Method for detecting chloroethanol in pharmaceutic adjuvant
A technology of pharmaceutical excipients and detection methods, which is applied in the direction of measuring devices, material separation, and analytical materials, etc., can solve the problem that the separation between the test object and the test product cannot meet the requirements, it is difficult to ensure the detection accuracy and sensitivity, and residues, etc. question
Active Publication Date: 2022-03-25
广东国标医药科技有限公司
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Problems solved by technology
[0003] 2-Chloroethanol is often used as an organic solvent, or in the preparation of ethylene oxide, synthetic medicine and pesticides, etc., so it is easy to cause residues in pharmaceutical products
At the same time, 2-chloroethanol is highly toxic, and its concentration monitoring as a genotoxic impurity in the drug must be strictly controlled
[0004] At present, in the detection method of chloroethanol reported in the literature, the selected solvent is more difficult to take into account the chemical characteristics of the test article and the test substance, resulting in poor solubility of the test article, the test substance cannot be completely released into the solution system, and the test substance The degree of separation from the test product cannot meet the requirements, and it is difficult to guarantee the accuracy and sensitivity of the test
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[0027] This example provides a method for detecting chlorohydrin in pharmaceutical excipients, and the operation steps are as follows: 1. Gas chromatography conditions: chromatographic column: VF-WAXms (30m×0.25mm×0.25μm); inlet temperature: 220°C; Flow rate: 1.0ml / min; Injection volume: 1μL; Control mode: Constant flow; Injection mode: Split flow, split ratio 5:1; Carrier gas: He; The heating rate was increased to 140 °C at a rate of °C / min, and then raised to 240 °C at a rate of 80 °C / min and kept for 2 min.
[0028] 2. Mass spectrometry parameter conditions: acquisition type: MRM; ion source: EI; solvent delay: 3min; transfer line temperature: 240°C; quadrupole MS1 temperature: 150°C; quadrupole MS2 temperature: 150°C; ion source temperature: 250 ℃; quantitative ion pair 79 / 43, qualitative ion pair 80 / 44.
[0029] 3. Preparation of reference substance solution: Accurately weigh about 10 mg of 2-chloroethanol reference substance, put it in a 10ml volumetric flask, add ultra...
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Abstract
The invention belongs to the technical field of pharmaceutical analysis. The invention provides a method for detecting chloroethanol in pharmaceutical excipients, which comprises the following steps: respectively dissolving a test sample and a reference substance with ultrapure water, and extracting with ethyl acetate to respectively obtain a test sample solution and a reference substance solution; respectively injecting the test solution and the reference solution into a gas chromatograph-mass spectrometer for analysis, and calculating the content of chloroethanol in the solutions by adopting a standard curve method. According to the detection method, methodological evaluation is carried out on the applicability, specificity, linearity and range, detection limit and quantitation limit, precision, accuracy and stability of the method system, the results all meet the requirements, and the detection method can be used for monitoring the content of chloroethanol in the pharmaceutic adjuvants.
Description
technical field [0001] The application belongs to the technical field of pharmaceutical analysis, in particular to a method for detecting chlorohydrin in pharmaceutical excipients. Background technique [0002] Hydroxyethyl cellulose is a kind of non-ionic soluble cellulose ether compound, which can be used as a medicine due to its good properties of thickening, suspending, dispersing, emulsifying, binding, film forming, protecting moisture and providing protective colloid. Excipients are widely used in the field of medicine and food. [0003] 2-Chloroethanol is often used as an organic solvent, or to prepare ethylene oxide, synthesize medicines and pesticides, etc., so it is easy to cause residues in pharmaceutical products. At the same time, 2-chloroethanol is highly toxic, and its concentration monitoring as a genotoxic impurity in the drug must be strictly controlled. [0004] At present, in the detection method of chloroethanol reported in the literature, the selected...
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IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/30G01N30/7206G01N30/8675G01N2030/047
Inventor 陈亿展黄军建陈新国张秋丽周颖虹麦华凤郑传奇蒋杰
Owner 广东国标医药科技有限公司