Refining method of polyethylene glycol containing ethylene oxide impurities

A refining method and ethylene oxide technology, applied in the refining field of polyethylene glycol, can solve the problems of high residual impurities, inability to meet high-level requirements, and difficulty in removing ethylene oxide, and achieve stable product quality and low cost. , the effect of short response time

Active Publication Date: 2015-01-07
辽宁奥克药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to overcome the defects of difficult removal of ethylene oxide, high residual impurities and inability to meet high-level requirements in the existing polyethylene glycol production process, the purpose of the present invention is to provide a polyethylene glycol containing ethylene oxide impurity Refining method, the content of ethylene oxide in the obtained refined polyethylene glycol can be reduced to less than 1ppm, which meets the pharmacopoeia standard, and can be applied to the fields of medicine, cosmetics and other products that are in contact with the human body

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1. Preparation of sodium triethylene glycol

[0025] Under the protection of nitrogen, add 751 mg of sodium metal to 10 grams of newly distilled commercially available triethylene glycol, and stir at room temperature until the metal sodium is completely reacted, thus obtaining a sodium triethylene glycol / triethylene glycol solution with a mass percentage of 50%. Stored in a glass bottle under nitrogen atmosphere for later use, referred to as high activity monomer 1.

[0026] 2. Refining of polyethylene glycol

[0027] In a well-ventilated fume hood, take 30 grams of spray and circulate 5m outside 3 Polyethylene glycol-4000 (containing 20 ppm residual ethylene oxide monomer) produced by the ethoxylation reaction device was put into a 50 ml glass reaction flask, and 2 mg of high activity monomer 1 was added. After nitrogen replacement, under stirring, Under the condition of maintaining a negative pressure of 0.05 bar, heating to 130°C, using gas chromatography to detect the res...

Embodiment 2

[0029] Refining of polyethylene glycol

[0030] In a well-ventilated fume hood, take 100 grams of spray and circulate 5m outside 3 The polyethylene glycol-6000 (containing 25 ppm residual ethylene oxide monomer) produced by the ethoxylation reaction device was put into a 150 ml glass reaction flask, and 6 mg of the highly active monomer 1 prepared in Example 1 was added. After nitrogen replacement, under stirring and maintaining a negative pressure of 0.05 bar, heating to 130°C, using gas chromatography to detect the residual ethylene oxide monomer in the reaction until the residual ethylene oxide monomer content is less than 1 ppm, the reaction is about For 30 minutes, cool to 70°C, neutralize with lactic acid to pH 7, and then cool to room temperature, so that the content of residual ethylene oxide monomer in the polyethylene glycol 6000 product is not more than 1ppm, which meets the pharmacopoeia standard .

Embodiment 3

[0032] The specific operation is the same as in Example 1, except that 4.473 grams of metallic barium is used instead of 751 mg of metallic sodium. The resulting polyethylene glycol 4000 product contains no more than 1 ppm residual ethylene oxide monomer, which complies with the Pharmacopoeia standard.

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PUM

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Abstract

The invention provides a refining method of polyethylene glycol containing ethylene oxide impurities. According to the method, the ethylene oxide impurities are removed through an ethoxylation reaction of a to-be-refined polyethylene glycol crude product and an initiator containing reactive hydrogen under the existence of a high-activity ethoxylation reaction unit, so that refined polyethylene glycol is obtained, wherein the high-activity ethoxylation reaction unit is selected from metal salt of triethylene glycol, tetraethylene glycol or polyethylene glycol. According to the refining method provided by the invention, trace ethylene oxide impurities in a polyethylene glycol product can be effectively removed, so that the content of the ethylene oxide impurities is reduced to be lower than 1 ppm, and the medical level requirement is met; new impurities cannot be introduced with the refining method, the quality of the polyethylene glycol product is guaranteed, the product batch repeatability is good, and the product quality is stable; and the refining method is short in reaction time, mild in condition, simple to operate, environment-friendly, high in production efficiency, low in cost and very suitable for industrial application.

Description

Technical field [0001] The invention relates to the field of pharmaceutical excipients, in particular to a method for refining polyethylene glycol containing ethylene oxide impurities. Background technique [0002] The structural formula of polyethylene glycol (PEG) is H(OCH 2 CH 2 ) n OH, n represents the average addition number of ethylene oxide, n can range from 4 to 900, and the corresponding average molecular weight is 180 to 40,000. PEG is usually prepared by ethoxylation reaction of ethylene oxide with water, ethylene glycol and diethylene glycol (US2007 / 0179199A1 Polyethylene glycol and producing of the same.). Medicinal polyethylene glycol is often in contact with human skin, and can also be taken orally or injected into the body. For example, it can be used as a solvent for active pharmaceutical ingredients, fixatives for spices in medicinal dripping pills, liquid components in injections, and dietary supplements. Ointment bases in tablets and suppositories, soft capsu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/46
Inventor 孔凡志朱建民刘兆滨仲崇纲
Owner 辽宁奥克药业股份有限公司
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