蛋白质基体对提取测定水产品中氨基甲酸酯类农药残留的影响及其消除  

Effects of protein matrix on the extraction and determination of carbamate pesticide residues in aquatic products and their elimination

作　　者：潘琳[1] 王雪梅[1] 宋跃进[1] 李玲[1] 李桂芝[1] 刘永明[1] 

机构地区：[1]烟台大学化学化工学院,山东烟台264005

出　　处：《化学研究与应用》2016年第10期1445-1449,共5页Chemical Research and Application

基　　金：山东省科技惠民计划项目(2014kjhmzc02)资助;国家自然科学基金项目(51472212)资助

摘　　要：利用乙腈水溶液为提取液,结合高效液相色谱建立了快速测定水产品中氨基甲酸酯类农药残留的方法。实验考察了蛋白质基质、有机溶剂种类、净化剂等因素对氨基甲酸酯类农药提取率的影响。结果表明,水产品中共存的蛋白质基体会影响氨基甲酸酯类农药的提取率。当采用80%的乙腈水溶液作为提取液时,提取液可以使蛋白质发生缓慢且完全的变性,释放与其结合的氨基甲酸酯类农药,从而提高提取效率。而目前广泛应用的Qu ECh ERS样品前处理方法,由于乙腈与无水硫酸镁的共同作用,引起了样品中蛋白质基质快速变性、聚集包埋药物不利于样品中农药残留的提取。80%的乙腈水溶液具有较强的化学极性,因而提取液中与药物残留共存的脂溶性杂质较少。在提取液中加入少量的PSA和C_(18)粉末即可达到满意的净化效果,简化了样品提取液的后续净化步骤。该方法用于水产品中四种常用氨基甲酸酯类农药(速灭威、异丙威、甲萘威与杀虫丹)的检测,相对标准偏差为0.7~2.5%,回收率为71.7%~103.8%,检出限为1.3~37 ng·g^(-1)。A multi residues determination method for analysis of carbamate pesticide residues in aquatic products based on the use acetonitrile aqueous solution as extracted solution followed by HPLC method. This paper is intended to study the influence of matrix proteins, organic solvents and purification agents on the extraction rate of carbamate pesticides. The results showed that the coexis-tence protein can influence the extraction rate of carbamate pesticide in aquatic products. When using 80% （volume fraction）aceto-nitrile-water solution as the extracted solution, the protein can denature slowly and completely, release the binding pesticides and improve the extraction efficiency. However,the QuEChERS sample pretreatment methods don^t work well in this case. Because the protein of main matrix in sample denatured rapidly and embedded the drug with the combined action of acetonitrile and anhydrous magnesium sulfate. But the 80% acetonitrile-water solution with strong chemical polarity can extract less impurities, simplified the extract purification step. Simultaneously, adding small amounts of PSA and C18 powder to the extracted solution can achieve a satis-factory purification effect. The sample preparation method was used satisfactorily for the determination of the carbamate pesticides （metolcarb,Isoprocarb,insecticide carbaryl and Dan） in aquatic products. The overall recoveries were in the rang of 71.7% ～ 103. 8% with acceptable RSD value of 0. 7 to 2. 5% and the detection limit were 1. 3 ～37 ng·mL-1.

关 键 词：氨基甲酸酯类农药 乙腈 蛋白质 水产品HPLC 

分 类 号：O657.7[理学—分析化学]