QuEChERS方法在HPLC测定豇豆中灭蝇胺残留量的应用研究

Application of the QuEChERS Method in the Determination of Cyromazine Residues in Cowpeas by HPLC

为优化豇豆中灭蝇胺残留量检测的前处理方法。以豇豆作为基质,对QuEChERS方法与(NY/T 1725-2009《蔬菜中灭蝇胺残留量的测定高效液相色谱法》)的检验方法进行回收率试验比较;并根据单一变量原则,优化QuEChERS方法中的PSA、GCB两种净化剂使用量。结果表明:采用QuEChERS方法前处理的豇豆样品加标回收率为76.7%~80.3%,标准偏差为6.2%~8.7%,其回收率和精密度都能达到分析检测要求。QuEChERS方法最优的净化剂组合为无水硫酸镁900mg+PSA 100mg,采用此净化剂组合前处理的豇豆样品回收率为83.3%~86.7%,标准偏差为8.2%~11.5%。综上分析表明,QuEChERS前处理方法简单快速、准确可靠,既可满足豇豆中灭蝇胺残留量检测的技术要求,又可用于大量样品的快速检测。

In order to optimize the pretreatment method for the detection of cyromazine residues in cowpeas,with the cowpea as the substrate,the comparative test of recovery was carried out between the QuEChERS method and the test method in NY/T 1725-2009 "Determination of cyromazine residues in vegetables by high performance liquid chromatography".According to the principle of single variable,the usage of the two cleaning agents PSA and GCB in the QuEChERS method was optimized.The results showed that the standard recovery rate of cowpea samples pretreated with the QuEChERS method was 76.7%-80.3%,and the standard deviation was 6.2%-8.7%.The recovery and precision could both meet the requirements of analysis and detection.The optimal combination of cleaning agents in the QuEChERS method was that the anhydrous magnesium sulfate 900 mg+PSA 100 mg,and the recovery rate of cowpea samples pretreated with the combination of cleaning agents in the QuEChERS method was 83.3%-86.7%,and the standard deviation was 8.2%-11.5%.In conclusion,the pretreatment method of QuEChERS was simple,rapid,accurate and reliable,which could not only meet the technical requirements for the detection of cyromazine residues in cowpeas,but also be used for the rapid detection of a large number of samples.