建立简单、灵敏的土壤中草甘膦残留量的高效液相色谱检测方法。土壤样品用0.6mol·L^-1KOH提取,经对甲基苯磺酰氯衍生化后,注入Cj8柱中分离,用紫外检测器在235FIB波长检测,流动相组成为0.05mol·L^-1磷酸盐缓冲液(pH5.5):甲醇=65:35(V:V)。样品中苹甘膦浓度在0.5~40mg·L^-1范围内与峰面积呈线性关系(R^2=0.9998)。草甘膦的最小检出量(LOD)为2×10^-10g,土壤中最低检出浓度(LOQ)为0.02mg·kg^-1,平均回收率及变异系数分别为81.3%-98.3%和0.66%~5.63%。
A simple, sensitive and selective method using high performance liquid chromatography (HPLC) was developed to determine residues of glyphosate in soil. The soil sample was extracted with 0.6 mol·L^-1 KOH, and glyphosate in solution was derivatized with p- toluenesulfonyl chloride under alkaline conditions. An aliquot of the reaction mixture was injected into a C18-column with a mobile phase consisting of 0. 05 mol·L^-1 phosphate buffer ( pH 5.5 ) -methanol (65 : 35, V/V) and detected at 235 nm. The response was linear in the range 0. 5 - 40 mg·L^-1 for glyphosate in the sample solution (R^2 = 0. 999 8). The limit of detection was estimated to be 2 × 10^-10 g, and the minimum determination concentration of glyphosate in soil samples was 0. 02 mg·L^-1. The ranges of average recoveries and coefficient variation of the method were 81.3% -98.3% and 0. 66% -5.63% ,respectively.