超高效液相色谱-串联质谱法测定人尿中毒死蜱的主要代谢产物3,5,6-三氯-2-吡啶醇

建立了人尿液中毒死蜱主要代谢产物3,5,6-三氯-2-吡啶醇(3,5,6-TCP)的超高效液相色谱-串联质谱分析测定方法。采用二氯甲烷-乙酸乙酯(20:80, v/v)溶液中性条件下提取,ACQUITY UPLC BEH C18柱色谱分离,以乙腈-水为流动相梯度洗脱,在电喷雾电离(ESI)负离子模式下,选择离子监测(SIR)方式检测。方法线性范围为0.005~0.4 mg/L,检出限为0.41 μg/L,平均加标回收率为97.9%,日内及日间精密度(RSD)均小于15%。该方法操作简单、灵敏度高、准确性好、重现性强,已成功应用于人尿液实际样品中3,5,6-TCP的测定,为毒死蜱的人体健康风险暴露评估以及其生物负荷的痕量监测提供了有效的方法支撑。

Determination of chlorpyrifos’ main metabolite 3,5,6-trichloro-2-pyridinol in human urine by ultra performance liquid chromatography coupled with tandem mass spectrometry

A method for the determination of 3,5,6-trichloro-2-pyridinol (3,5,6-TCP) in human urine, which is the main metabolite of chlorpyrifos, has been established employing ultra performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS). The urine samples were prepared by liquid-liquid extraction with dichloromethane-ethyl acetate (20:80, v/v) solution followed by the separation with the gradient elution of acetonitrile-water on an ACQUITY UPLC BEH C18 column. The analyte was detected by tandem mass spectrometry under the negative ion mode with the electrospray ionization (ESI) source and the selective ion recording (SIR) mode. Under the optimized conditions, the calibration curve was linear in the range of 0.005-0.4 mg/L. The limit of detection was 0.41 μg/L. The average recovery was 97.9%. The intra-and inter-day precisions calculated with RSDs were all within 15% at each quality control (QC) level. The developed method is simple, sensitive, accurate and repeatable, which has been successfully applied to determine the exposure level of 3,5,6-TCP in the real samples of human urine. The results show that this method is supportive for the exposure assessment in human health risk analysis and monitoring the biological burden of chlorpyrifos.