检测动物源性食品中安定与奋乃静残留的环境友好样品前处理方法研究

Study on the environment friendly sample pretreatment method for determination of diazepam and perphenazine residues in animal-origin foods

结合液相色谱检测技术,建立了一种环境友好的,检测牛肉、猪肉、猪血清中安定与奋乃静药物残留的样品前处理方法。运用平衡透析法研究了药物与三种实际样品之间的结合率,实验结果表明,安定、奋乃静与样品之间均存在较强的结合作用,这种结合作用可以降低从样品中提取两种药物的提取率。以体积分数为80%的乙醇水溶液作为提取试剂时,样品中的蛋白质会发生缓慢且完全的变性,释放出与蛋白质结合的药物,进而得到较高的提取率。由于80%的乙醇水溶液极性较大,提取液中的脂溶性杂质较少,在提取液中加入少量的PSA（N-丙基乙二胺修饰的硅胶）和C18固体净化剂即可达到满意的净化效果,大大简化了样品溶液的净化步骤。该方法应用于牛肉、猪肉、猪血清中安定与奋乃静的测定,结果令人满意,回收率均在71.2%-96.8%之间,RSD值为0.4%-3.7%。

A multi residues determination method for analysis of diazepam and perphenazine residues in beef,pork and pig serum, based on the use of a new sample preparation approach followed by HPLC method,is reported. Equilibrium dialysis method was ap-plied to investigate the binding ratios of three samples with drugs. Experiment results showed that the strong binding interactions be-tween drugs and protein decreased the extraction efficiency of diazepam and perphenazine from three samples. However,in the 80%（volume fraction）ethanol-water solution,a slow protein denaturation might take place,which would cause the unfolding of protein and the release of drugs. This resulted in the high extraction efficiency of two drugs from protein matrix samples. In this work,the purification steps were greatly simplified by adding PSA（ primary secondary amine modified silica gel） and C18 to the crude extrac-tion solution because the impurities extracted less in the high polarity of 80%ethanol-water solution. The sample preparation method was used satisfactorily for the determination of diazepam and perphenazine in spiked samples. The overall recoveries were in the range of 71. 2% -96. 8%with acceptable RSD value of 0. 4% -3. 7%.