固相萃取-气相色谱-串联质谱法同时测定人体尿液中4种有机磷农药代谢物

发布时间：2018-04-11 15:44

本文选题：固相萃取 + 气相色谱-串联质谱　；参考：《分析化学》2016年05期

【摘要】：建立了同时测定尿液中4种有机磷类农药代谢物的气相色谱/串联质谱分析方法。尿液样品以WCX固相萃取柱富集提取,乙酸乙酯-乙腈(70∶30,V/V)再萃取,浓缩干燥,甲苯溶解,N-叔丁基二甲基甲硅烷基-N-甲基三氟乙酰胺衍生化。采用HP-5MS色谱柱(30 m×0.25 mm×0.25μm)程序升温分离,串联质谱多反应检测,内标法定量。通过比较尿样中代谢物在不同萃取溶剂、固相萃取柱及p H值洗脱液等条件下的回收率,优化了前处理方法。在0.2~200μg/L范围内,4种代谢物峰面积与内标峰面积的比值与质量浓度的线性关系良好(R~2≥0.992),方法检出限为0.083~0.667μg/L,定量限为0.2~2.0μg/L,平均回收率为54.1%~68.6%,相对标准偏差均小于8.5%(n=6)。本方法稳定、可靠,分析时间短,不需要使用大量有机溶剂,可同时处理大批量样品,适用于人群有机磷类农药暴露情况的评估。
[Abstract]:A method for simultaneous determination of four organophosphorus pesticide metabolites in urine by gas chromatography / tandem mass spectrometry (GC-MS) was developed.Urine samples were enriched and extracted by WCX solid phase extraction column. Ethyl acetate and acetonitrile 70: 30 V / V) were extracted, then concentrated and dried, and toluene dissolved in toluene. The dimethylsilyl dimethylsilyl N-methyltrifluoroacetamide was dissolved in toluene.HP-5MS chromatographic column (30 m 脳 0.25 mm 脳 0.25 渭 m) was used for temperature programmed separation, tandem mass spectrometry (MS) multireaction detection and internal standard determination.The pretreatment method was optimized by comparing the recoveries of metabolites in urine under different extraction solvents solid phase extraction columns and pH eluents.This method is stable, reliable, short analysis time, no need to use a large number of organic solvents, can simultaneously treat a large number of samples, suitable for population assessment of exposure to organophosphorus pesticides.
【作者单位】：中国药科大学药物质量与安全预警教育部重点实验室;环境保护部南京环境科学研究所;金陵药业股份有限公司;
【基金】：2014中央级公益性科研院所基本科研业务费资助
【分类号】：R446.12;O657.63

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