivating, unrighted acid free in system is washed away, at 90kpa, 80 ℃, thin film evaporation is concentrated, obtains liquid matter structure soybean lecithin, obtains powder matter structure soybean lecithin crude product A after spraying is dry;
3) use purification by liquid extraction at 75 ℃ of 95% ethanol to obtain powder matter structure soybean lecithin, the matter structure soybean lecithin of purification is decoloured by active carbon carbon post and silicagel column successively, collect the matter structure soybean lecithin after decolouring, at 66kPa, 70 ℃, Vacuum Concentration 2h obtains paste matter structure soybean lecithin, paste matter structure soybean lecithin carries out after freeze drying at-20 ℃, obtains powder matter structure soybean lecithin finished product B.
Embodiment 6
1) get yolk phospholipid and mix with AA, cod-liver oil, add the LecitaseUltra carboxylic ester hydrolases of phosphatide quality 10%, 40 ℃, under pH=4.0, react 3h and carry out ester exchange;
2) be warming up to 60 ℃ by enzyme-deactivating, unrighted acid free in system is washed away, at 90kpa, 80 ℃, thin film evaporation is concentrated, obtains liquid matter structure yolk phospholipid, obtains powder matter structure yolk phospholipid crude product A after spraying is dry;
3) use purification by liquid extraction at 75 ℃ of 95% ethanol to obtain powder matter structure egg yolk lecithin, the matter structure egg lecithin of purification is decoloured by active carbon carbon post and silicagel column successively, collect the matter structure egg yolk lecithin after decolouring, at 66kPa, 70 ℃, Vacuum Concentration 2h obtains paste matter structure egg yolk lecithin, paste matter structure egg yolk lecithin carries out after freeze drying at-20 ℃, obtains powder matter structure egg yolk lecithin finished product B.
Embodiment 7
1) get yolk phospholipid and mix with MCT, LCP, add the LecitaseUltra carboxylic ester hydrolases of phosphatide quality 10%, 45 ℃, under pH=4.5, react 3.5h and carry out ester exchange;
2) be warming up to 70 ℃ by enzyme-deactivating, unrighted acid free in system is washed away, at 90kpa, 80 ℃, thin film evaporation is concentrated, obtains liquid matter structure yolk phospholipid, obtains powder matter structure yolk phospholipid crude product A after spraying is dry;
3) use purification by liquid extraction at 75 ℃ of 95% ethanol to obtain powder matter structure egg yolk lecithin, during by purification, matter structure egg yolk lecithin decolours by active carbon carbon post and silicagel column successively, collect the matter structure egg yolk lecithin after decolouring, at 66kPa, 70 ℃, Vacuum Concentration 2h obtains paste matter structure egg yolk lecithin, paste matter structure egg yolk lecithin carries out after freeze drying at-20 ℃, obtains powder matter structure egg yolk lecithin finished product B.
Certainly, in the present invention, the extraction of matter structure phosphatide also can be used supercritical extract, and extraction efficiency is higher like this, in extraction, can also purify.
Matter structure lecithin prepared by the inventive method, there is ester exchange in the saturated fatty acid on phosphatidase 11,3, all by unrighted acid, substituted simultaneously, nutritious, more healthy for human body; Reaction condition is gentle, can not destroy the structure of finished product, particularly can well protect the unsaturated bond in unrighted acid.
Claims (9)
1. a method of producing matter structure phosphatide and lecithin, comprises the following steps:
1) by phosphatide or concentrated phosphatide and consaturated oil mixing, add catalysis phosphatide under lipase;
2) after reaction finishes, by lipase deactivation, remove free fatty, concentrated, dryly obtain Powdered matter structure phosphatide crude product A;
3) powder matter structure phosphatide crude product A further extracted, decolour, concentratedly obtain paste matter structure lecithin, after freeze drying, obtain Powdered matter structure lecithin finished product B.
2. a kind of method of producing matter structure phosphatide and lecithin according to claim 1, is characterized in that: described phosphatide comprises plant oil sources phosphatide, yolk phospholipid.
3. a kind of method of producing matter structure phosphatide and lecithin according to claim 2, is characterized in that: the extracting method of plant oil sources phosphatide is: first vegetable crude oil is filtered, then carry out hydration degum, then by the concentrated concentrated phosphatide that obtains of jelly.
4. a kind of method of producing matter structure phosphatide and lecithin according to claim 1, is characterized in that: the temperature of ester exchange reaction is 40～90 ℃.
5. a kind of method of producing matter structure phosphatide and lecithin according to claim 1, is characterized in that: the pH of ester exchange reaction is 4～9.5.
6. a kind of method of producing matter structure phosphatide and lecithin according to claim 1, is characterized in that: described lipase comprises phosphatidase, immobilized lipase, carboxylic ester hydrolases.
7. a kind of method of producing matter structure phosphatide and lecithin according to claim 1, is characterized in that: grease, DHA, EPA, DPA, medium chain fatty acid fat MCT, cod-liver oil that described consaturated oil comprises C >=18 long-chain unsaturated fatty acid, contains these long-chain unsaturated fatty acids.
8. a kind of method of producing matter structure phosphatide and lecithin according to claim 1, is characterized in that: extraction comprises solvent extraction.
9. a kind of method of producing matter structure phosphatide and lecithin according to claim 8, is characterized in that: described solvent comprises ethanol.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310602796.3A CN103636919A (en) | 2013-11-26 | 2013-11-26 | Method for preparing textural phosphatide and phosphatidylcholine |
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| CN201310602796.3A CN103636919A (en) | 2013-11-26 | 2013-11-26 | Method for preparing textural phosphatide and phosphatidylcholine |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104962590A (en) * | 2015-08-05 | 2015-10-07 | 嘉必优生物工程（武汉）有限公司 | Microbe-derived phospholipid polyunsaturated fatty acid oil and preparation method thereof |
| CN108456699A (en) * | 2018-02-26 | 2018-08-28 | 浙江海洋大学 | A kind of phosphatide type calendic acid fat or oil composition and its preparation method and application |
| CN110004190A (en) * | 2019-04-13 | 2019-07-12 | 湖南万全裕湘生物科技有限公司 | A method of preparing lecithin epoxy-type polyunsaturated fatty acid |
| CN112618723A (en) * | 2020-12-14 | 2021-04-09 | 北京化工大学 | Structured phospholipid and preparation method and application thereof |
-
2013
- 2013-11-26 CN CN201310602796.3A patent/CN103636919A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104962590A (en) * | 2015-08-05 | 2015-10-07 | 嘉必优生物工程（武汉）有限公司 | Microbe-derived phospholipid polyunsaturated fatty acid oil and preparation method thereof |
| CN106434777A (en) * | 2015-08-05 | 2017-02-22 | 嘉必优生物技术（武汉）股份有限公司 | Polyunsaturated phospholipid fatty acid grease from microorganisms |
| CN104962590B (en) * | 2015-08-05 | 2018-08-17 | 嘉必优生物技术（武汉）股份有限公司 | A kind of microbe-derived phosphatide type polyunsaturated fatty acid grease and preparation method |
| CN108456699A (en) * | 2018-02-26 | 2018-08-28 | 浙江海洋大学 | A kind of phosphatide type calendic acid fat or oil composition and its preparation method and application |
| CN110004190A (en) * | 2019-04-13 | 2019-07-12 | 湖南万全裕湘生物科技有限公司 | A method of preparing lecithin epoxy-type polyunsaturated fatty acid |
| CN112618723A (en) * | 2020-12-14 | 2021-04-09 | 北京化工大学 | Structured phospholipid and preparation method and application thereof |
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Application publication date: 20140319 |