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建立了土壤中草甘膦及其主要代谢物氨甲基膦酸高效液相色谱-串联质谱(HPLC-MS/M S)残留检测方法。样品经0.6 mol/L的氢氧化钾溶液提取、C18固相萃取柱过滤净化、9-芴基甲基三氯甲烷(FMOC-Cl)柱前衍生,以乙腈和5 mmol/L的乙酸铵为流动相,C18反相色谱梯度洗脱,电喷雾负离子多反应监测模式(MRM)HPLC-MS/MS检测。结果表明:草甘膦和氨甲基膦酸在1.6~200μg/L范围内线性关系良好,检出限(以信噪比S/N=3计)分别为0.80和0.94μg/kg,定量限(以S/N=10计)分别为2.6和3.0μg/kg;不同类型土壤样品中两种目标物3个水平的平均添加回收率在84%~104%之间,相对标准偏差(RSD)为2.8%~7.5%。应用本方法对部分供试土壤样品进行分析,结果发现所检样品中草甘膦和氨甲基膦酸的检出率较高,分别为38.9%和61.1%,两种物质土壤残留行为较为普遍。
A method for the determination of glyphosate and its metabolite Aminomethylphosphonic acid in soil by HPLC-MS / MS was established. The sample was extracted with 0.6 mol / L potassium hydroxide solution, filtered with C18 solid phase extraction column, pre-column derivatized with 9-fluorenylmethyl chloroform (FMOC-Cl), acetonitrile and 5 mmol / L ammonium acetate as Mobile phase, C18 reversed-phase gradient elution, electrospray negative ion multiple reaction monitoring (MRM) HPLC-MS / MS. The results showed that glyphosate and aminomethylphosphonic acid had a good linear relationship in the range of 1.6 ~ 200μg / L with the detection limits (S / N = 3) of 0.80 and 0.94μg / kg, respectively. The limits of quantitation (S / N = 10) were 2.6 and 3.0 μg / kg, respectively. The average recoveries of three species in two soil samples ranged from 84% to 104%. The relative standard deviations (RSDs) 2.8% ~ 7.5%. The results showed that the detection rates of glyphosate and aminomethylphosphonic acid were 38.9% and 61.1%, respectively. The soil residue behavior of the two materials was more common .