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摘 要：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900 mg+PSA 100 mg，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。

关键词：豇豆;灭蝇胺;高效液相色谱法;QuEChERS方法

中图分类号：S436.43 文献标志码：A 文章编号：0253-2301（2020）08-0007-06

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.

Key words： Cowpea; Cyromazine; High performance liquid chromatography; QuEChERS method

滅蝇胺是一种三嗪类化合物，具有内吸作用，属新型高效、低毒、含氮杂环类杀虫剂，目前广泛登记用于豇豆、菜豆、黄瓜、茄子等农作物，用于防治双翅目昆虫病虫害[1-6]。在相关食品抽查结果报告以及笔者日常检验工作中，豇豆中灭蝇胺残留量超限量值的情况时有发生[7]。因此，检测灭蝇胺残留情况保证食品安全具有重要作用。依据（GB 2763-2019《食品安全国家标准 食品中农药最大残留限量》）[8]的规定，灭蝇胺残留量指定的检验方法为（NY/T 1725-2009《蔬菜中灭蝇胺残留量的测定 高效液相色谱法》）[9]（以下简称标准方法），但该方法的前处理较为复杂，溶剂的使用量较大，不适用于大批量检测工作。

目前在蔬菜水果农药残留检测中，QuEChERS方法具有快速、高效、回收率高的优点，与色谱质谱联用技术配合，可以大大提高检验效率，被广泛应用于农药残留的检测工作中[10]。……