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Method for determining content of 2-chloropropionic acid in iopanol

A technology of meclopropionic acid and iopamidol, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of low sensitivity and achieve the effects of strong specificity, high precision and good accuracy

Active Publication Date: 2020-01-14
上海明捷医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, gas chromatography and headspace gas chromatography are used to detect 2-chloropropionic acid, and the sensitivity is low

Method used

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  • Method for determining content of 2-chloropropionic acid in iopanol
  • Method for determining content of 2-chloropropionic acid in iopanol
  • Method for determining content of 2-chloropropionic acid in iopanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A method for measuring 2-chloropropionic acid content in iopamidol, comprising the steps:

[0018] S1. Prepare 2 parts of 2-chloropropionic acid reference solution in parallel:

[0019] Take 24.74 mg of 2-chloropropionic acid reference substance, use purified water as solvent, prepare 2-chloropropionic acid reference substance stock solution (1 mg / ml), and gradually dilute until the concentration of 2-chloropropionic acid reference substance solution is 69.272 nanometers g / ml, then accurately measure 1.0 ml of this solution, place it in a 20 ml headspace bottle, add 0.5 ml of sulfuric acid-ethanol (3:17) solution, seal it, and obtain reference solution 1;

[0020] Take 24.98 mg of 2-chloropropionic acid reference substance, use purified water as solvent, prepare 2-chloropropionic acid reference substance stock solution (1 mg / ml), and gradually dilute until the concentration of 2-chloropropionic acid reference substance solution is 69.994 nanometers g / ml, then accuratel...

Embodiment 2

[0027] The linear range investigation of the assay method that embodiment 1 provides

[0028] Take 24.74mg of 2-chloropropionic acid into a 25mL volumetric flask, add purified water to dissolve, adjust the volume to the mark, shake well, and use it as 2-chloropropionic acid stock solution A; precisely pipette 0.7mL of 2-chloropropionic acid stock solution A to a 10mL volumetric flask, dilute with purified water and constant volume, shake well, as 2-chloropropionic acid stock solution B; precisely pipette 0.5mL 2-chloropropionic acid stock solution B into a 50mL volumetric flask, add purified water to dilute and Constant volume, shake well, as 2-chloropropionic acid stock solution C;

[0029] L-200 (0.1377μg / mL): Accurately measure 2.0mL of 2-chloropropionic acid stock solution C into a 10mL measuring bottle, dilute to the mark with diluent, and shake well. Accurately measure 1.0mL from the above solution and place it in a 20mL headspace bottle, add 0.5mL sulfuric acid-ethanol...

Embodiment 3

[0034] The sample addition recovery test of the assay method that embodiment 1 provides

[0035] Through the method of sample addition and recovery, analyze the accuracy of the determination method provided in Implementation 1, take 100 mg of the raw material drug, weigh it accurately, place it in a 20 mL headspace bottle, and make 11 copies in parallel, take 2 of them, add 1.0 mL for purification water, add 0.5mL sulfuric acid-ethanol (3:17) solution, seal, and measure the 2-chloropropionic acid content in the sample to be tested; get 3 parts, add 1mL L-50 respectively, add 0.5mL sulfuric acid-ethanol (3 :17) solution, sealed, as 50% recovery rate of standard addition solution; 3 parts were taken, respectively added 1mL L-100, and 0.5mL sulfuric acid-ethanol (3:17) solution, sealed, as 100% recovery rate of standard addition Solution: get 3 parts wherein, add 1mL L-150 respectively, add 0.5mL sulfuric acid-ethanol (3:17) solution, seal, as 150% standard addition recovery rate...

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Abstract

The invention provides a method for determining the content of 2-chloropropionic acid in iopalol. S1, taking a reference solution of 2-chloropropionic acid, and using water and acid-ethanol (3:17) solution as a solvent, the 2-chloropropane acid reference solution as a reference solution is prepared; and taking the drug substance, and using water and acid-ethanol (3:17) solution as a solvent, the sample test solution is prepared; S2, two parts of 2-chloropropionic acid reference solution are prepared in parallel, and the peak areas of 2-chloropropionic acid in the two reference solutions are obtained respectively by HS-GC-MS detection method; S3, the peak area of 2-chloropropionic acid in the sample test solution is obtained by HS-GC-MS detection method, and the content of 2-chloropropionicacid in the sample test solution is calculated by external standard method. The invention has the advantages of short detection time, strong specificity, good accuracy, high precision and good repeatability.

Description

technical field [0001] The invention belongs to the technical field of drug detection, and relates to a method for determining the content of 2-chloropropionic acid in iopamidol. Background technique [0002] 2-chloropropionic acid is mainly used in the production of pesticides and herbicides. It is also used in the production of lactic acid and lower alcohol esters with industrial value. Colorless liquid with special odor. Miscible with water, soluble in ether, acetone, benzene, carbon tetrachloride, toxic, corrosive, harmful to skin contact and swallowed, causing severe burns. Iopamidol is a non-ionic water-soluble contrast agent. Due to its high iodine content, it is X-ray attenuation to achieve the purpose of contrast imaging. It is suitable for X-ray contrast for intravascular injection. Clinically, Iopamidol is used For various angiography, such as cerebral angiography, cardiovascular angiography and so on. However, the detection of 2-chloropropionic acid by gas ch...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/32G01N30/72
CPCG01N30/02G01N30/06G01N30/30G01N30/32G01N30/72G01N2030/324
Inventor 邓惠娟朱子丰顾凯
Owner 上海明捷医药科技有限公司
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