LC-MS/MS法测定全血中瑞芬太尼含量

Quantitative.determination of remifentanil in human whole blood with liquid chromatography-tandem mass spectrometry method

目的:建立液相色谱一串联质谱法(LC-MS/MS)测定全血中瑞芬太尼的含量。方法:抗凝全血经乙腈直接沉淀后,以液相色谱分离、电喷雾离子化串联质谱进行检测,瑞芬太尼、利伐司替明(内标)的 MRM 扫描离子通道 m/z 分别选择为377.6→317.0和251.6→206.1,瑞芬太尼的保留时间为1.64 min,每个样品分析用时3.0 min。结果:瑞芬太尼在0.0625～8 ng·mL^(-1)范围内线性关系良好(r=0.9978)。日内、日间 RSD 分别为1.4%～7.4%及4.5%～14%,准确度分别为95.6%～102.1%及94.4%～102.6%。结论:该方法的样品预处理快速简便,检测专一灵敏,可满足瑞芬太尼临床研究药物浓度测定的要求。

Objective ：To establish a liquid chromatography tandem mass spectrometry （ LC - MS/MS） method for the determination of remifentanil in human whole blood. Method： Heparinized whole blood was precipitated with acetonitrile and the drug was determined by LC - MS/MS using electrospray ionization. Remifentanil and internal standard were detected on multiple reaction monitoring mode by the transitions from the precursor to the product ion （ m/z 377. 6/317. 0 and m/z 251.6/206. 1 ）. The retention time of the analyte was 1.64 min and total run time was 3.0 rain for each sample. Results： Calihration curve was linear in the range from 0. 0625 to 8. 0 ng · mL^-1 with a correlation coefficient of 0. 9978. The intra -and inter- day precision （RSD） were all within 15% and the accuracy were all within 85% - 115%. Conclusion： The LC - MS/MS method for the quantitative determination of remifentanil in human whole blood presented simple and fast sample process, sensitive detection and acceptable precision. Therefore it can be used for remifentanil determination in clinic applications.