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

A technology of gas chromatography-mass spectrometry and detection method, which is applied in the field of gas chromatography-mass spectrometry for the determination of genotoxic impurity 1,3-dichloro-2-propanol, which can solve the problems of cumbersome pretreatment, difficult ionization, and large sample usage and other problems, to achieve the effect of good linear relationship, ensuring the safety of medication, and less pretreatment steps

Inactive Publication Date: 2022-01-28
ZHEJIANG HISUN PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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 chlor

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Example 1: Positioning Experiment

[0062] Virtue: SH-RXI-5SIL MS, 30m * 250μm, 0.25μm; carrier gas: high purity helium; carrier gas flow rate: 1.2ml / min, diversion ratio is 5: 1, inventive amount: 1.0μL , Inlet temperature: 250 ° C, the program is raised: 60 ° C is maintained at 20 ° C to 120 ° C, and then heated to 240 ° C at 40 ° C / min to keep 2 min.

[0063] Mass spectrometry: ionization source is EI source, ion source temperature: 230 ° C, analyzer: single four rod quality analyzer, full sweep range is 20 ~ 400, solvent delay: 3 min.

[0064] Diluent: n-heptane

[0065] Reserve reserve A: Precision 1,3-dichloro-2-propanol Rejection 30mg to 100 mL volumetric flask, add diluent to the scale, mix; precisely remove the above solution 1.0ml The 10ml volumetric flask was diluted with a diluent to the scale, mixed, and the concentration of 30 μg / ml of the reserve reserve A was obtained.

[0066] Reparative solution: Removal of concentrated sulfuric acid solution (100 μL...

Embodiment 2

[0067] Example 2: Methodology

[0068] Vectors: SH-RXI-5SIL MS, 30M * 250μm, 0.25μm; carrier gas: high purity helium; carrier gas flow rate: 1.2ml / min, diversion ratio is 3: 1, inventive amount: 1.0μL The temperature of the inlet temperature: 250 ° C, using the program temperature rise: 60 ° C for 2 min, at 20 ° C to 100 ° C for 2 min, and then warmed up to 240 ° C for 2 min at 40 ° C / min.

[0069] Mass spectrometry: ionization source is EI source, ion source temperature: 230 ° C, analyzer: single four-stage rod quality analyzer, monitoring mode is selected from ion monitoring mode (SIM), extract ions 110, 225, solvent delay: 3 min.

[0070] Diluent: n-heptane.

[0071] Reservoir reserve B: Precision 1,3-dichloro-2-propanol Rejection 30mg to 100 mL volumetric flask, add diluent to the scale, mix; precisely remove the above solution 1.0ml The 50ml volumetric flask was diluted with a diluent to the scale, mixed, gave a concentration of 6.0 μg / ml reserve reserve b.

[0072] Lin...

Embodiment 3

[0085] Example 3: Sample detection

[0086] Vectors: SH-RXI-5SIL MS, 30M * 250μm, 0.25μm; carrier gas: high purity helium; carrier gas flow rate: 1.2ml / min, diversion ratio is 3: 1, intraday flow rate 1.0μL, Input temperature: 250 ° C, the primection temperature: 60 ° C is maintained at 20 ° C to warm to 100 ° C for 2 min, and then warmed to 240 ° C for 2 min at 40 ° C / min.

[0087]Mass spectrometry: ionization source is EI source, ion source temperature: 230 ° C, analyzer: single four-stage rod quality analyzer, monitoring mode is selected from ion monitoring mode (SIM), extract ions 110, 225, solvent delay: 3 min.

[0088] Sample solution formulated: 20 mg of a total of 20 ml of a plug-in glass tube is weighed, respectively, 20% sulfuric acid solution (100 μl) + n-heptane (100 μl) + perfluorionic acid (100 μl) ), Water (5 mL), n-heptane (0.9 mL) was added, and the orthopedane (0.9 mL) was added, and the orthodium heptane (0.9 mL) was added, and the layered sample solution wa...

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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...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/72C07C67/08C07C69/63
CPCG01N30/02G01N30/06G01N30/7206C07C67/08G01N2030/067C07C69/63
Inventor 麻新华周贝贝陈延安金美春
Owner ZHEJIANG HISUN PHARMA CO LTD
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