论文部分内容阅读
目的:建立LC/MS/MS测定比格犬血浆中丁螺环酮的方法,并应用于其缓释制剂药代动力学研究。方法:血浆样品经液-液萃取,内标选用曲马多,色谱柱采用Zorbax SB-C18柱(2.1 mm×100 mm,3.5μm);流动相为甲醇-水-甲酸(40∶60∶0.1),流速0.2 ml/min;用美国Finnigan公司TSQ Quantum型液相色谱-质谱联用仪器,配有电喷雾离子化电离源(ESI),正离子检测模式,扫描方式为选择反应监测(SRM),用于定量分析的离子反应分别为m/z386.2→121.97(丁螺环酮)和m/z 264.3→58.0(内标,曲马多)。结果:测定丁螺环酮的线性范围为0.025~7.5μg/L,相关系数为0.99893,提取回收率为72.2%,方法回收率为99.1%,日内日间精密度均小于10.7%,血浆中丁螺环酮的最低定量下限为0.025μg/L。结论:该方法简便、快速、准确,灵敏度高,专一性好,成功应用于丁螺环酮缓释制剂的药代动力学研究。
OBJECTIVE: To establish a method for the determination of buspirone in beagle dogs plasma by LC / MS / MS, and to study the pharmacokinetics of sustained-release preparations. Methods: The plasma samples were separated by liquid-liquid extraction with tramadol as internal standard. The column was Zorbax SB-C18 (2.1 mm × 100 mm, 3.5 μm). The mobile phase consisted of methanol-water- ), The flow rate of 0.2 ml / min; with the United States Finnigan company TSQ Quantum liquid chromatography - mass spectrometry equipment, equipped with electrospray ionization ionization source (ESI), positive ion detection mode, scanning mode selective reaction monitoring (SRM) The ion reactions for quantitative analysis were m / z 386.2 → 121.97 (buspirone) and m / z 264.3 → 58.0 (internal standard, tramadol), respectively. Results: The linear range of buspirone was 0.025 ~ 7.5μg / L, the correlation coefficient was 0.99893, the recovery rate was 72.2%, the recovery rate was 99.1%, the intra-day and inter-day precision were less than 10.7% The lowest limit of quantitation of spiroketone is 0.025 μg / L. Conclusion: The method is simple, rapid, accurate, sensitive and specific and has been successfully applied to the pharmacokinetics of buspirone sustained-release preparation.