Method for detecting content of dimethyl sulfate in sulfamethoxazole bulk drug
A technology of dimethyl sulfate and sulfamethoxazole, which is applied in the field of detection of dimethyl sulfate content in sulfamethoxazole raw materials, can solve the problems of high equipment requirements, complicated operation, low sensitivity, etc., and achieve specificity Strong, simple operation, high sensitivity effect
Pending Publication Date: 2021-11-12
YICHANG HUMANWELL PHARMA
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Problems solved by technology
Conventional detection methods are mostly derivatization with dimethyl sulfate and derivatization reagents, and then detect the reaction products, but the derivatization time is long, the operation is complicated, the requirements for equipment are high, and it is not easy to reproduce
And routine method such as liquid chromatography, gas chromatography method can't meet the detection sensitivity requirement of dimethyl sulfate in the sulfamethoxazole raw material
Chinese patent 202010533342.5 discloses a method for determining the content of dimethyl sulfate in clopidogrel bisulfate by using GC-MS analysis method Researchers found that the content of dimethyl sulfate in sulfamethoxazole could not be detected by using this method , and the sensitivity of the method is also low
[0007] At present, no analytical method for the determination of dimethyl sulfate in sulfamethoxazole has been reported, so it is necessary to establish a set of simple, rapid and sensitive analytical methods for the determination of potential genotoxic impurity sulfuric acid in sulfamethoxazole raw materials. Dimethyl ester content
Method used
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Embodiment 1
[0143] 1. Instrument: Agilent 7890B-5977B gas chromatography mass spectrometry;
[0144] 2. Chromatography and mass spectrometry conditions:
[0145] 1) Chromatographic column: Agilent CP8944, VF-5ms (30m×0.25mm×0.25μm), the initial temperature is 50°C, keep for 4min, raise the temperature to 200°C at a rate of 30°C / min, and keep for 6min;
[0146] 2) Inlet temperature: 200°C;
[0147] 3) Carrier gas: high-purity helium, the flow rate is 1.0mL / min, and the split ratio is 10:l;
[0148] 4) Transfer line temperature and injection volume: the transfer line temperature is 230°C, and the injection volume is 1 μL;
[0149] 5) The ion source temperature is 200°C; the quadrupole temperature is 150°C.
[0150] 3. Solution preparation
[0151] (1) Reference substance stock solution: Accurately weigh 31.9mg of dimethyl sulfate, place in a 20mL volumetric flask, dissolve and dilute to the mark with ethyl acetate, shake well; then accurately measure 1mL of the solution, place in a 100m...
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Abstract
The invention provides a method for detecting the content of dimethyl sulfate in a sulfamethoxazole bulk drug, the method comprises the following steps: A) mixing the sulfamethoxazole bulk drug with ammonia water, adding a solvent for extraction, and taking supernate to obtain a test solution; mixing a reference substance dimethyl sulfate with ammonia water, adding a solvent for extraction, and taking supernate to obtain a reference substance solution; b) respectively measuring the test solution and the reference solution by adopting a gas chromatography-mass spectrometry method, and quantifying by adopting an external standard method; detection conditions are as follows: a chromatographic column is a capillary column and a gas chromatographic column; the carrier gas is helium; a split-flow sampling mode is adopted; the temperature rising procedure: keeping the initial column temperature at 50-70 DEG C for 4 minutes, raising the temperature to 200 DEG C at the rate of 30 DEG C / min, and keeping the temperature for 6 minutes; the invention provides the method for detecting the content of dimethyl sulfate in the sulfamethoxazole bulk drug, which is simple and rapid to operate, high in sensitivity, strong in specificity and good in repeatability.
Description
technical field [0001] The invention relates to the technical field of drug analysis, in particular to a method for detecting the content of dimethyl sulfate in sulfamethoxazole bulk drug. Background technique [0002] Sulfamethoxazole, the chemical name is 4-amino-N-(5-methyl-3-isoxazolyl)-benzenesulfonamide; the CAS number is 723-46-6; the molecular formula is C 10 h 11 N 3 o 3 S; the structural formula is as follows: [0003] [0004] The trade name of sulfamethoxazole is Sinomine, which is a broad-spectrum antibiotic. It has inhibitory effect on most Gram-positive and Gram-negative bacteria. Cotrimoxazole formed with trimethoprim has been recommended by the World Health Organization (WHO) and the United Nations Program on AIDS (UNAIDS) for standard medical services for HIV-infected and AIDS patients. In addition, compound sulfamethoxazole not only has a good therapeutic and preventive effect on Pneumocystis pneumonia (PCP), but also has a good effect on othe...
Claims
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IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/04G01N30/30G01N30/16G01N30/60G01N30/86G01N30/88
CPCG01N30/02G01N30/06G01N30/72G01N30/04G01N30/30G01N30/16G01N30/60G01N30/8634G01N30/88G01N2030/062G01N2030/047G01N2030/884
Inventor 李小聪廖宗权孙净王敏易斌熊俊李莉娥吕金良汪淼
Owner YICHANG HUMANWELL PHARMA