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A kind of preparation method of injection-grade high-purity phosphatidylcholine

A phosphatidylcholine, injection-grade technology, applied in the field of chemical engineering, can solve the problems of easy membrane fouling, incomplete separation of phospholipid components, difficulty in balancing product purity and yield, and achieve high selective separation ability and product quality Stable and controllable, easy to recycle and reuse

Active Publication Date: 2015-09-02
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent ZL200510026994.5 discloses a process for preparing phosphatidylcholine by high-shear leaching with ethanol as a solvent. The content of phosphatidylcholine is only 55%. Low
Chinese patents ZL02121550.2 and ZL02149601.3 disclose a method for preparing phosphatidylcholine by multistage countercurrent leaching of soybean powder phospholipids using a mixed solvent of acetonitrile, methanol, ethanol and other monohydric low-carbon alcohols. Phosphatidylcholine The content is about 80%, the purity and quality of the product obtained by this method are still low, and the countercurrent extraction technology has the deficiency that the product purity and yield are difficult to balance
Membrane separation method has disadvantages such as easy membrane fouling, difficult regeneration, poor repeatability, high cost, small processing capacity, etc., and low separation selectivity, which cannot completely separate phospholipid components with similar molecular weights. Therefore, relevant research is limited to laboratory scale and difficult to apply. in industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] (1) Prepare commercially available phospholipid raw materials (weight percentage of phosphatidylcholine: 19%) and n-heptane to form a raw material solution with a phospholipid concentration of 350 g / L, centrifugally filter to remove insoluble impurities, and use 1,2 propylene glycol As the extractant, use n-heptane as the detergent, conduct a fractional distillation extraction at 35°C, and collect the extract. The extract is concentrated in vacuo to obtain the primary extraction product of phosphatidylcholine.

[0057] (2) Dissolve the primary extraction product of phosphatidylcholine in 1,2 propylene glycol and methanol binary mixed solvent B (volume ratio 7:3), the concentration is 80 g / L, use n-heptane as the extraction agent, and use 1,2 2 Propylene glycol and methanol binary mixed solvent B (volume ratio 7:3) is used as detergent, and at 35°C, carry out secondary fractionation extraction, and collect the extract. The extract is concentrated in vacuum to obtain the...

Embodiment 2

[0060] (1) Commercially available phospholipid raw materials (weight percentage of phosphatidylcholine: 19%) and n-hexane are made into a raw material solution with a phospholipid concentration of 350 grams per liter, centrifugal filtration to remove insoluble impurities, and 1-hydroxypropyl Base-3-methylimidazole acetic acid ionic liquid-ethanol binary mixed solvent A (volume ratio 1:9) was used as the extractant, n-hexane was used as the detergent, and a fractional extraction was performed at 30°C to collect the extract. The extract is evaporated to remove the ethanol solvent, then back-extracted with n-hexane, and concentrated in vacuo to obtain the primary extraction product of phosphatidylcholine.

[0061] (2) Dissolve the primary extraction product of phosphatidylcholine in 1-hydroxypropyl-3-methylimidazolium acetate ionic liquid-methanol binary mixed solvent B (volume ratio 5:5), the concentration is 100 g / L, and n-Hexane was used as extractant, 1-hydroxypropyl-3-methyl...

Embodiment 3

[0064] (1) Commercially available phospholipid raw materials (weight percentage of phosphatidylcholine: 25%) and petroleum ether with a boiling range of 90-120 ° C are formulated into a raw material solution with a phospholipid concentration of 260 g / L, and centrifugal filtration to remove insoluble impurities , using 1-carboxylic acid propyl-3-methylimidazole-trifluoromethanesulfonimide ionic liquid-ethanol binary mixed solvent A (volume ratio 2:8) as the extraction agent, and petroleum with a boiling range of 90-120°C Ether is used as a detergent. At 20°C, a fractional distillation extraction is carried out, and the extract is collected by flow ratio. The extract is evaporated to remove the ethanol solvent, back-extracted, and concentrated in vacuo to obtain the primary extraction product of phosphatidylcholine.

[0065] (2) Dissolve the primary extraction product of phosphatidylcholine in 1-carboxypropyl-3-methylimidazole-trifluoromethanesulfonimide ionic liquid-ethanol bin...

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Abstract

The invention discloses a preparation method of injection grade high-purity phosphatidyl choline. The preparation method comprises the following steps of: (1) dissolving a phospholipid raw material in a non-polar solvent to prepare primary extraction raw material liquid, carrying out centrifugal filtration to remove solid impurities, and carrying out primary fractional extraction to obtain primary extraction liquid; (2) carrying out vacuum concentration on the primary extraction liquid to obtain a primary phosphatidyl choline product; (3) preparing the phosphatidyl choline primary product to secondary extraction raw material liquid, and carrying out secondary fractional extraction to obtain secondary extraction liquid; (4) carrying out vacuum concentration on the secondary extraction liquid to obtain a secondary phosphatidyl choline extraction product; and (5) dissolving the secondary phosphatidyl choline extraction product in a polar solvent, continuously collecting effluent through a decoloration adsorption column, and carrying out vacuum concentration and freeze drying to obtain an injection grade high-purity phosphatidyl choline product. According to the preparation method, a process route comprising a primary fractional extraction unit, a secondary fractional extraction unit, a decoloration unit, a freeze drying unit and the like is adopted, and the purity of the phosphatidyl choline product is high.

Description

technical field [0001] The invention relates to a method for separating phosphatidylcholine, which belongs to the technical field of chemical engineering, in particular to a method for preparing injection-grade high-purity phosphatidylcholine. Background technique [0002] High-purity phosphatidylcholine is a natural, safe and efficient emulsifier, which can be used as an emulsifier for infusion or intravenous injection. It is the most commonly used and safest emulsifier in the field of injection. At the same time, due to its liposome characteristics, phosphatidylcholine can be used as a carrier for anticancer drugs and other slow-release drugs, which can significantly improve the activity of drugs and reduce side effects. Compared with other drug carriers, it has the advantages of low toxicity and high efficiency. When phosphatidylcholine is used for injection, liposome, etc., there are strict requirements on the purity, impurity content, and water content of phosphatidylch...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/10
CPCY02P20/54
Inventor 邢华斌鲍宗必杨启炜张治国苏宝根任其龙杨亦文苏云闻光东陈丽芬
Owner ZHEJIANG UNIV
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