论文部分内容阅读
目的:建立小鼠血浆和组织样品中多西他赛的含量测定方法。方法:选择紫杉醇为内标物,进样前用甲基叔丁基醚萃取,Hypersil BDS C_(18)色谱柱(2.1 mm×50 mm,2.4μm),流动相甲醇-0.1%甲酸(80∶20),柱温40℃,流速0.3 m L·min~(-1),进样量10μL。电喷雾离子源,多反应检测模式进行正离子检测,离子源喷雾电压3.5 kV,加热毛细管温度320℃,鞘气压力35 Pa,辅助气压力10 Pa,碰撞能量30 V,碰撞诱导解离电压12 V,多西他赛检测离子对m/z 876.3~549.1,紫杉醇检测离子对m/z 830.3~307.9。结果:多西他赛在小鼠血浆中的线性范围0.013~13 mg·L~(-1),在心、肝、脾、肺、肾的线性范围分别为0.012~12.937,0.013~13.068,0.012~13.001,0.013~13.133,0.011~12.965 mg·L~(-1);日内及日间精密度、各条件下稳定性均<15%;血浆中低、中、高质量浓度多西他赛的平均回收率分别为98.24%,97.51%,93.70%;在小鼠心、肝、脾、肺、肾各组织的平均回收率在87.87%~98.90%。结论:相较于HPLC,LC-MS/MS更适合检测小鼠血浆及组织液中多西他赛的含量,该方法稳定可行、重复性好。
Objective: To establish a method for the determination of docetaxel in mouse plasma and tissue samples. Methods: Paclitaxel was selected as the internal standard. The sample was extracted with methyl tert-butyl ether (Hypersil BDS C 18 column, 2.1 mm × 50 mm, 2.4 μm) and methanol-0.1% formic acid 20). The column temperature was 40 ℃ and the flow rate was 0.3 m L · min -1. The injection volume was 10 μL. Electrospray ionization source and multi-reaction detection mode. The ion source spraying voltage 3.5 kV, heating capillary temperature 320 ℃, sheath gas pressure 35 Pa, auxiliary gas pressure 10 Pa, collision energy 30 V, collision induced dissociation voltage 12 V, docetaxel test ion pair m / z 876.3 ~ 549.1, paclitaxel test ion pair m / z 830.3 ~ 307.9. Results: The linear range of docetaxel in mice plasma was 0.013 ~ 13 mg · L -1. The linear range of heart, liver, spleen, lung and kidney were 0.012 ~ 12.937, 0.013 ~ 13.068 and 0.012 ~ 13.001,0.013 ~ 13.133,0.011 ~ 12.965 mg · L -1. The intra- and inter-day precision was <15%, and the average plasma concentrations of docetaxel at low, medium and high concentrations The recoveries were 98.24%, 97.51% and 93.70%, respectively. The average recoveries in the tissues of heart, liver, spleen, lung and kidney in mice ranged from 87.87% to 98.90%. Conclusion: Compared with HPLC, LC-MS / MS is more suitable for the determination of docetaxel in mouse plasma and tissue fluid. The method is stable and reproducible.