托西酸舒他西林中对甲基苯磺酸烷基酯检查方法研究  

Study on the determination of p-toluenesulfonic acid alkyl ester in sultamicillin tosilate

作　　者：姚兰 傅蓉 邹宇 孙苓苓 Yao Lan;Fu Rong;Zou Yu;Sun Lingling(Liaoning Institute for Drug Control,Shenyang 110032)

机构地区：[1]辽宁省药品检验检测院,沈阳110032

出　　处：《中国抗生素杂志》2023年第12期1362-1372,共11页Chinese Journal of Antibiotics

摘　　要：目的对工艺中可能产生的对甲基苯磺酸烷基酯建立气相色谱-三重四极杆质谱联用的测定方法。方法以(5%-苯基)-甲基聚硅氧烷为固定液的弹性石英毛细管柱为色谱柱;进样口温度为200℃,程序升温,起始温度50℃,维持1 min,以每分钟10℃升温至300℃;进样体积1μL。以三重四极杆串联质谱仪检测;离子源为电子轰击源(EI),质谱监测模式为多反应监测(MRM)。结果经方法学验证,混合对照品溶液各峰分离良好,对甲基苯磺酸甲酯、乙酯、异丙酯分别在0.002485~0.1863μg/mL、0.002019~0.1514μg/mL、0.001879~0.1409μg/mL浓度范围内线性关系良好,在0.05~0.15μg/mL浓度范围内回收率为94.5%~113.7%,方法检出灵敏度低于1%TTC。结论该方法准确可靠,适用于托西酸舒他西林中对甲基苯磺酸烷基酯的测定。按该方法形成质量标准草案,并采用拟修订方法对生产企业提供的6批样品进行测定,6批样品均符合规定。Objective A gas chromatography-triple quadrupole mass spectrometry(GC-MSMS)method was developed for the determination of alkyl p-toluenesulfonate.Method An elastic quartz capillary column with(5%-phenyl)-methylpolysiloxane as stationary liquid was used as the chromatographic column.The inlet temperature is 200℃.The column temperature was programmed.The starting temperature was set at 50℃ for 1 minute,then the temperature was increased to 300℃ at a rate of 10℃ per minute;the injection volume was 1μL.The Electron Ionization source(EI)was used as the ion source,the monitoring mode was multiple reaction monitoring(MRM).Result The results showed that the peak area of methyl p-toluenesulfonate,ethyl p-toluenesulfonate,isopropyl p-toluenesulfonate had a good linear relationship in the concentration range of 0.002485~0.1863μg/mL,0.002019~0.1514μg/mL and 0.001879~0.1409μg/mL,respectively.The recovery rates were 94.5%~113.7% in the range of 0.05~0.15μg/mL,respectively.The detection sensitivity concentration was less than 1%TTC.Conclusion The method was accurate and reliable.According to this method,a draft of quality standard was formed,6 batches of samples were determined by the proposed method.All 6 batches of samples met the requirements.

关 键 词：托西酸舒他西林 对甲基苯磺酸甲酯 对甲基苯磺酸乙酯 对甲基苯磺酸异丙酯 气相色谱-三重四极杆质谱联用 

分 类 号：R917[医药卫生—药物分析学]