UFLC-MS/MS法测定中毒患者血清中氨氯地平的浓度

2014-08-07赵国良,程远泽,李勇等

灾害医学与救援(电子版) 2014年2期

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。

氨氯地平；高效液相色谱-串联质谱法；中毒

[Abstrractbjecttiive：To develop an method for the determination of the amlodipine in human serum by ultra fast liquid chromatography-tandem mass spectrometry（UFLC-MS/MS）and provide proof for the poisoners′fast diagnosis.Meetthod：Amlodipine was extracted from serum by acetonitrile which was used as deproteinated solvent，and separated on a Shim-pack XR-ODS column maintained at 40℃with acetonitrile and 10 mmol/L ammonium acetate as mobile phase by gradient elution.The flow rate was 0.30 mL/min-and 10μL aliquot of residues were injected.Detection was carried out by multiple reaction monitoring on a 3200 MRM system.Ressullttss：The assay was linear over the range 0.078-500 ng/mL with a limit of quantitation of 0.05ng/mL and a limit of detection of 0.005ng/mL.The relative deviation of intra-and inter-day were 3.1%and 2.5%.Conclussiion：The method was rapid，sensitive and reliable for the determination of amlodipine in human blood serum.The assay was applied to a fast qualitative and quantitative determination of amlodipine poisoners.

氨氯地平（Amlodipine），分子式：C20H25CLN2O5，分子量：408.1，化学结构式如下。

氨氯地平是一种1，4－二氢吡啶类的长效降压药，其终末消除半衰期约为35～50 h，7～8天后血药浓度可达稳态。因其具有服药剂量低、药效维持时间长等特点，目前已成为临床一线用药。因此，血液中氨氯地平浓度的测定显得尤为重要。血清中氨氯地平浓度的测定主要采用液相色谱-串联质谱法，酶联吸附免疫分析法等方法[1-2]。本实验利用快速高效液相色谱-质谱联用仪（UFLC-MS/MS）建立了一种检测血清氨氯地平的方法，为临床急慢性中毒患者的快速诊断和抢救提供了科学依据。