摘要
建立了LC-MS/MS法同时测定人血浆中罗氟司特(1)和活性代谢物罗氟司特N-氧化物(2)。血浆样品经叔丁基甲醚提取处理,经Phenomenex Gemini C_(18)柱(2.0 mm×100 mm,3 μm)分离,流动相为乙腈∶5 mmol/L乙酸铵缓冲液(含0.006%甲酸)(62∶38);采用电喷雾离子源(ESI),多反应监测(MRM)模式。以稳定同位素标记内标d_(4)-1和d_(4)-2分别作为1和2的内标。结果显示,1、2分别在0.040 7~15.89、0.205 8~20.58 ng/ml内线性关系良好,1、2的日内、日间精密度和准确度均符合生物样品分析的相关要求。建立的LC-MS/MS法准确、灵敏、方便,可用于1和2的人体药代动力学研究。
An LC-MS/MS method was established for the simultaneous determination of roflumilast(1) and its active metabolite roflumilast N-oxide(2) in human plasma.Plasma samples were extracted with tert-butyl methyl ether and separated on a Phenomenex Gemini C_(18) column(2.0 mm×100 mm,3 μm).The mobile phase was acetonitrile∶5 mmol/L ammonium acetate buffer containing 0.006% formic acid(62∶38).Electron spray ionization(ESI) and multiple reaction monitoring(MRM) mode were used.Stable isotope-labeled internal standards of d_(4)-1 and d_(4)-2 were used as internal standards for 1 and 2,respectively.The results showed that it was linear for 1 and 2 in the ranges of 0.040 7-15.89 and 0.205 8-20.58 ng/ml,respectively.The intra-day and inter-day precision and accuracy of 1 and 2 all met the relevant requirements for biological sample analysis.The established LC-MS/MS method is accurate,sensitive and convenient,which can be used for human pharmacokinetic studies of 1 and 2.
作者
张军
孙冰婷
戴国梁
居文政
ZHANG Jun;SUN Bingting;DAI Guoliang;JU Wenzheng(Affiliated Hospital of Nanjing University of Chinese Medicine,Nanjing 210029;Nanjing Hospital of Chinese Medicine Affiliated to Nanjing University of Chinese Medicine,Nanjing 210002)
出处
《中国医药工业杂志》
CAS
CSCD
北大核心
2022年第4期553-558,共6页
Chinese Journal of Pharmaceuticals
基金
江苏省中医药领军人才(SLJ0208)
江苏省自然科学基金面上项目(BK20211394)。
