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反相高效液相色谱法测定农药中间体3-二氟甲基-1-甲基-1H-吡唑-4-甲酸及其主要杂质的含量
引用本文:施力玮.反相高效液相色谱法测定农药中间体3-二氟甲基-1-甲基-1H-吡唑-4-甲酸及其主要杂质的含量[J].化学世界,2022,63(1):30-34.
作者姓名:施力玮
作者单位:上海格瑞产品检测有限公司,上海201210
摘    要:建立了反相高效液相色谱法测定农药中间体3-二氟甲基-1-甲基-1H-吡唑-4-甲酸和3-二氟甲基-1-甲基-1H-吡唑-4-羧酸酯含量方法.甲醇和20 mmol/L乙酸铵(pH 5.0)为流动相,采用HC-C18色谱柱,在波长240 nm处检测.该方法在12.387~1238.7 mg/L 3-二氟甲基-1-甲基-1H...

关 键 词:反相高效液相色谱法  农药中间体  3-二氟甲基-1-甲基-1H-吡唑-4-甲酸  3-二氟甲基-1-甲基-1H-吡唑-4-羧酸酯

Determination of 3-(Difluoromethyl)-1-methyl-1H-4-carboxylate and Its Impurities in Pesticide Intermediate by Reversed Phase High Performance Liquid Chromatography
Shi Liwei.Determination of 3-(Difluoromethyl)-1-methyl-1H-4-carboxylate and Its Impurities in Pesticide Intermediate by Reversed Phase High Performance Liquid Chromatography[J].Chemical World,2022,63(1):30-34.
Authors:Shi Liwei
Affiliation:(Shanghai Gerui Products Testing Company Limited,Shanghai 201210,China)
Abstract:A testing method for the quantitative determination of 3-(difluoromethyl)-1-methyl-1H-4-carboxylate and ethyl-3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate, which are important pesticide intermediates, by reversed phase high performance liquid chromatography with methanol and ammonium acetate(20 mmol/L, pH = 5.0) solution as mobile phase, HC-C18 column and UV detection at 240 nm, was established. This method has a good linear relationship at range of 12.387~1238.7 mg/L for 3-(difluoromethyl)-1-methyl-1H-4-carboxylate and 4.29~214.5 mg/L for ethyl-3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate correlation coefficient(r2)>0.999]. The recoveries are 98.84%~100.23% for 3-(difluoromethyl)-1-methyl-1H-4-carboxylate and 98.04%~100.37% for ethyl-3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate.
Keywords:reversed phase high performance liquid chromatography  pesticide intermediates  3-(difluoromethyl)-1-methyl-1H-4-carboxylate  ethyl-3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate
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