CN108101938B - Preparation method of high-purity polyene phosphatidylcholine - Google Patents
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Abstract
The invention discloses a preparation method of high-purity polyene phosphatidylcholine, which comprises the step of preparing the high-purity polyene phosphatidylcholine by respectively adsorbing soybean phospholipid powder by neutral alumina and silica gel. The polyene phosphatidyl choline prepared by the preparation method has low peroxide value, high purity and simple process operation, is beneficial to industrial production, and has purity of over 98 percent and content of over 95 percent, and all related substances are qualified.
Description
Technical Field
The invention belongs to the field of pharmacy, and particularly relates to a preparation method of high-purity polyene phosphatidylcholine, wherein the polyene phosphatidylcholine can be used for adjuvant therapy of liver diseases.
Background
The natural phospholipid is the basic component of animal and plant cell membrane, nuclear membrane and plastid membrane, and is the material basis of living body. The soybean phospholipid contains components such as Phosphatidylcholine (PC), Phosphatidylethanolamine (PE), Phosphatidylinositol (PI), Phosphatidic Acid (PA) and the like, wherein the phosphatidylcholine is also called lecithin, is a lipid substance containing phosphoric acid, has special physiological activity, has an oleophylic non-polar end of fatty acyl and a hydrophilic polar end of phosphate ester group and choline group, is a surfactant with excellent performance, and is widely applied to the fields of food, cosmetics, medicines and the like.
Natural Phosphatidylcholine (PC), also known as polyenylphosphatidylcholine, contains a large amount of unsaturated fatty acids, mainly linoleic acid (about 70%), linolenic acid and oleic acid, which are used for various liver diseases such as hepatitis, chronic hepatitis, hepatic necrosis, liver cirrhosis, hepatic coma (including precursor hepatic coma); fatty liver (also found in diabetics); bile obstruction; poisoning; preventing the recurrence of gallstone; pre-and post-operative treatment, particularly hepatobiliary surgery; gestational toxicities, including vomiting; psoriasis; neurodermatitis and radiation syndrome.
However, the problem of how to increase the purity of PC has been restricting the application of PC. The purification method of soybean PC mainly comprises solvent extraction (building, Qiangming, Xujie, Sunwmeimin, etc.. preparation of high-purity phosphatidylcholine and fatty acid analysis thereof. food science 2010,31(18):224-2A process for separating phosphatidylcholine from soybean phosphatide by supercritical fluid separation includes such steps as separating soybean phosphatidylcholine by gay, membrane separation (Wang Yong, Wang Xingguan, Ooshiyi, etc.), (Chinese oil and fat, 2002,27(3):72-73), and column chromatography (6-8 for Cao, Tu Ericheng, Wang, etc.). the chromatographic separation of phosphatidylcholine in soybean phosphatide by alumina column is disclosed, Chinese oil and fat, 2001,26(6):51-53, 2, Hanxue, Wang, huchang, etc., and column chromatography (19-22 for separating and purifying soybean phosphatidylcholine by column chromatography). The solvent extraction method has overlarge solvent consumption and loss, and toxicity can cause pollution to the environment; although the inorganic salt precipitation method can improve the purity of PC, the inorganic salt precipitation method can increase the residual amount of inorganic salt in the product; although the supercritical technology has the advantages of environmental protection, no pollution and high product purity, the equipment cost is too high, the power consumption is large, and the industrial production is not facilitated.
Disclosure of Invention
The invention develops a method for preparing high-purity polyene phosphatidyl choline, the prepared polyene phosphatidyl choline has low peroxide value, high purity and simple process operation, is beneficial to industrial production, the purity can reach more than 98 percent, the content can reach more than 90 percent, and all related substances are qualified.
The invention aims to provide a preparation method of high-purity polyene phosphatidylcholine.
Specifically, in an embodiment of the present invention, the present invention provides a method for preparing high purity polyene phosphatidylcholine, comprising the steps of:
(1) using soybean phospholipid powder with the purity of 35-60% as a raw material, and adopting neutral alumina for adsorption to prepare polyene phosphatidylcholine with the purity of more than 90%;
(2) and (2) the polyene phosphatidylcholine with the purity of more than 90 percent obtained in the step (1) is used as a raw material, and silica gel is adopted for adsorption to prepare the polyene phosphatidylcholine with the purity of more than 95 percent.
In the embodiment of the invention, the preparation method of high-purity polyene phosphatidylcholine provided by the invention comprises the following steps of (1) dissolving soybean phospholipid powder with the purity of 35-60% as a raw material in an organic solvent 1, then carrying out adsorption and filtration for 1-5 times by using neutral alumina, and concentrating the filtrate to obtain polyene phosphatidylcholine with the purity of more than 90%.
In the embodiment of the invention, the preparation method of high-purity polyene phosphatidylcholine provided by the invention is characterized in that in the step (2), polyene phosphatidylcholine with the purity of more than 90% obtained in the step (1) is used as a raw material, the polyene phosphatidylcholine is dissolved in an organic solvent 2, silica gel is adopted for adsorption and filtration for 1-5 times, and the filtrate is concentrated to obtain polyene phosphatidylcholine with the purity of more than 95%.
In an embodiment of the present invention, the present invention provides a method for preparing high-purity polyene phosphatidylcholine, wherein the soybean phospholipid powder has a purity of preferably 40 to 60%, particularly preferably 50 to 60%.
In an embodiment of the present invention, the present invention provides a method for preparing high-purity polyene phosphatidylcholine, wherein the organic solvent 1 in step (1) is selected from 95 vol% ethanol, absolute ethanol, methanol, dichloromethane, chloroform, a mixed solvent of absolute ethanol and dichloromethane, a mixed solvent of absolute ethanol and trichloromethane, a mixed solvent of methanol and dichloromethane, or a mixed solvent of methanol and trichloromethane, preferably methanol.
In an embodiment of the present invention, the present invention provides a method for preparing high-purity polyene phosphatidylcholine, wherein the mass ratio of the soybean phospholipid powder in step (1) to the organic solvent 1 is 1: 2.4-1: 8, preferably 1: 4-1: 4.8.
in the embodiment of the invention, the invention provides a preparation method of high-purity polyene phosphatidylcholine, wherein the mesh number of the neutral alumina in the step (1) is 100-200 meshes, 200-300 meshes or 300-400 meshes, preferably 200-300 meshes.
In an embodiment of the present invention, the present invention provides a method for preparing high-purity polyene phosphatidylcholine, wherein the mass ratio of the soybean phospholipid powder to the neutral alumina in the step (1) is 1: 2-1: 8, preferably 1: 2-1: 3.
in an embodiment of the present invention, the present invention provides a method for preparing high-purity polyene phosphatidylcholine, wherein the adsorption and filtration times of the neutral alumina in the step (1) are preferably 1 to 4 times, and more preferably 2 to 3 times.
In an embodiment of the present invention, the present invention provides a method for preparing high purity polyene phosphatidylcholine, wherein the time of each adsorption of the neutral alumina in the step (1) is 1-3 hours, preferably 1-2 hours.
In the embodiment of the invention, the invention provides a preparation method of high-purity polyene phosphatidylcholine, wherein the adsorption temperature in the step (1) is 0-45 ℃, preferably 20-30 ℃.
In a preferred embodiment of the present invention, the present invention provides a method for preparing high-purity polyene phosphatidylcholine, wherein the mass ratio of the soybean phospholipid powder to the organic solvent 1 in step (1) is 1: 4, wherein the organic solvent 1 is methanol; the mass ratio of the soybean lecithin powder to the neutral alumina is 1: 2; the mesh number of the neutral alumina is as follows: 200-300 meshes; the adsorption temperature is 20-30 ℃; the adsorption time is 1-2 hours, and the adsorption times are 2-3 times.
In an embodiment of the present invention, the present invention provides a method for preparing high-purity polyene phosphatidylcholine, wherein the organic solvent 2 in step (2) is selected from dichloromethane, chloroform, a mixed solvent of methanol and dichloromethane, or a mixed solvent of methanol and chloroform, preferably a mixed solvent of dichloromethane and methanol.
In an embodiment of the present invention, the present invention provides a preparation method of high-purity polyene phosphatidylcholine, wherein the organic solvent 2 in the step (2) is a mixed solvent of dichloromethane and methanol, and the volume ratio of dichloromethane to methanol is 2: 1-10: 1, preferably, 5: 1.
in an embodiment of the present invention, the present invention provides a method for preparing high-purity polyene phosphatidylcholine, wherein the volume ratio of polyene phosphatidylcholine having a purity of 90% or more obtained in step (1) in step (2) to organic solvent 2 is 1: 2-1: 6, preferably, 1: 4.
in an embodiment of the present invention, the present invention provides a method for preparing high-purity polyene phosphatidylcholine, wherein the mass ratio of polyene phosphatidylcholine having a purity of 90% or more obtained in the step (1) in the step (2) to silica gel is 1: 1-1: 3, preferably, 1: 2.
in an embodiment of the present invention, the present invention provides a method for preparing high purity polyene phosphatidylcholine, wherein the number of times of adsorption and filtration of the silica gel in the step (2) is 1 to 4, preferably 2.
In the embodiment of the invention, the invention provides a preparation method of high-purity polyene phosphatidylcholine, wherein the mesh number of the silica gel in the step (2) is 100-200 meshes, 200-300 meshes or 300-400 meshes, preferably 200-300 meshes.
In the embodiment of the invention, the invention provides a preparation method of high-purity polyene phosphatidylcholine, wherein the adsorption temperature in the step (2) is 0-45 ℃, preferably 20-30 ℃.
In an embodiment of the present invention, the present invention provides a method for preparing high purity polyene phosphatidylcholine, wherein the adsorption in step (2) is performed for 1-3 hours, preferably 2 hours each time.
In a preferred embodiment of the present invention, there is provided a method for preparing high-purity polyene phosphatidylcholine, wherein the organic solvent 2 in the step (2) is a mixture of organic solvents in a volume ratio of 5: 1, and the volume ratio of the polyene phosphatidylcholine with the purity of more than 90% obtained in the step (1) in the step (2) to the organic solvent 2 is 1: 4, the mass ratio of the polyene phosphatidylcholine with the purity of more than 90 percent obtained in the step (1) in the step (2) to the silica gel is 1: 2, the mesh number of the silica gel is: 200-300 meshes, the adsorption temperature is as follows: the adsorption time is 2 hours at 20-30 ℃ and the adsorption frequency is 2 times.
Compared with column chromatography, the process disclosed by the invention has the advantages of simple process, small organic solvent consumption, short concentration time, less industrial three wastes, contribution to peroxide value control and the like. The column chromatography process is a traditional method for purifying polyene phosphatidylcholine, but the characteristics of huge dosage of organic solvent, long concentration time and the like in the column chromatography process directly influence the batch and peroxide value of the process. According to experimental investigation, the peroxide value of the polyene phosphatidylcholine is increased rapidly from 1.95 to 14.86 by concentrating the polyene phosphatidylcholine at 40 +/-5 ℃ for 48 hours under the protection of nitrogen. Therefore, if the batch size of the traditional column chromatography process is more than 4.0 kg/batch, the concentration time is greatly prolonged, the peroxide value is uncontrollable, and the industrial production amplification is not facilitated. The present invention can effectively solve the above problems.
Detailed Description
The technical solutions of the present invention are further described below by examples, which are exemplary and do not limit the scope of the present invention. The technical features of the invention are equally replaced by the prior art according to the teaching of the invention and the technical scope of the invention is also covered by the technical personnel in the technical field.
In the following examples, soybean phospholipid powder having a purity of 50% in step (1) was obtained from Shenyang Tianfeng biopharmaceutical Co., Ltd, and neutral alumina was obtained from Chemicals Co., Ltd, and other materials and reagents were all commercially available products unless otherwise specified.
Example 1
Preparation of polyene phosphatidyl choline with purity more than 90%
Adding methanol (500ml) into a 1L three-neck round-bottom reaction flask, replacing three times with vacuum nitrogen, adding soybean phospholipid powder (100g) with the purity of 50% under the protection of nitrogen, stirring for dissolving, adding 200-mesh 300-mesh neutral alumina (200g), controlling the temperature to be 20-30 ℃, stirring for adsorption for 2 hours, filling diatomite for suction filtration, leaching a filter cake by 100ml of methanol, collecting filtrate, and completing one-time adsorption.
And adding the filtrate into a 1L three-neck round-bottom reaction flask again, replacing the filtrate with nitrogen in vacuum for three times, adding 200-mesh 300-mesh neutral alumina (200g) under the protection of nitrogen, controlling the temperature to be 20-30 ℃, stirring and adsorbing for 2 hours, performing suction filtration by using kieselguhr, leaching a filter cake by using 100ml of methanol, collecting the filtrate, and completing secondary adsorption.
And adding the filtrate into a 1L three-neck round-bottom reaction flask again, replacing the filtrate with nitrogen in vacuum for three times, adding 200-mesh 300-mesh neutral alumina (200g) under the protection of nitrogen, controlling the temperature to be 20-30 ℃, stirring and adsorbing the mixture for 2 hours, performing suction filtration by using kieselguhr, leaching a filter cake by using 100ml of methanol, collecting the filtrate, and performing reduced pressure concentration at 45 +/-5 ℃ under the protection of nitrogen to obtain a light yellow waxy solid.
The yield thereof was found to be 38%. Hplc (elsd) purity > 97.8%.
Example 2
Preparation of polyene phosphatidyl choline with purity greater than 95%
Dissolving the light yellow waxy solid obtained after concentration in example 1 in 150ml of mixed solvent (the volume ratio of dichloromethane to methanol is 5: 1), replacing the mixture by vacuum nitrogen for three times, adding 200-mesh and 300-mesh silica gel (76g) under the protection of nitrogen, stirring and adsorbing for 2 hours at the temperature of 20-30 ℃, leaching a filter cake by using pad diatomite, leaching 38ml of mixed solvent (the volume ratio of dichloromethane to methanol is 5: 1), collecting filtrate, and completing primary adsorption.
And adding the filtrate into a 250ml three-neck round-bottom reaction flask again, replacing the filtrate with nitrogen in vacuum for three times, adding 200-mesh 300-mesh silica gel (76g) under the protection of nitrogen, controlling the temperature to be 20-30 ℃, stirring and adsorbing the mixture for 2 hours, performing suction filtration by using kieselguhr, leaching a filter cake by using 38ml of a mixed solvent (the volume ratio of dichloromethane to methanol is 5: 1), collecting the filtrate, and performing reduced pressure concentration at 45 +/-5 ℃ under the protection of nitrogen to obtain a light yellow waxy solid.
The yield thereof was found to be 73%. Hplc (elsd) purity > 99.4% with a peroxide value of 1.20.
Example 3
Preparation of polyene phosphatidyl choline with purity more than 90%
Adding methanol (500ml) into a 1L three-mouth round-bottom reaction flask, replacing three times with vacuum nitrogen, adding soybean phospholipid powder (100g) under the protection of nitrogen, stirring for dissolving, adding 200-mesh 300-mesh neutral alumina (300g), stirring for adsorbing for 2 hours at the temperature of 20-30 ℃, filtering by using kieselguhr, leaching a filter cake by using 100ml of methanol, collecting filtrate, and completing one-time adsorption.
And adding the filtrate into a 1L three-neck round-bottom reaction flask again, replacing the filtrate with nitrogen in vacuum for three times, adding 200-mesh 300-mesh neutral alumina (300g) under the protection of nitrogen, controlling the temperature to be 20-30 ℃, stirring and adsorbing the mixture for 2 hours, performing suction filtration by using kieselguhr, leaching a filter cake by using 100ml of methanol, collecting the filtrate, and performing reduced pressure concentration at 45 +/-5 ℃ under the protection of nitrogen to obtain a light yellow waxy solid.
The yield thereof was found to be 40%. Hplc (elsd) purity > 96.3%.
Example 4
Preparation of polyene phosphatidyl choline with purity greater than 95%
Dissolving the light yellow waxy solid obtained after concentration in example 3 in 160ml of mixed solvent (the volume ratio of dichloromethane to methanol is 2: 1), replacing the mixture by vacuum nitrogen for three times, adding 200-mesh and 300-mesh silica gel (80g) under the protection of nitrogen, stirring and adsorbing for 2 hours at the temperature of 20-30 ℃, leaching filter cakes by using kieselguhr as a pad, leaching 40ml of mixed solvent (the volume ratio of dichloromethane to methanol is 2: 1), collecting filtrate, and completing primary adsorption.
And adding the filtrate into a 250ml three-neck round-bottom reaction flask again, replacing the filtrate with nitrogen in vacuum for three times, adding 200-mesh 300-mesh silica gel (80g) under the protection of nitrogen, controlling the temperature to be 20-30 ℃, stirring and adsorbing the mixture for 2 hours, performing suction filtration by using kieselguhr, leaching a filter cake by using 40ml of a mixed solvent (the volume ratio of dichloromethane to methanol is 2: 1), collecting the filtrate, and performing reduced pressure concentration at 45 +/-5 ℃ under the protection of nitrogen to obtain a light yellow waxy solid.
The yield thereof was found to be 64%. Hplc (elsd) purity > 98.7% with a peroxide value of 1.95.
Example 5
Preparation of polyene phosphatidyl choline with purity more than 90%
Adding a mixed solvent (the volume ratio of dichloromethane to methanol is 1:1) (500ml) into a 1L three-neck round-bottom reaction flask, replacing the mixture with nitrogen in vacuum for three times, adding soybean phospholipid powder (100g) under the protection of nitrogen, stirring to dissolve the mixture clearly, adding 200-mesh 300-mesh neutral alumina (200g), controlling the temperature to be 20-30 ℃, stirring and adsorbing for 2 hours, filtering by using kieselguhr, leaching a filter cake by using 100ml of the mixed solvent (the volume ratio of dichloromethane to methanol is 1:1), collecting a filtrate, and completing primary adsorption.
Adding the filtrate into a 1L three-neck round-bottom reaction flask again, replacing the filtrate with nitrogen in vacuum for three times, adding 200-mesh 300-mesh neutral alumina (200g) under the protection of nitrogen, controlling the temperature to be 20-30 ℃, stirring and adsorbing for 2 hours, performing suction filtration by using kieselguhr, leaching a filter cake by using 100ml of mixed solvent (the volume ratio of dichloromethane to methanol is 1:1), collecting the filtrate, and completing secondary adsorption.
Adding the filtrate into a 1L three-neck round-bottom reaction flask again, replacing the filtrate with nitrogen in vacuum for three times, adding 200-mesh 300-mesh neutral alumina (200g) under the protection of nitrogen, controlling the temperature to be 20-30 ℃, stirring and adsorbing the mixture for 2 hours, performing suction filtration by using kieselguhr, leaching a filter cake by using 100ml of a mixed solvent (the volume ratio of dichloromethane to methanol is 1:1), collecting the filtrate, and performing reduced pressure concentration at 45 +/-5 ℃ under the protection of nitrogen to obtain a light yellow waxy solid.
The yield thereof was found to be 33%. Hplc (elsd) purity > 95.1%.
Example 6
Preparation of polyene phosphatidyl choline with purity greater than 95%
Dissolving the light yellow waxy solid obtained after concentration in the example 5 in 130ml dichloromethane, replacing the solution for three times by vacuum nitrogen, adding 200-mesh and 300-mesh silica gel (66g) under the protection of the nitrogen, controlling the temperature to be 20-30 ℃, stirring and adsorbing the mixture for 2 hours, performing suction filtration by using kieselguhr, leaching a filter cake by using 33ml dichloromethane, collecting filtrate, and completing one-time adsorption.
And adding the filtrate into a 250ml three-neck round-bottom reaction flask again, replacing the filtrate with nitrogen in vacuum for three times, adding 200-mesh 300-mesh silica gel (66g) under the protection of nitrogen, controlling the temperature to be 20-30 ℃, stirring and adsorbing the mixture for 2 hours, filtering the mixture by using kieselguhr, leaching a filter cake by using 33ml of dichloromethane, collecting the filtrate, and concentrating the filtrate under reduced pressure at 45 +/-5 ℃ under the protection of nitrogen to obtain a light yellow waxy solid.
The yield thereof was found to be 48%. Hplc (elsd) purity > 98.5% with a peroxide value of 1.73.
Example 7
Preparation of polyene phosphatidyl choline with purity more than 90%
Adding a mixed solvent (the volume ratio of dichloromethane to absolute ethyl alcohol is 1:1) (500ml) into a 1L three-neck round-bottom reaction flask, replacing the mixture with nitrogen in vacuum for three times, adding soybean phospholipid powder (100g) under the protection of nitrogen, stirring to dissolve, adding 200-mesh 300-mesh neutral alumina (200g), controlling the temperature to be 20-30 ℃, stirring and adsorbing for 2 hours, filtering by using kieselguhr, leaching a filter cake by using 100ml of the mixed solvent (the volume ratio of dichloromethane to absolute ethyl alcohol is 1:1), collecting filtrate, and completing primary adsorption.
Adding the filtrate into a 1L three-neck round-bottom reaction flask again, replacing the filtrate with nitrogen in vacuum for three times, adding 200-mesh 300-mesh neutral alumina (200g) under the protection of nitrogen, controlling the temperature to be 20-30 ℃, stirring and adsorbing for 2 hours, performing suction filtration by using kieselguhr, leaching a filter cake by using 100ml of mixed solvent (the volume ratio of dichloromethane to absolute ethyl alcohol is 1:1), collecting the filtrate, and completing secondary adsorption.
Adding the filtrate into a 1L three-neck round-bottom reaction flask again, replacing the filtrate with nitrogen in vacuum for three times, adding 200-mesh 300-mesh neutral alumina (200g) under the protection of nitrogen, controlling the temperature to be 20-30 ℃, stirring and adsorbing the mixture for 2 hours, performing suction filtration by using kieselguhr, leaching a filter cake by using 100ml of a mixed solvent (the volume ratio of dichloromethane to absolute ethyl alcohol is 1:1), collecting the filtrate, and concentrating the filtrate under the protection of nitrogen and under the reduced pressure at 45 +/-5 ℃ to obtain a light yellow waxy solid.
The yield thereof was found to be 39%. Hplc (elsd) purity > 95.9%.
Example 8
Preparation of polyene phosphatidyl choline with purity greater than 95%
The light yellow waxy solid obtained after the concentration in the example 7 is dissolved in 150ml of mixed solvent (the volume ratio of the dichloromethane to the methanol is 10:1), the mixture is replaced by nitrogen in vacuum for three times, 200-mesh and 300-mesh silica gel (78g) is added under the protection of the nitrogen, the temperature is controlled to be 20-30 ℃, the mixture is stirred and adsorbed for 2 hours, the filter cake is leached by using the diatomite, 39ml of the mixed solvent (the volume ratio of the dichloromethane to the methanol is 10:1), the filtrate is collected, and the primary adsorption is completed.
And adding the filtrate into a 250ml three-neck round-bottom reaction flask again, replacing the filtrate with nitrogen in vacuum for three times, adding 200-mesh 300-mesh silica gel (78g) under the protection of nitrogen, controlling the temperature to be 20-30 ℃, stirring and adsorbing the mixture for 2 hours, performing suction filtration by using kieselguhr, leaching a filter cake by using 39ml of a mixed solvent (the volume ratio of dichloromethane to methanol is 10:1), collecting the filtrate, and performing reduced pressure concentration at 45 +/-5 ℃ under the protection of nitrogen to obtain a light yellow waxy solid.
The yield thereof was found to be 61%. Hplc (elsd) purity > 98.9% with a peroxide value of 1.80.
Claims (13)
1. A preparation method of high-purity polyene phosphatidyl choline comprises the following steps:
(1) dissolving soybean phospholipid powder with purity of 35-60% in organic solvent 1, adsorbing with neutral alumina for 1-5 times, filtering, and concentrating the filtrate to obtain polyene phosphatidylcholine with purity of above 90%; the organic solvent 1 is selected from 95 volume percent ethanol, absolute ethanol, methanol, dichloromethane, trichloromethane, a mixed solvent of absolute ethanol and dichloromethane, a mixed solvent of absolute ethanol and trichloromethane, a mixed solvent of methanol and dichloromethane, or a mixed solvent of methanol and trichloromethane;
(2) dissolving the polyene phosphatidyl choline with the purity of more than 90 percent obtained in the step (1) in an organic solvent 2, adsorbing and filtering the polyene phosphatidyl choline for 1 to 5 times by using silica gel, and concentrating the filtrate to obtain the polyene phosphatidyl choline with the purity of more than 95 percent; the organic solvent 2 is selected from dichloromethane, trichloromethane, a mixed solvent of methanol and dichloromethane, or a mixed solvent of methanol and trichloromethane.
2. The production method according to claim 1, wherein the organic solvent 1 in step (1) is methanol.
3. The production method according to claim 1, wherein the mass ratio of the soybean phospholipid powder to the organic solvent 1 in step (1) is 1: 2.4-1: 8.
4. the production method according to claim 3, wherein the mass ratio of the soybean phospholipid powder to the organic solvent 1 in step (1) is 1: 4-1: 4.8.
5. the method as claimed in claim 1, wherein the mesh size of the neutral alumina in step (1) is 100-200 mesh, 200-300 mesh or 300-400 mesh.
6. The preparation method according to claim 5, wherein the mesh size of the neutral alumina in the step (1) is 200-300 meshes.
7. The method according to claim 1, wherein the mass ratio of the soybean phospholipid powder to the neutral alumina in the step (1) is 1: 2-1: 8.
8. the method according to claim 7, wherein the mass ratio of the soybean phospholipid powder to the neutral alumina in the step (1) is 1: 2-1: 3.
9. the production method according to claim 1, wherein the organic solvent 2 in the step (2) is a mixed solvent of dichloromethane and methanol.
10. The process according to claim 1, wherein the volume ratio of the polyene phosphatidylcholine having a purity of 90% or more obtained in the step (1) in the step (2) to the organic solvent 2 is 1: 2-1: 6.
11. the process according to claim 10, wherein the volume ratio of the polyene phosphatidylcholine having a purity of 90% or more obtained in the step (1) in the step (2) to the organic solvent 2 is 1: 4.
12. the process according to claim 1, wherein the mass ratio of polyene phosphatidylcholine having a purity of 90% or more obtained in step (2) in step (1) to silica gel is 1: 1-1: 3.
13. the production method according to claim 12, wherein the mass ratio of the polyene phosphatidylcholine having a purity of 90% or more obtained in step (1) in step (2) to the silica gel is 1: 2.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5783210A (en) * | 1986-11-28 | 1998-07-21 | The Liposome Company, Inc. | Phospholipid composition |
| CN1837222A (en) * | 2006-04-17 | 2006-09-27 | 江南大学 | Process for preparing high purity soy phoshatidylcholine without lysophosphatide |
| CN104592292A (en) * | 2014-12-30 | 2015-05-06 | 广州白云山汉方现代药业有限公司 | Preparation method for polyene phosphatidyl choline for injection |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5783210A (en) * | 1986-11-28 | 1998-07-21 | The Liposome Company, Inc. | Phospholipid composition |
| CN1837222A (en) * | 2006-04-17 | 2006-09-27 | 江南大学 | Process for preparing high purity soy phoshatidylcholine without lysophosphatide |
| CN104592292A (en) * | 2014-12-30 | 2015-05-06 | 广州白云山汉方现代药业有限公司 | Preparation method for polyene phosphatidyl choline for injection |
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