A method for detecting the purity of 3-methylamino-1,2-propanediol by gas chromatography

A technology of gas chromatography and detection method, which is applied in the field of separation of various impurity components in 3-methylamino-1,2-propanediol, and can solve the problems of difficult data accuracy, complicated post-processing steps, and large amount of n-hexane and other problems, to achieve the effect of simple operation, saving analysis time and high recovery rate
CN105758970BInactive Publication Date: 2018-05-15TAISHAN MEDICAL UNIV
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
TAISHAN MEDICAL UNIV
Publication Date
2018-05-15
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention provides a method for detecting the purity of 3-methylamino-1,2-propanediol by gas chromatography. The method includes sample preparation, setting of chromatographic conditions, and detection operation; the setting of the chromatographic conditions, The column temperature is 240‑260°C. The invention can simultaneously detect and analyze the content of 3-methylamino-1,2-propanediol and impurities therein; improve the accuracy and precision of the analysis data, have good repeatability and high sensitivity; the detection time is short, the operation is simple, and analysts are saved analysis time; improve work efficiency; prolong the service life of the chromatographic column and reduce costs; no need for derivatization, use chromatographically pure methanol to dissolve the sample to reduce the viscosity of the sample and inject the sample directly.
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Description

technical field

[0001] The invention relates to a method for measuring the purity of 3-methylamino-1,2-propanediol, an intermediate of non-ionic contrast agent iopromide, by gas chromatography, especially to realize the purity of each of 3-methylamino-1,2-propanediol. The separation of impurity components belongs to the technical field of product instrument analysis. Background technique

[0002] 3-Methylamino-1,2-propanediol is an important raw material for the synthesis of low-osmotic non-ionic contrast agent iopromide, and its purity, quantity and content of impurities directly affect the purity and clinical application of the final product iopromide . In the synthesis reaction of iopromide, if the impurity content of 3-methylamino-1,2-propanediol is too high or the impurity components are more, it will react with the intermediate 3-(2-methoxy)acetamido]-5 -(2,3-Dihydroxy-n-propylcarbamoyl)-2,4,6-triiodobenzoyl chloride undergoes a variety of side reactions to produce a...

Claims

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