摘要
目的:利用快速高效液相色谱-质谱联用仪(UFLC-MS/MS)建立血清中秋水仙碱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乙酸铵为流动相,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,多重反应监测(MRM)方式检测。结果:秋水仙碱的线性范围为0.1 ng/ml~1000 ng/ml,定量下限和最低检测限分别为0.5 ng/ml和0.05 ng/ml。日内精密度(RSD)为3.3%,日间精密度(RSD)为3.8%。结论:本法快速、灵敏,重复性好,适用于秋水仙碱中毒患者血液标本的快速定性定量检测。
Objective:To develop an ultra fast liquid chromatography-tandem mass spectrometry(UFLC-MS/MS) method for the determination of the colchicine in human serum and provide proof for the poisoners′ diagnosis.Methods: Colchicine was extracted from serum by acetonitrile,and then 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 injection volume was 10 μl.Detection was carried out by multiple reaction monitoring.Results: The assay was linear over the range of 0.1 ng/ml^1000 ng/ml with quantitation limit of 0.5 ng/ml and lowest detection limit of 0.05 ng/ml.The relative deviation of intra-and inter-day were 3.3%,3.8%,respectively.Conclusion: The method is rapid,sensitive and reliable and suitable for the determination of colchicine in human serum blood.The assay is applied to a fast qualitative and quantitative determination of colchicine poisoners.
出处
《中国卫生检验杂志》
北大核心
2012年第11期2571-2573,共3页
Chinese Journal of Health Laboratory Technology