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目的:利用快速高效液相色谱-质谱联用仪(UFLC-MS/MS)建立血清中氨氯地平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Shim-pack XR-ODS色谱柱,以乙腈10 mmol/L醋酸铵为流动相,采用梯度洗脱进行分离,流速:0.3 ml/min;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:氨氯地平的线性范围为0.078~500 ng/ml,定量下限和最低检测限分别为0.05 ng/ml和0.005 ng/ml。日内精密度为2.5%,日间精密度为3.1%。结论:本研究所建立的方法快速、灵敏,重复性好,适用于氨氯地平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 amlodipine in serum by using high performance liquid chromatography-mass spectrometry (UFLC-MS / MS) to provide a basis for the rapid diagnosis and treatment of clinical poisoning patients. Methods: Shim-pack XR-ODS column was used with 10 mmol / L ammonium acetate as mobile phase. The mobile phase was separated by gradient elution. The flow rate was 0.3 ml / min. The column temperature was 40 ℃. The injection volume was 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 amlodipine was 0.078-500 ng / ml. The limits of quantification (LOQ) and the lowest limit of detection (LOD) were 0.05 ng / ml and 0.005 ng / ml, respectively. The intraday precision was 2.5% and the intraday precision was 3.1%. Conclusion: The method established in this study is rapid, sensitive and reproducible. It is suitable for the rapid and qualitative detection of blood samples from amlodipine poisoning patients.