摘 要: 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10~400ng/ml范围内呈线性关系,最低检测限分别为4.66ng/ml和1.77ng/ml,LOQ分别为15.52ng/ml、5.91ng/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。 |
关键词: 草甘膦(PMG) 氨甲基膦酸(AMPA) 除草剂 尿 衍生化 气相色谱联用质谱法(GC/MS) 最小检测浓度(LOQ) |
中图分类号: R446.12; O625.636
文献标识码:
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基金项目: 国家职业卫生标准项目(20140701)江苏省医学领军人才(LJ201130) |
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Detection of glyphosate and aminomethyl phosphonic acid in human urine by GC/MS |
Pan Liping, Zhang Feng, Liu Qingdong, Zhu Bao1i
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School of Public Health, Nanjing Medical University, Nanjing 211166, China
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Abstract: Objective To establish a GC/MS method for detection of glyphosate and aminomethyl phosphonic acid in human urine simiultaneously. Methods First, the urine samples were fully dried by derivatization with TFAA and HFB, dissolved by 0.2% citral ethyl acetate solution, then, PMG and AMPA in the extracts were measured by GC/MS method with DB-5MS capillary column and EI ion-source. Results The results showed that the calibration curves for PMG and AMPA in the samples were linear in the concentration ranges of 10-400ng/ml. The minimum detection limits were 4.66ng/ml and 1.77ng/ml for PMG and AMPA, the LOQ were 15.52ng/ml, 5.91ng/ml for PMG and AMPA, respectively, the recovery rate for PMG ranged from 85.2%-97.5%, while 89.2%-99.1% for AMPA, RSD all were less than 10%. Conclusion The established GC/MS method can used for detection of PMG and AMPA in human urine samples simultaneously, and might be used in routine assessment or monitoring of PMG and AMPA. |
Keywords: g1yphosate(PMG) aminomethyl phosphoric acid(AMPA),herbicide human urine derivatization GC/MS,1imit of quantification (LOQ) |