Gas chromatography-mass spectrometry method for determining genotoxic impurity 1, 3-dichloro-2-propanol

Abstract

The invention discloses a gas chromatography-mass spectrometry analysis method for genotoxic impurity 1, 3-dichloro-2-propanol, which comprises the following steps of: (1) pretreating a sample to prepare a sample solution, and taking perfluoropropionic acid as a derivatization reagent; and (2) detecting the sample solution by adopting a gas chromatograph-mass spectrometer so as to determine the content of the 1, 3-dichloro-2-propanol impurity in the sample. The method is good in linearity, strong in specificity, good in precision, high in accuracy and high in sensitivity, and the content of the 1, 3-dichloro-2-propanol can be rapidly and accurately measured.

Description

Technical field [0001] The present invention belongs to the field of drug analysis detection, and more particularly to a method of determining a gas chromatography spectroscopy of genetic toxic impurities 1,3-dichloro-2-propanol. Background technique [0002] Linezolid is an artificially synthetic oxazolidone antibiotic, acting on bacterial 50s ribosome subunit, inhibition of mRNA and ribosome connection, preventing the formation of the 70s start complex during the initial stage of the translation system, Thereby suppressing the synthesis of bacterial protein. In 2000, the US FDA was approved for treatment of leather. + ) Infection caused by Sococcus. Its structural formula is as follows: [0003] [0004] Intermediate body rryazole epoxy (Formula II) is used in the synthesis process of londylolide, and the starting material used in the synthesis of the intermediate is epoxyhydropane, and the preparation process of epoxyhydlorohydrin is produced. 1,3-dichloro-2-propanol. On Oct...

AI Technical Summary

Problems solved by technology

[0006] Since 1,3-dichloro-2-propanol has a low limit (15ppm) and no ultraviolet absorption, it cannot be directly detected by liquid chromatography, and it is not easy to ionize, so it can be directly detected by LC-MS or GC-MS. signal is generally poor

[0007] Domestic and international detection of 1,3-dichloro-2-propanol is mostly in the food field. The food processing method needs to add adsorbents such as diatomaceous earth, and then use column chromatography for enrichment treatment. There are many steps in sample pretreatment. , and the amount of sample used is large, and the food sample processing method is not suitable for the pretreatment of drug solutions (Zhou Xiangjuan, Xie Jingjing, Zhao Yuqi, et al. Determination of chloropropanols in soy sauce by gas chromatography-mass spectrometry[J]. Chinese seasoning Product, 2011(05):88-90.)

[0008] CN201910616208.9 discloses a detection method for residual chloropropanol compounds in ornidazole, which uses headspace gas chromatography and uses a hydrogen flame ionization detector (FID) for measurement, and the sensitivity of the instrument is relatively poor (the detection limit concentration 150ng / mL: prepare the reference substance stock solution of 7.5μg / ml, then take 0.2ml to 10ml volumetric flask to constant volume, draw the detection limit concentration to be 150ng / mL), the sample usage is relatively large and the concentration of the sample The pretreatment is relatively cumbersome (take about 1.0g of ornidazole, weigh it accurately, put in a 10mL iodine volumetric bottle, add 4.0mL of mixed solvent, namely acetone:n-hexane (1:9) and seal it, until the speed regulating oscillator is 50 times per minute Shake for 10 minutes, bath in ice water for 30 minutes, filter with 0.22 μm nylon membrane, take the filtrate after returning to room temperature as the test solution)

Images