论文部分内容阅读
目的建立一种同时检测人血浆中9种有机磷农药的高效液相色谱串联质谱法(LC-MS/MS)。方法色谱柱为Thermo C18(4.6mm×250mm,5μm),柱温25℃,流动相为乙腈-水(含20mmol.L 1醋酸铵和0.1%甲酸)(85∶15),流速0.3 mL.min-1。血浆样品采用乙腈沉淀蛋白,质谱以正离子方式检测,采用多重反应监测模式(MRM)。结果 9种有机磷农药的线性范围为0.05～10μg.mL-1,定量下限为0.05μg.mL-1,检测限在0.1～5 ng.mL-1之间,方法回收率在93.23%～107.5%之间,批内、批间精密度均<10%,稳定性良好。结论该方法准确灵敏、简单快速,可用于筛查、测定患者体内的有机磷农药,有效辅助临床对中毒患者的诊断和疗效评价。
Objective To establish a high performance liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for simultaneous determination of nine organophosphorus pesticides in human plasma. Methods The column was Thermo C18 (4.6 mm × 250 mm, 5 μm). The column temperature was 25 ℃ and the mobile phase was acetonitrile-water (containing 20 mmol·L -1 ammonium acetate and 0.1% formic acid) (85:15) -1. Plasma samples were precipitated with acetonitrile and detected by mass spectrometry using multiple reaction monitoring (MRM). Results The linear range of the nine organophosphorus pesticides was 0.05-10μg.mL-1, the lower limit of quantitation was 0.05μg.mL-1, the detection limit was between 0.1-5 ng.mL-1 and the recovery was 93.23% -107.5 %, Within and between the batch precision <10%, good stability. Conclusion The method is accurate, sensitive, simple and rapid and can be used for screening and determination of organophosphorus pesticides in patients. It can effectively assist the clinical diagnosis and evaluation of poisoning patients.