Gas chromatgraphy-mass spectrometry detection method of residual chloromethyl methyl ether in crude drug

A technology of gas chromatography-mass spectrometry and chloromethyl methyl ether, which is applied in the field of gas chromatography-mass spectrometry detection of chloromethyl methyl ether residues in raw materials, can solve the problems of time-consuming, low precision and accuracy of quantitative analysis, production The sample process is cumbersome and other issues

Active Publication Date: 2018-02-13
上海药明康德新药开发有限公司
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  • Application Information

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Problems solved by technology

The inventor measured the residue of chloromethyl methyl ether in the crude drug according to this method, and found that the sample

Method used

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  • Gas chromatgraphy-mass spectrometry detection method of residual chloromethyl methyl ether in crude drug
  • Gas chromatgraphy-mass spectrometry detection method of residual chloromethyl methyl ether in crude drug
  • Gas chromatgraphy-mass spectrometry detection method of residual chloromethyl methyl ether in crude drug

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Embodiment 1

[0031] The specificity research of chloromethyl methyl ether residual determination in embodiment 1 crude drug:

[0032] Precisely weigh about 100mg of chloromethyl methyl ether (CMME) into a 100mL volumetric flask containing about 10mL of dichloromethane, dilute to the mark with dichloromethane, shake well, and mark it as CMME-DCM solution. Chloromethyl methyl ether is stable in dichloromethane.

[0033] Precisely weigh about 100mg of chloromethyl methyl ether into a 100mL volumetric flask containing about 10mL of isopropanol, dilute to the mark with isopropanol, shake well, and mark it as CMME-IPA solution. Chloromethyl methyl ether reacts with isopropanol in isopropanol solution, and the reaction is as follows:

[0034]

[0035] Carry out GC-MS analysis to CMME-DCM solution and CMME-IPA solution respectively, method condition:

[0036] The chromatographic column adopts DB-624 capillary gas chromatography column, the chromatographic column length is 30m, the inner diame...

Embodiment 2

[0045] Sensitivity, precision, linearity, accuracy and stability research of chloromethyl methyl ether residual determination in embodiment 2 crude drug:

[0046] Accurately weigh about 100mg of chloromethyl methyl ether into a 100mL volumetric flask containing about 10mL of isopropanol, dilute to the mark with isopropanol and shake well, accurately pipette 0.6mL of the solution into a 100mL volumetric flask, Dilute the volume of propanol to the mark, shake well, and mark it as the reference substance stock solution.

[0047] GC-MS analysis method conditions:

[0048] The chromatographic column adopts DB-624 capillary gas chromatography column, the chromatographic column length is 30m, the inner diameter is 0.32mm, and the film thickness is 1.8μm. ;

[0049] Helium was used as the carrier gas, and the carrier gas flow rate was 1.5mL / min;

[0050] Direct injection was adopted, the injection volume was 1 μL, and the temperature of the injection port was 200°C;

[0051] Using...

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Abstract

The invention discloses a gas chromatgraphy-mass spectrometry detection method of residual chloromethyl methyl ether in a crude drug. Alcohol is adopted as a solvent and a derivatization reagent, a capillary gas chromatography column, direct sample introduction and temperature programming are adopted, and a mass spectrometry detector is further adopted for detection. The method can effectively detect chloromethyl methyl ether in the crude drug; a spectrogram baseline is stable and free from drift; a sample treatment process of the method is simple, convenient and quick; alcohol serves as the solvent and the derivatization reagent at the same time; a derivatization reaction is mild, quick and complete. The method greatly simplifies a sample preparation process, avoids interference of a complicated derivatization reagent with detection and improves detection precision and accuracy; the method is used for determining residual chloromethyl methyl ether in the crude drug, has a good linearrelationship, high precision, high accuracy and high sensitivity and has an important research value in aspects such as crude drug quality research, and impurity analysis and control research.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a gas chromatography-mass spectrometry (GC-MS) detection method for residual chloromethyl methyl ether in raw materials. Background technique [0002] A pharmaceutical impurity is an active pharmaceutical ingredient (API, API) or a chemical component that is undesirably present in a pharmaceutical formulation. Impurities in APIs may originate from the synthesis process or starting materials, intermediates, solvents, catalysts, reaction by-products, instability of API components, incompatibility with excipients, or reactions with packaging materials, etc. Various impurities in the drug have a great impact on the safety of the final drug. Among them, genotoxic impurity (Genotoxic Impurity, GTI) means that the compound itself directly damages cell DNA, produces gene mutation or mutagenesis in vivo, and has the possibility or tendency to cause cancer. Its characteristic is th...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 樊华军陈斌涂继辉刘振钱晓暐
Owner 上海药明康德新药开发有限公司
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