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目的:利用高效液相色谱-质谱联用仪(LC-MS/MS)建立血清中地芬诺酯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:35℃;进样量:5μl。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:地芬诺酯的线性范围为0.1 ng/ml～1000 ng/ml,定量下限和最低检测限分别为0.1 ng/ml和0.01 ng/ml。日内精密度RSD为2.7%,日间精密度RSD为3.8%。结论:本研究所建立的方法快速、灵敏,重复性好,适用于地芬诺酯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 diltiazem 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 ammonium acetate as mobile phase and separated by gradient elution. The flow rate was 0.3 ml / min. The column temperature was 35 ℃. The injection volume was 5μl . 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 diphenoxylate ranged from 0.1 ng / ml to 1000 ng / ml. The lower limit of detection and the lowest limit of detection were 0.1 ng / ml and 0.01 ng / ml, respectively. The intraday RSD was 2.7% and the intraday RSD was 3.8%. Conclusion: The method established in this study is rapid, sensitive and reproducible. It is suitable for the rapid qualitative and quantitative detection of blood samples of diphenoxylate poisoning patients.