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目的:利用高效液相色谱-质谱联用仪(LC-MS/MS)建立血清中西布曲明的快速定性定量分析方法,为临床中毒患者的快速诊治提供依据。方法:选用Sh im-pack XR-ODS色谱柱,以乙腈-10 mmol.L-1醋酸铵为流动相,采用等度洗脱进行分离,流速:0.3 m l.m in-1;柱温:40℃;进样量:10μl。样品用乙腈进行蛋白沉淀后进样,选用3200型质谱仪的多重反应监测(MRM)扫描方式进行检测。结果:西布曲明的线性范围为0.1 ng.m l-1~1000 ng.m l-1,定量下限和最低检测限分别为0.5 ng.m l-1和0.05 ng.m l-1。日内精密度RSD为3.6%,日间精密度RSD为4.0%。结论:本研究所建立的方法快速、灵敏,重复性好,适用于西布曲明中毒患者血液标本的快速定性定量检测。
OBJECTIVE: To establish a rapid qualitative and quantitative method for the determination of sibutramine in serum by high performance liquid chromatography-mass spectrometry (LC-MS / MS), and provide a basis for the rapid diagnosis and treatment of clinical poisoning patients. METHODS: Shim-pack XR-ODS column was used with acetonitrile-10 mmol.L-1 ammonium acetate as the mobile phase and separated by isocratic elution. The flow rate was 0.3 m lm in-1. The column temperature was 40 ℃ ; Injection volume: 10μl. The samples were submitted to protein precipitation with acetonitrile, and then detected by multiplex reaction monitoring (MRM) scan using a 3200 mass spectrometer. Results: The linear range of sibutramine was 0.1 ng.m l -1 to 1000 ng.m l -1, and the limits of quantitation (LOQs) and the limits of detection were 0.5 ng.m l -1 and 0.05 ng.m l -1, respectively. The intraday RSD was 3.6% and the intraday RSD was 4.0%. Conclusion: The method established in this study is rapid, sensitive and reproducible. It is suitable for rapid qualitative and quantitative detection of blood samples from patients with sibutramine poisoning.