固相萃取-高效液相色谱联用检测饮用水中的磺酰脲类除草剂

The Determination of Sulfonylurea Herbicides in Drinking Water by Solid-phase Extraction Coupled with High Performance Liquid Chromatography

本研究基于固相萃取-高效液相色谱联用技术,建立了同时检测饮用水中两种磺酰脲类除草剂-苯磺隆、氯磺隆农药残留的方法。用甲基丙烯酸、乙二醇二甲基丙烯酸酯、偶氮二异丁腈分别作为功能单体、交联剂和引发剂,合成新型的高选择性材料,并将此吸附材料用做固相萃取的吸附剂。同时对洗脱剂的种类、体积以及样品的pH进行了优化。结果表明,在0.1 mg/L^5 mg/L的范围内两种物质线性关系良好,最低检出限分别为0.74μg/L和0.81μg/L,7次重复实验精密度分别为1.30%和2.10%。最佳的洗脱条件下,在饮用水中加标三个不同的浓度(10μg/L、15μg/L、20μg/L)的苯磺隆和氯磺隆混合物,经固相萃取后测得两种目标物的回收率可达到70.14~80.24%和76.52~106.03%。结果表明该方法可以用于饮用水中磺酰脲类除草剂的定量研究。

The determination of lribenuron-methyl and chlorsulfuron belonged to sulfonylurea herbicides in drinking water was developed based on solid-phase extraction coupled with high performance liquid chromatography （SPE-HPLC） technology. The high selectivity material was synthesized using methacrylic acid as function monomer, ethylene glycol dimethacrylate as cross-linker, and azodiisobutyronitrile as initiator. Then, tribenuron-methyl and chlorsulfuron were extracted by employing the material as absorbent. Several condition parameters, such as elution solvents, volume and sample pH, were optimized to obtain high recoveries. It was found that the linearity was good ranging from 0.1 mg/L to 5 mg/L; the limit of detections of this method for tribenuron-methyl and chlorsulfuron were 0.74 μg/L and 0.81 μg/L, respectively; and the RSD for seven replicate extractions was 1.30% and 2.10%, respectively. Under the optimized conditions, the blank water spiked with different levels of tribenuron-methyl and chlorsulfuron mixture （10 μg/L, 15 μg/L, 20 μg/L） were extracted and determined with the same method, the recoveries of tribenuron-methyl and chlorsulfuron were 70.14-80.24% and 76.52-106.03%, respectively. This method can be applied for the quantitative analysis of sulfonylurea herbicides in drinking water.