摘要
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 of HPLC-MS / MS was established for the determination of glyphosate and aminomethylphosphonic acid（ AMPA） in soil. The sample was extracted by KOH（ 0. 6 mol / L）,purified by C18-SPE, and then pre-column derivatization by FMOC-Cl. The chromatographic separation was performed on C18 column with gradient elution using acetonitrile and ammonium acetate（ 5 mmol/L） as mobile phases. Mass spectrometric acquisitions were carried out by means of multiple reaction monitoring（ MRM） in the electrospray negative ionization mode. The results showed that the calibration curve of glyphosate and AMPA was linear within the range of 1. 6- 200 μg / L. The limits of detection（ LOD, S / N = 3） were 0. 80 μ and 0. 94 μg / kg respectively, and the limits of quantification（ LOQ,S / N = 10） were 2. 6 and 3. 0 μg / kg respectively. The recoveries in differentsamples at three spiked concentration levels ranged from 84% to 104 % with the relative standard deviations from 2. 8% to 7. 5%. The current method has been applied in the analysis of some soil samples. The results showed that the detection rate of glyphosate and AMPA were 38. 9% and 61. 1%,respectively.
出处
《农药学学报》
CAS
CSCD
北大核心
2015年第4期439-446,共8页
Chinese Journal of Pesticide Science
基金
西北农林科技大学大型仪器设备功能开发项目(dysb130217)
关键词
柱前衍生
高效液相色谱-串联质谱
土壤
草甘膦
代谢物
氨甲基膦酸(AMPA)
pre-column derivatization
high performance liquid chromatography-tandem mass spectrometry
soil
glyphosate
metabolites
aminomethylphosphonic acid（AM PA）
