固相萃取-液相色谱-串联质谱法快速分析血浆中特布他林  

RAPID ANALYSIS OF TERBUTALINE BY COMBINED SOLID PHASE EXTRACTION/LIQUID CHROMATOGRAPHY TANDEM MASS SPECTROMETRY

作　　者：陈笑艳[1] 杨汉煜[1] 钟大放[1] 徐海燕[1] 张逸凡[1] 

机构地区：[1]沈阳药科大学药物代谢与药物动力学实验室,辽宁沈阳110016

出　　处：《药学学报》2001年第9期686-689,共4页Acta Pharmaceutica Sinica

基　　金：国家自然科学基金资助项目 ( 39930 180 )

摘　　要：目的　建立快速、高灵敏度 (5 0pg·mL- 1 )分析血浆中特布他林浓度的液相色谱 串联质谱法。方法　以沙丁胺醇为内标 ,血浆样品经固相萃取后 ,进行色谱分离 ,电喷雾离子化四极串联质谱检测 ,采用选择离子反应监测(SRM)方式进行定量分析 ,用于监测的离子为m z 2 2 6→ 15 1(特布他林 )和m z 2 40→ 148(沙丁胺醇 ,内标 )。结果　特布他林的线性范围为 0 0 5 - 8 0ng·mL- 1 ;以质控样品 (0 1,0 4和 4 0ng·mL- 1 )计算 ,该法的批间精密度 (RSD)为2 5 % - 7 1% ,准确度 (RE)为 - 3 1% - 5 7% ;批内精密度为 4 2 % - 6 6 % ;每个样品测试时间仅 3 8min。结论　该法操作简便、快速 ,灵敏度高于文献报道的结果 ,可检测出受试者单剂量口服 10mg盐酸班布特罗 6 0h后特布他林的血浆浓度 ,适用于临床药物动力学研究。AIM To develop a liquid chromatography-electrospray ionization tandem mass spectrometry method for rapid analysis of terbutaline at level of 50 pg·mL -1 in human plasma. METHODS Samples containing terbutaline and salbutamol (internal standard, IS) were extracted using C 18 solid-phase extraction cartridges, followed by liquid chromatographic separation and mass spectrometric detection. The mobile phase consisted of acetonitrile-water-formic acid (20∶80∶1), at a flow-rate of 0 4 mL·min -1 . Selected reaction monitoring with mass transitions m/z 226→151 and m/z 240→148 were used for terbutaline and IS, respectively. RESULTS The chromatographic analysis time for each sample was approximately 3 8 min. The assay was linear from 0 05 to 8 0 ng·mL -1 . The between-run precision and accuracy of the quality controls (QCs, 0 1, 0 4 and 4 0 ng·mL -1 ) were characterized by relative standard deviation (RSD) of 2 5% to 7 1% and relative errors of -3 1% to 5 7%, respectively. The within-run precision of QCs was characterized by RSD of 4 2% to 6 6%. This method was applied to the analysis of samples taken up to 60 h after oral administration of 10 mg bambuterol in healthy volunteers. CONCLUSION The method is shown to be suitable for clinical investigation of terbutaline pharmacokinetics, which offers advantages of specificity, speed, and greater sensitivity over previously reported methods.

关 键 词：特布他林 液相色谱-质谱-质谱联用法 血药浓度 支气管平滑肌松驰作用 

分 类 号：R974[医药卫生—药品] R969.1[医药卫生—药学]