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目的建立液质联用(LC-MS/MS)法测定血浆中舒芬太尼血药浓度。方法以芬太尼为内标,血浆样品经乙腈沉淀蛋白后,以Ultimate XB C18(100 mm×2.1 mm,3.0μm)柱为色谱柱,流动相为水-甲醇(15∶85,V/V),各含10 mmol.L-1乙酸铵,流速为0.2 mL.min-1,柱温40℃;质谱条件为电喷雾电离源(ESI),检测方式为正离子电离、多离子反应监测(MRM),用于定量分析的离子为舒芬太尼m/z387.2→238.1,芬太尼m/z337.2→188.2。结果舒芬太尼线性范围为0.05~2μg.L-1(r=0.996 4),线性关系良好。舒芬太尼的提取回收率为83.68%~88.06%。批内和批间精密度RSD均<10%。结论本研究建立的测定舒芬太尼血药浓度的方法简单、快速、准确、灵敏,可用于临床上血药浓度监测和药动学研究。
Objective To establish a method for the determination of sufentanil in plasma by liquid chromatography-mass spectrometry (LC-MS / MS). Methods Using fentanyl as an internal standard, the plasma samples were precipitated with acetonitrile and analyzed by column with Ultimate XB C18 (100 mm × 2.1 mm, 3.0 μm). The mobile phase was water-methanol (15:85, V / V ), Each containing 10 mmol.L-1 ammonium acetate at a flow rate of 0.2 mL.min-1 and a column temperature of 40 ° C. The mass spectrometry conditions were electrospray ionization (ESI), positive ionization and multi-ion reaction monitoring MRM) and sufentanil for the quantitative analysis m / z 387.2 → 238.1, fentanyl m / z 337.2 → 188.2. Results Sufentanil linear range of 0.05 ~ 2μg.L-1 (r = 0.996 4), a good linear relationship. Sufentanil extraction recovery was 83.68% ~ 88.06%. Intra-and inter-batch precision RSD <10%. Conclusion The method for determining sufentanil concentration in this study is simple, rapid, accurate and sensitive and can be used in the clinical monitoring of plasma concentration and pharmacokinetics.