超高效液相色谱-质谱法测定人全血中甲胺磷、乙酰甲胺磷含量

Determination of methamidophos and acephate in human blood by UPLC-MS/MS

目的应用超高效液相色谱-质谱法(UPLC-MS/MS)对人全血中甲胺磷、乙酰甲胺磷进行定量测定。方法采用去离子水直接稀释人全血,提取血中的甲胺磷及乙酰甲胺磷,以甲醇-水(含0.1%甲酸)为流动相梯度洗脱,正离子化多反应监测(MRM)模式测定。结果甲胺磷、乙酰甲胺磷的回收率均高于87%。在选定条件下全血中甲胺磷、乙酰甲胺磷的线性范围为2～200ng/ml,最小定量限为2ng/ml。结论将全血样品进行直接稀释并应用液相色谱-质谱法进行检测可作为甲胺磷及乙酰甲胺磷中毒的快速检测方法。

Objective ： To establish an UPLC-MS/MS method for determination of methamidophos and acephate in whole blood.Methods methamidophos and acephate were extracted from blood by diluted with deionized water.The separation was carried out on an Acquity UPLCTM HSS T3 column with mobile phase 0.1% formic acid and CH3OH.Methamidophos and acephate were analyzed by UPLC-ESI MS/MS in positive electrospray ionization and multiple reaction monitoring（MRM） mode.Results The average recoveries of methamidophos and acephate in blood were above 87%.The method was linear from 2 to 200 ng/mL,with a correlation coefficient of 0.9891 and 0.9901,respectively.The quantitation limits were 2ng/L.Conclusion The developed method was applied to analyze the blood sample of a case.The results showed that the method was fast and accurate.It is useful for forensic medicine.