双咪唑离子液体基固相萃取-高效液相色谱法测定有机磷农药

    Bisimidazole ionic liquid-based solid-phase extraction and determination of organophosphorus pesticides by combining with high-performance liquid chromatography

    • 摘要: 有机磷农药广泛用于防治植物病虫害,故其在食品中常有残留,因此,有效萃取和测定食品基体中有机磷农药对食品安全评价有重要的意义。制备和表征了一种双咪唑基聚合3,3′-十二烷基-1,1′-二-1-乙烯基咪唑溴盐离子液体修饰的硅胶(Poly-(3,3′-dodecane-1,1′-bis-1-vinylimidazolium dibromide-modified silica),Poly (DBVD)-Sil),将其作为固相萃取吸附剂,结合高效液相色谱-紫外光谱法,考察了Poly (DBVD)-Sil对3种有机磷农药(喹硫磷、倍硫磷和辛硫磷)的萃取性能,并对影响萃取过程的4种参数(吸附剂的质量、上样流速、洗脱剂的种类和洗脱剂的体积)进行了优化。在优化的萃取条件下,建立的方法对3种有机磷农药在0.1~400 μg/L范围内有良好的线性关系(r>0.993 4),LOD(3倍信噪比)均为0.01 μg/L,RSD(n=5)为1.71%~4.08%。将该方法用于测定茉莉蜜茶和茉莉花茶饮料中有机磷农药,相对回收率为83.23%~109.89%,RSD(n=3)为3.07%~6.62%。建立的方法可以成功用于茶饮料中有机磷农药的测定,为食品中痕量有机磷农药的测定提供了一种新的途径。

       

      Abstract: Organophosphate pesticides(OPPs)have been widely used for pest control in recent years.Although they are effective tools in control of plant disease, their residue in food samples has a large of potential hazard to humans.Thus, effective extraction and determination of OPPs from food samples is vital for the food safety.In this study, poly-(3, 3′-dodecane-1, 1′-bis-1-vinylimidazolium dibromide)modified-silica(Poly(DBVD)-Sil)was prepared, characterized and used as adsorbent in solid-phase extraction.The extraction performance of the resulting Poly(DBVD)-Sil was evaluated using three OPPs(quintiophos, fenthion and phoxim)as model analytes by combining with high-performance liquid chromatography-ultraviolet detection.Some parameters(adsorbent amount, sample flow rate, elution solvent and elution volume)affecting the extraction efficiency were investigated in detail.Under the optimized conditions, the method showed good linearity for the analytes in the concentration range of 0.1-400 μg/L and low RSD of 1.71%-4.08%(n=5).The limit of detection, based on a signal-to-noise(S/N)of 3, was 0.01 μg/L for three OPPs.The proposed method was successfully used to determine OPPs from two tea drink samples with satisfactory relative recoveries of 83.23%-109.89% and RSDs of 3.07%-6.62%(n=3).The results indicate that the developed method has great potential to determine trace OPPs from food samples.

       

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