血液和尿液中草甘膦的净化富集及检测

目的建立血液、尿液中草甘膦的净化富集及定性定量方法。方法取适量血、尿样品,用80%甲醇水溶液稀释,经Agilent Accu Bond NH2（弱阴离子交换柱）净化富集,用3m L 5%氨水溶液洗脱后进行ESI/LC/MRM对草甘膦的定性及阴离子色谱法（IC）的定量检验分析。结果血液、尿液中草甘膦的IC法检验回收率均大于90%,方法的线性范围均在1-100μg/m L,血检测限为0.1μg/m L,尿液为0.08μg/m L。血液、尿液中草甘膦的LC/MRM的方法检测限均在5ng/m L左右。结论建立的血、尿中草甘膦的前处理方法和LC/MRM定性分析及IC定量分析方法,可满足司法检验要求。

Exploration of the glyphosate analysis in the urine and plasma

Objective To establish the qualitative and quantitative methods for the glyphosate in the plasma and urine. Methods Sampled appropriate amount of the urine and plasma,then diluted the samples by 80% methanol water solution,depurated and enriched by the SPE column of Agilent Accu Bond NH2,and eluted by 3m L of 5% hartshorn. At last,the elution solution was qualitative detected by ESI / LC / MRM and quantitative determined by IC. Results The quantitative results by IC were that the recoveries were all greater than 90%,and linearity ranges were all between 1-100μg / m L. The limits of the IC detection was0. 1μg / m L in the blood and 0. 08μg / m L in the urine,respectively. The extraordinary sensitivity which is just 5ng / m L as detectability for glyphosate in both of the plasma and urine by LC / MRM. Conclusion The pretreatment method and the qualitative and quantitative detection methods by LC / MRM and IC respectively for the glyphosate in plasma and urine were suitable to the forensic requirement.