甲硫嘧磺隆在小麦及土壤中残留的分析方法

建立了一种小麦和土壤中甲硫嘧磺隆残留的检测方法,采用层析柱和SPE小柱对样品进行净化、萃取,采用C18柱,以乙腈-0.5%冰乙酸混合溶剂为流动相,于236nm检测。在选定条件下该方法的最小检出量为0.35ng,籽粒和土壤中甲硫嘧磺隆的最低检测浓度为0.018mg/kg,植株中甲硫嘧磺隆的最低检测浓度为0.050mg/kg,甲硫嘧磺隆的质量浓度在0.1～5.0mg/L之间线性关系良好。在土壤和籽粒中以0.02、0.2、2.0mg/kg进行空白样品添加试验,平均回收率为92.14%～96.41%,变异系数为3.15%～9.45%之间,在小麦植株中以0.05、0.5、2.0mg/kg进行空白样品添加试验,平均回收率为86.93%～94.80%,变异系数为6.28%～8.30%之间。该方法的灵敏度、准确度、精密度均符合农药残留技术测定要求。

Residue Analysis Method of HNPC-C9908 in Wheat and Soil

A method was developed for determination of HNPC-C9908 residues in wheat and soil by HPLC. The herbicide HNPC-C9908 residues in wheat and soil was extracted with acetone/water(8/2) followed by clean-up with aluminum oxide column or SPE column and determined by HPLC equipped with a C18 column,a mixture of acetylnitrile plus acetic acid(0.5%)as mobile phase, with detection of UV wavelength at 236 nm. Limit of quantitation(LOQ)was 0.35 ng,while minimal detection concentration(MDC)in seed and soil was 0.018 mg/kg and 0.050 mg/kg in plant. There existed a good linear connection between concentration of HNPC-C9908 and its peak area in the range of 0.1～5.0 mg/L. The average recovery of seed and soil at the spiked amount of 0.02,0.2 and 2.0 mg/kg was 92.14%～96.41%,and the coefficient of variation was 3.15%～9.45%. The average recovery of plant at the spiked amount of 0.05,0.5 and 2.0 mg/kg was 86.93%～94.80%%,and the coefficient of variation was 6.3%～8.3%,respectively. The sensitivity,accuracy and precision of this method were satisfactory for pesticide residue analysis.