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目的建立液相色谱质谱联用(LC-MS/MS)测定静脉复合麻醉患者血浆中舒芬太尼的药物浓度方法。方法血浆样品经2 mol.L-1 NaOH溶液20μL碱化后用乙醚萃取,以芬太尼为内标,采用LC-MS/MS测定。色谱柱为Diamonsil C18柱(4.6mm×150 mm,5μm),以甲醇-5 mmol.L-1醋酸铵-醋酸(74∶26∶0.5)为流动相,流速为0.5 mL.min-1;质谱条件采用TIS离子源,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反应分别为m/z 387.2→m/z 238.2(舒芬太尼)和m/z 337.4→m/z 188.2(芬太尼)。结果舒芬太尼在0.01～1.00μg.L-1(r=0.998 1)内线性关系良好,高、中、低3浓度的提取回收率在64.2%以上,日内、日间精密度均小于11.6%。结论本试验建立的舒芬太尼血药浓度的测定方法简单、快速、准确、灵敏,可用于临床上复合麻醉中小剂量应用舒芬太尼患者的血药浓度测定及临床药动学研究。
Objective To establish a method for the determination of sufentanil concentration in plasma by liquid chromatography-mass spectrometry (LC-MS / MS). Methods The plasma samples were extracted with 20 μL 2 mol·L-1 NaOH solution and extracted with diethyl ether. The internal standard of fentanyl was determined by LC-MS / MS. The column was a Diamonsil C18 column (4.6 mm × 150 mm, 5 μm) with a mobile phase of methanol-5 mmol·L-1 ammonium acetate-acetic acid (74:26:0.5) at a flow rate of 0.5 mL · min-1. The conditions were TIS ion source, positive ion detection and multi-ion reaction monitoring (MRM), and the ion reactions for quantitative analysis were m / z 387.2 → m / z 238.2 (sufentanil) and m / z 337.4 → m / z 188.2 (fentanyl). Results Sufentanil showed a good linearity in the range of 0.01-1.00 μg.L-1 (r = 0.998 1). The recoveries of high, middle and low concentrations were higher than 64.2%, and the intra-day and inter-day precision were less than 11.6 %. Conclusion The method for determining sufentanil concentration in this study is simple, rapid, accurate and sensitive and can be used for the determination of serum concentration and clinical pharmacokinetics of sufentanil in small and medium dose clinical anesthesia.