【摘要】 目的利用GC-MS鉴定出SD大鼠尿液中敌百虫的代谢产物三氯乙醇和2,2-二氯乙酰胺,并建立GC-ECD同时测定SD大鼠尿中三氯乙醇和2,2-二氯乙酰胺的分析方法。方法尿液经乙腈萃取,以1,3-二氯-2-丙醇和2-氯乙酰胺作为双内标,采用HP-INNOWAX(30 m×0.32 mm,0.25μm)色谱柱,检测器为ECD检测器,检测器温度为280℃。进样口温度为200℃,不分流进样,进样量为1μl。程序升温为初始温度120℃保持2 min,以10℃/min升至150℃保持1 min,再以10℃/min升至200℃保持1 min,最后以5℃/min升至240℃保持2 min。结果三氯乙醇、2,2-二氯乙酰胺分别在2.84 ng/ml~210.52 ng/ml(r=0.999 9)、42.51 ng/ml~411 ng/ml(r=0.999 7)质量浓度时线性关系良好,最低检出限为0.82 ng/ml、13.23 ng/ml,平均回收率(n=9)为81.65%、104.60%。结论该方法灵敏准确、简便实用,可用于尿液中三氯乙醇、2,2-二氯乙酰胺的含量分析。更多还原

【Abstract】 Objective To identify trichloroethanol and 2,2-dichloroacetamide from the trichlorfon metabolites in SD rat urine by GC- MS,and to determine trichloroethanol and 2,2- dichloroacetamide in rat urine by gas chromatography with ECD detection.Methods The urine was extracted with acetonitrile.1,3-dichloro-2-propanol and 2- chloroacetamide were used as internal standards.The GC was performed on an HP-INNOWAX column(30 m ×0.32 mm,0.25 μm) with ECD detector.The temperature of detector was set at 280℃.The temperature of injector was 200℃.Splitless mode was used and the injection volume was 1 μl.The temperature program of column oven was programmed as follows:120 ℃ for 2 min,then increased to150 ℃ at 10 ℃/min,and kept for 1 min;And then increased to 200 ℃ at 10 ℃/min and held for 1 min;And finally increased to 240 ℃ at 5 ℃/min and kept for 2 min.Results The calibration curves of trichloroethanol and 2,2- dichloroacetamide showed good linearity in the range of 2.74 ng/ml-210.52 ng/ml(r =0.999 9) and 42.51 ng/ml-411 ng/ml(r=0.999 7),respectively.The detection limits were 0.82 ng/ml and 13.23 ng/ml,respectively.The mean recoveries(n =9) were 81.65%and 104.60%,respectively.Conclusion The method is sensitive,accurate,simple and practical,and it can be used to determine trichloroethanol and 2,2- dichloroacetamide in urine.更多还原