固相微萃取/高效液相色谱联用分析食品中痕量苯并咪唑

建立了整体柱固相微萃取/高效液相色谱-紫外联用方法用于食品中6种痕量苯并咪唑的分析。在三元溶剂(N,N-二甲基甲酰胺、对二甲苯和异辛烷)体系下,以4-乙烯基苯硼酸与乙二醇二甲基丙烯酸酯原位聚合法制备了4-乙烯基苯硼酸-乙二醇二甲基丙烯酸酯固相微萃取整体柱,并采用热重分析仪、红外光谱、电镜进行表征。分别研究了萃取溶剂、萃取流速、净化体积、解吸溶剂、解吸流速和解吸体积对富集量的影响。在优化条件下,该方法对苯并咪唑的富集倍数高达1 607~3 015倍,方法的线性范围为0.100~100μg/L,检出限为21~33 ng/L,相对标准偏差(RSD)不大于7.4%。采用该方法分析鱼肉、鸭肉、鸭血和鸭肝样品中的苯并咪唑,加标回收率为75.0%~118%,RSD为1.6%~8.7%。该方法灵敏、准确,能满足食品中痕量苯并咪唑的分析要求。

Determination of Trace Benzimidazoles in Foods by Solid-phase Microextraction Coupled with High Performance Liquid Chromatography

A novel method based on the monolith solid-phase microextraction(SPME) coupled with high performance liquid chromatography was developed for the determination of trace benzimidazoles in foods.The preparation of poly (vinylphenylboronic acid-co-ethylene glycol dimethacrylate) microextraction monolith based on ternary porogen was synthesized by in situ technique.The characteristics of the monolith were investigated by thermogravimetric,infrared spectroscopy and scanning electron microscopy analysis.Effects of extraction solvents,extraction velocity,purification volume,desorption solvents,desorption velocity and desorption volume on extraction amount were investigated.Under the optimal conditions,the enrichment factors of SPME monolith for benzimidazoles were in the range of 1 607-3 015.The calibration curves of benzimidazoles showed good linear relationships in the range of 0.100-100 μg/L,with detection limits of 21-33 ng/L and relative standard deviations (RSD) no more than 7.4％.The proposed method was successfully applied in the determination of benzimidazoles in fish,duck,duck blood and duck liver samples,with recoveries of 75.0％-118％ and RSDs of 1.6％-8.7％.The proposed method based on SPME monolith was sensitive and accurate in the trace determination of benzimidazoles in complex samples.