Method for detecting residual dimethyl sulfate in medicine by liquid chromatography-mass spectrometry

A technology of dimethyl sulfate and LC/MS, applied in measurement devices, instruments, scientific instruments, etc., can solve problems such as residual excess dimethyl sulfate, achieve good peak shape, improve safety performance, and avoid hydrolysis.

Inactive Publication Date: 2021-06-08
ZUNYI NO 1 PEOPLES HOSPITAL
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  • Abstract
  • Description
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Problems solved by technology

[0005] Aiming at the deficiencies in the prior art, the invention provides a method for detecting residual dimethyl sulfate in medicines by liquid chromatography-mass spectrometry, mainly to solve the problem of excessive residual dimethyl sulfate in medicines

Method used

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  • Method for detecting residual dimethyl sulfate in medicine by liquid chromatography-mass spectrometry

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Effect test

Embodiment 1

[0032] refer to figure 1 , a method for liquid chromatographic detection of dimethyl sulfate residues in medicines, comprising the following steps:

[0033] S1: Prepare the derivatization solution, take 15 mg of dimethyl fumarate powder, use the acetonitrile solution containing secondary amine as the derivatizer to prepare the sample derivation solution, the mass ratio of dimethyl malate to acetonitrile solution is 1:2, select Chromatography-grade acetonitrile solvent can accurately detect dimethyl sulfate for derivatization reaction, so that the detected ion peak has good peak shape, large molecular weight, and no other debris peaks, which is convenient for testing personnel to observe and compare the testing results.

[0034] S2: prepare a blank solution, weigh the derivative solution in S1, the volume is 30 mg, add deionized water to dilute to obtain a blank solution;

[0035] S3: Prepare a control stock solution, dissolve and dilute the reference substance dimethyl sulfat...

Embodiment 2

[0042] refer to figure 1 , a method for liquid chromatographic detection of dimethyl sulfate residues in medicines, comprising the following steps:

[0043] S1: Prepare a derivatization solution, take 20 mg of dimethyl fumarate powder, and use acetonitrile solution containing secondary amines as a derivatizer to prepare a sample derivation solution. The mass ratio of dimethyl malate to acetonitrile solution is 2:5. Chromatography-grade acetonitrile solvent can accurately detect dimethyl sulfate for derivatization reaction, so that the detected ion peak has good peak shape, large molecular weight, and no other debris peaks, which is convenient for testing personnel to observe and compare the testing results.

[0044] S2: prepare a blank solution, weigh the derivative solution in S1, the volume is 50 mg, add deionized water to dilute to obtain a blank solution;

[0045]S3: Prepare a control stock solution, dissolve and dilute the reference substance dimethyl sulfate in acetone ...

Embodiment 3

[0052] refer to figure 1 , a method for liquid chromatographic detection of dimethyl sulfate residues in medicines, comprising the following steps:

[0053] S1: Prepare the derivatization solution, take 28 mg of dimethyl fumarate powder, and use the acetonitrile solution containing secondary amine as the derivatizer to prepare the sample derivation solution. The mass ratio of dimethyl malate to acetonitrile solution is 3:7. Chromatography-grade acetonitrile solvent can accurately detect dimethyl sulfate for derivatization reaction, so that the detected ion peak has good peak shape, large molecular weight, and no other debris peaks, which is convenient for testing personnel to observe and compare the testing results.

[0054] S2: prepare a blank solution, weigh the derivative solution in S1, the volume is 75 mg, add deionized water to dilute to obtain a blank solution;

[0055] S3: Prepare a control stock solution, dissolve and dilute the reference substance dimethyl sulfate i...

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Abstract

The invention relates to the technical field of dimethyl sulfate detection, and discloses a method for detecting dimethyl sulfate residues in a medicine by liquid chromatography-mass spectrometry, which comprises the following steps: S1, preparing a derivative solution, taking 10-30mg of dimethyl fumarate powder, and preparing a sample derivative solution by using a secondary amine-containing acetonitrile solution as a derivative agent, wherein the mass ratio of the dimethyl fumarate to the acetonitrile solution is (1-5):(2-8); S2, preparing a blank solution, weighing the derivative solution in the step S1 with the volume of 20-80 mg, and adding deionized water for dilution to obtain the blank solution; and S3, preparing a control stock solution. According to the method, dimethyl sulfate is accurately detected through the derivatization reaction of the acetonitrile solvent, so that the detected ion peak is good in peak shape, detection personnel can conveniently observe and compare the detection result, and meanwhile, a worker can conveniently compare data obtained through the reaction by preparing the reference substance solution and the to-be-detected solution, and therefore, the detected data is more persuasive.

Description

technical field [0001] The invention relates to the technical field of detection of dimethyl sulfate, in particular to a method for detecting residues of dimethyl sulfate in medicines by liquid chromatography-mass spectrometry. Background technique [0002] Liquid chromatography-mass spectrometry (HPLC-MS) is also called liquid chromatography-mass spectrometry technology. It uses liquid chromatography as the separation system and mass spectrometry as the detection system. The sample is separated from the mobile phase in the mass spectrometer part. The mass analyzer separates the ion fragments according to the mass number, and the mass spectrum is obtained through the detector. The liquid chromatography-mass spectrometry reflects the complementary advantages of chromatography and mass spectrometry. The high separation ability of chromatography for complex samples, and MS have high selectivity and high Combined with the advantages of sensitivity and the ability to provide rela...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/7266G01N30/8675
Inventor 王远敏
Owner ZUNYI NO 1 PEOPLES HOSPITAL
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