高坤,陈凤菊,孙进,何仲贵
GAO Kun,CHEN Feng-ju,SUN Jin,HE Zhong-gui (School of Pharmacy

• 1:沈阳药科大学药学院
• 2:沈阳药科大学药学院
• 3:沈阳药科大学药学院
• 4:沈阳药科大学药学院 辽宁沈阳110016

摘要(Abstract)：

目的建立大鼠血浆中多西他赛含量的测定方法,为药物动力学研究提供方法学基础。方法采用高效液相色谱-质谱联用法(HPLC-MS)。采用Diamonsil C18色谱柱(4.6 mm×200 mm,5μm),乙腈-质量分数为0.2%的甲酸水溶液(体积比66∶34)为流动相,流速为1.0 mL.min-1,柱温为25℃,进样量为20μL。质谱选择电喷雾电离源(ESI),选择离子监测(SRM)检测多西他赛母离子[M+H]+m/z809,内标格列吡嗪子离子m/z321。结果本法的线性范围为25~4 000μg.L-1;最低定量限为12.5μg.L-1;低、中、高质量浓度质控供试品的日内RSD均在4.09%~6.96%内,日间RSD均在5.34%~14.29%内,准确度相对误差(ER)均在-0.29%~-3.42%内,提取回收率均在85%以上。结论本法操作简便,灵敏度高,分析速度快,适用于大鼠血浆中多西他赛的含量测定。
Objective To establish a high-performance liquid chromatography-electrospray mass spectrometry(HPLC-MS) method for the determination of docetaxel in rat plasma.Methods The HPLC-MS method was performed on Diamonsil C18 column(4.6 mm×200 mm,5 μm) at 25 ℃,taking acetonitrile-0.2% formic acid(V∶V=66∶4) as mobile phase with flow rate of 1.0 mL·min-1;the injection volume was 20 μL.Acquisition was performed with the selected ion reaction monitoring mode(SRM) after the ionization in the electrospray ionization source.The parent ion+ m/z 809 and product ion m/z 321 were used for quantification analysis of docetaxel and internal standard glipizide,respectively.Results The method was linear over the range of 25-4 000 μg·L-1;the limit of quantification was 12.5 μg·L-1.The intra-day and inter-day precision(RSD) ranged form 4.09% to 6.96% and 5.34% to 14.29%,respectively;the accuracy(ER) ranged from-0.29% to-3.42%,and the extraction recovery was above 85% for the low,middle and high concentrations of check samples,respectively.Conclusions The developed method is simple,sensitive and fast.It can be applied to determine the content of docetaxel in rat plasma.

关键词(KeyWords)： 多西他赛;高效液相色谱-质谱联用法;含量测定
doctaxel;high-performance liquid chromatography-electrospray mass spectrometry;content determination

Abstract:

Keywords:

基金项目(Foundation): 辽宁省科技计划项目(2007102071)

作者(Author): 高坤,陈凤菊,孙进,何仲贵
GAO Kun,CHEN Feng-ju,SUN Jin,HE Zhong-gui (School of Pharmacy

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