动态基质固相分散-离子液体双水相微萃取结合高效液相色谱法检测粮谷中的三嗪类除草剂

Dynamic Matrix Solid Phase Dispersion-Ionic Liquid-Based Aqueous Two-Phase Microextraction Combined with High Performance Liquid Chromatography for the Determination of Triazine Herbicides in Cereals

将动态基质固相分散与离子液体双水相微萃取技术相结合,建立高效、绿色、快速的样品前处理方法用于萃取粮谷中残留的5种三嗪类除草剂,通过高效液相色谱对目标物进行分离和测定。以离子液体为萃取溶剂,样品经基质固相分散法处理后,采用离子液体双水相体系富集目标分析物,通过Plackett-Burman试验判断各个因素对响应值的影响,采用Box-Behnken试验对显著性因素进行优化。在最佳实验条件时,目标物在线性范围内具有良好的线性关系(r≥0.9969),其检出限和定量限分别为0.62~0.76μg/kg和2.06~2.53μg/kg,加标回收率为82.92%~106.98%。本法具有萃取时间短、试剂用量少、操作简单、绿色环保等优点,可用于粮谷中三嗪类除草剂的分析与检测。

An efficient,green and fast dynamic matrix solid phase dispersion coupled with ionic liquid-based aqueous two-phase microextraction system was developed and applied to the determination of five triazine herbicides in cereals,including simetone,atraton,terbuthylazine,dipropetryn and terbumeton by high performance liquid chromatography(HPLC).In this method,after pretreatment by matrix solid phase dispersion,the ionic liquid-based aqueous two-phase microextraction system was used for the enrichment of the target analytes.The Plackett-Burman design was used to identify factors that could significantly affect the average recovery of the analytes,which were subsequently optimized using the Box-Behnken design.The results demonstrated that under optimized experimental conditions,the calibration curves for the target analytes displayed good linearity(r≥0.9969)in the concentration range of 5.00–100.00μg/kg.The limits of detection for the analytes were 0.62–0.76μg/kg and the limits of quantification were 2.06–2.53μg/kg.The spiked recoveries were in the range of 82.92%–106.98%.The developed method has the advantages of simple operation,short extraction time,low consumption of organic reagents and environmental friendliness and can be used for the analysis and detection of triazine herbicides in cereals.