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目的建立一种同时检测人尿样中草甘膦(PMG)和氨甲基膦酸(AMPA)含量的气相色谱联用质谱(GC/MS)分析方法。方法采用GC/MS法,EI检测器,色谱柱为DB-5MS毛细管色谱柱。进样前尿样经三氟乙酸酐(TFAA)和七氟丁醇(HFB)衍生化后用氮气吹干,0.2%柠檬醛乙酸乙酯溶液溶解混匀后供GC/MS分析。结果 PMG和AMPA在10~400 ng/ml范围内呈线性关系,最低检测限分别为4.66 ng/ml和1.77 ng/ml,最小检测浓度(LOQ)分别为15.52 ng/ml、5.91 ng/ml,回收率分别为85.2%~97.5%、89.2%~99.1%,精密度均小于10%。结论本实验可同时检测尿液中草甘膦及其代谢产物氨甲基膦酸,且最低检测限较单个检测方法灵敏。
Objective To establish a gas chromatography-mass spectrometry (GC / MS) method for the simultaneous determination of glyphosate (PMG) and aminomethylphosphonic acid (AMPA) in human urine samples. Methods The GC / MS method and EI detector were used. The column was DB-5MS capillary column. Urine samples were derivatized with trifluoroacetic anhydride (TFAA) and heptafluorobutanol (HFB) before injection and then dried in nitrogen. The 0.2% citral in ethyl acetate was dissolved and mixed for GC / MS analysis. Results The linear range was 10-400 ng / ml for PMG and AMPA. The detection limits were 4.66 ng / ml and 1.77 ng / ml, respectively. The minimum detectable concentrations (LOQ) were 15.52 ng / ml and 5.91 ng / The recoveries were 85.2% -97.5% and 89.2% -99.1% respectively, with the precision of less than 10%. Conclusion This experiment can detect glyphosate and its metabolite aminomethylphosphonic acid in urine simultaneously, and the minimum detection limit is more sensitive than single detection method.