环境样品中碘甲磺隆钠盐残留量的高效液相色谱分析

Determination of Residue of Iodosulfuron- methyl- sodium in Environmental Samples by High Performance Liquid Chromatography

采用高效液相色谱仪,研究了环境样品中碘甲磺隆钠盐残留量的分析方法。样品用二氯甲烷提取,液-液分配结合柱层析净化,高效液相色谱法测定。不同浓度水平的添加回收率试验结果表明,当碘甲磺隆钠盐的添加水平在0.01～1.00mg·kg-1时,加标回收率为81.24%～99.77%,变异系数为2.08%～13.41%。给定色谱条件下的线性范围为0.06～6.00μg·mL,对20.00g样品,最小检出浓度为0.003mg·kg-1,且灵敏度、准确度和精密度均符合农药残留分析的要求。

A high performance liquid chromatographic method for the determination of Iodosulfuron- methyl- sodium was developed. The samples were extracted with dichloromethane and the residues were solved in 30 mL 0.02 mol· L- 1 triethylcholine after concentrated, then the dichloromethane extract was transferred into 250 mL separatory funnels for one time extraction with 10 mL petroleum. The petroleum phase was extracted one time with 0.02 mol· L- 1 triethylcholine, and then the water phase was combined and transferred into another separatory funnel. The high pH value of triethylcholine extract was regulated to between 3 and 4 by formic acid (0.1 mol· L- 1 water). This mixture was finally extracted again, three times with 35 mL dichloromethane. The extract was cleaned up on a florisil column and analyzed by HPLC. The linear range of the method was 0.06 to 6.00 mg· L- 1. The detection limit was 0.003 mg· kg- 1 for 20.00 g samples, the recoveries of spiked samples ranged from 81.24% ～ 99.77% with the coefficients of variation 2.08% ～ 13.41% . The sensitivity, detection limit and precision of the method meet the requirement of pesticide residue detection.