摘要
目的 建立超高效液相色谱-串联质谱法(UPLC-MS/MS)测定人血中15种有机磷农药的分析方法。方法 血液样品经乙腈沉淀蛋白,采用Waters ACQUITY UPLC HSS T3(2.1 mm×100 mm×1.8μm)色谱柱进行分离,以甲醇/水体系进行梯度洗脱,流速0.35 mL/min。以电喷雾离子源正离子(ESI+)和多反应监测(MRM)模式进行检测,内标法定量。结果 在优化的仪器条件下,15种有机磷农药均能有效检出,且分离良好。在所测质量浓度范围内,15种有机磷农药均呈现良好的线性关系,相关系数r均> 0.99,加标回收率为80.1%~117.9%,相对标准偏差(RSD)为0.36%~9.06%。结论 该方法选择性强、精密度高、重现性好,能同时检测人血中15种有机磷农药成分,可有效应用于有机磷农药中毒的快速筛查和中毒案(事)件的法医学鉴定。
Objective To develop a rapid ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) for determinnation of 15 organophosphorous pesticides in human blood. Methods The blood samples were precipitated by acetonitrile. The organophosphorous pesticides were separated on a Waters ACQUITY UPLC HSS T3 column(2.1 mm × 100 mm × 1.8 μm) by gradient elution with a flow rate of 0.35 mL/min, using purified water and methanol as mobile phases. Electrospray ion source positive ion(ESI+) and multiple reaction monitoring(MRM) were used for detection and internal standard quantification. Results The 15 organophosphorous pesticides were effectively detected and separated well under the optimized instrument conditions. All 15 organophosphorous pesticides showed a good linear relationship within the range of measured mass concentration,with all correlation coefficients greater than 0.99. The spiked recoveries of pesticides in human blood samples ranged from 80.1 % to 117.9 % with relative standard deviations(RSD) of 0.36 % to 9.06 %. Conclusion With high selectivity, high precision and good reproducibility, this method can detect 15 organophosphorous pesticides in human blood at the same time, which can be effectively used for rapid screening of organophosphorus pesticide poisoning and forensic identification of poisoning cases(incidents).
作者
富利祥
卓晓聪
徐峰
王斌杰
吴元钊
徐念来
陈峰
陶俊
邵朋阳
Fu Lixiang;Zhuo Xiaocong;Xu Feng;Wang Binjie;Wu Yuanzhao;Xu Nianlai;Chen Feng;Tao Jun;Shao Pengyang(Office of criminal Science and Technology,Xiaoshan District Branch of Hangzhou Public Security Bureau,Hangzhou,31l200,China;Key Laboratory of Drug Prevention and Control Technology of Zhejiang Province,Zhengjiang Police College,Hangzhou,310051,China)
出处
《中国法医学杂志》
CSCD
2022年第6期565-570,共6页
Chinese Journal of Forensic Medicine
