分散固相萃取法在火腿有机磷农药检测中的应用与固相萃取法的比较  

Application of dispersive solid phase extraction in the determination of organophosphorus pesticides in ham and the comparison with solid-phase extraction

作　　者：侯逸众[1] 黄方取 申屠平平[1] 周鸿艳[1] 吴位新 徐小民[2] 

机构地区：[1]金华市疾病预防控制中心,浙江金华321002 [2]浙江省疾病预防控制中心,浙江杭州310051

出　　处：《中国卫生检验杂志》2017年第6期777-780,共4页Chinese Journal of Health Laboratory Technology

基　　金：浙江金华市科技局资助项目(2014-3-102)

摘　　要：目的建立分散固相萃取法(DSPE)净化处理火腿样品,气相色谱-质谱法测定29种有机磷农药残留量,为火腿中有机磷农药残留检测提供参考。方法通过优化气相色谱与质谱的采集参数,确定适用于有机磷农药的最佳仪器检测条件。样品加水浸泡后依次加入乙腈、氯化钠、无水硫酸镁提取,离心,冷冻去除油脂后取有机相以C_(18)、PSA和无水硫酸镁作为分散固相萃取试剂去除杂质,浓缩后以丙酮定容气相色谱-质谱仪测定,配制基质,绘制标准曲线,在选择性离子监测(SIM)模式下采用内标法定量。结果 29种有机磷农药在考察范围内线性关系良好(r值为0.996 8~0.999 9),加标回收率为62.9%~115.8%,相对标准偏差(RSD)为0.4%~4.7%。结论该方法操作方便,试剂消耗量少,回收率稳定,结果准确可靠,适合快速筛查检测火腿中有机磷农药残留。Objective To establish a dispersive solid phase extraction（ SPE） method for the purification of ham,and to detect the 29 organophosphate residues by gas chromatography-mass spectrometry,so as to provide reference for the detection of organophosphorus pesticide residues in ham. Methods Through the optimization of the parameters of gas chromatography and mass spectrometry,the best conditions for detection of organophosphorus pesticide were obtained. After soaked in water,sample was extracted by acetonitrile,sodium chloride and anhydrous magnesium sulfate,centrifuged,frozen to remove the oil. The organic phase purified by the method used C18,PSA,and anhydrous magnesium sulfate was set as the dispersive solid phase extraction reagent to remove impurities; after concentration and dilution,acetone was quantified by gas chromatography-mass spectrometry. The matrix-matched internal standard calibration curves were used for quantitative analysis under selected ion monitor（ SIM）. Results Good linearity was obtained when the 29 organophosphorus pesticides were within the reference range,and the correlation coefficient（ r） was within 0. 996 8-0. 999 8,the recoveries were within 62. 9%-115. 8%,and the relative standard deviation（ RSD） was within 0. 4%-4. 7%. Conclusion The method is easy to operate with less reagent consumption,stable recoveries,accurate and reliable results,which is suitable for rapid screening of organophosphorus pesticide residues in ham.

关 键 词：分散固相萃取 气相色谱-质谱法 火腿 有机磷农药 

分 类 号：O657.63[理学—分析化学]