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以乙腈-无机盐-水双水相体系,建立了一种环保、高效的用于气相色谱法检测鱼肉样品中拟除虫菊酯的样品前处理方法.实验利用荧光猝灭法与气相色谱法研究了拟除虫菊酯药物在以蛋白质为主要基质的水产品中的存在状态,考察了双水相的形成条件,并探讨了蛋白质对双水相萃取率的影响.结果表明,拟除虫菊酯药物通过疏水作用力与蛋白质牢固结合.以体积分数为80%的乙腈水溶液作为萃取液可以引起水产品中的蛋白质基质缓慢而彻底地变性,从而充分释放与蛋白质结合的药物,实现拟除虫菊酯的均相高效萃取.80%的乙腈水溶液具有较强的化学极性,因而在双水相系统上相中与药物残留共同萃入的脂溶性杂质较少,萃取液净化步骤大大简化.在双水相上相中加入无水MgSO4,PSA去除水分与杂质后,直接进样进行气相色谱检测.该方法用于鱼肉样品中六种拟除虫菊酯的萃取检测,回收率为81.1%～96.4%,检出限为8～14ng·mL-1.
An environment-friendly and efficient sample pretreatment method was developed for the determination of pyrethroids in fish samples by gas chromatography with acetonitrile-inorganic salt-water aqueous two-phase system.Fluorescence quenching and gas chromatography The existence of pyrethroid drugs in aquatic products with protein as the main substrate was investigated by investigating the formation conditions of aqueous two phases and the effect of protein on the extraction efficiency of aqueous two phases.The results showed that pyrethroid drugs Force and protein firm combination.At volume fraction of 80% acetonitrile as an extract solution can cause the protein matrix in aquatic products slowly and thoroughly denatured, and thus fully release the protein binding drugs, pyrethroid homogeneous homogeneous extraction .80% acetonitrile aqueous solution has a strong chemical polarity, so the phase in the aqueous two-phase system with the drug residue co-extraction of fat-soluble impurities less purification step greatly simplifies the extract.In the aqueous phase Addition of anhydrous MgSO4, PSA removal of water and impurities, direct injection gas chromatography detection.The method for the six samples of fish samples pyrethroids extraction Measured recovery was 81.1% ~ 96.4%, the detection limit was 8 ~ 14ng · mL-1.