中山麻鸭及其副产品中外用杀虫药的残留测定

    Residue Determination of External Insecticides on Zhongshan Muscovy Duck and Its By-products

    • 摘要: 建立一种简便快速的样品前处理技术,结合气相色谱、电子捕获检测器(GC-ECD)和外标定量法,构建可同时检测中山麻鸭肉及鸭蛋副产品中4种氟虫腈及其代谢物、4种拟除虫菊酯类共8种外用杀虫药残留的分析方法。样品经Waters Oasis PRiME HLB SPE固相萃取小柱净化后上机测定,结果表明:8 种目标物在0.04~0.4 mg·L−1范围内线性关系优异,校正曲线相关系数(r2)均大于0.999 28;方法检出限(LOD)为0.01~0.10 mg·kg−1。设置3档加标水平开展回收试验:目标物加标浓度为 0.01、0.04、0.10 mg·kg−1,另氯氟氰菊酯、氯菊酯单独设置 0.10、0.40、1.00 mg·kg−1梯度,所有组分加标回收率区间为80.01%~90.34%,相对标准偏差(RSD)4.28%~9.88%。本方法前处理步骤简便、净化效果优良、检测成本低,适合基层检测机构批量开展禽肉产品中外用杀虫药残留监测。

       

      Abstract: In this study, a simple and rapid sample pretreatment technology was established, combined with gas chromatography, electron capture detector (GC-ECD) and external standard quantitative method to construct a method for the simultaneous detection of 8 kinds of topical insecticides residues including 4 kinds of fipronil and its metabolites, 4 kinds of pyrethroid compounds in Zhongshan muscovy duck meat and duck egg by-products was established. The samples were purified by Waters Oasis PRiME HLB SPE solid phase extraction column and then determined by machine. The results showed that: the linear relationship of the eight target compounds was excellent in the range of 0.04-0.4 mg·L−1, and the correlation coefficient (r2) of the calibration curve was greater than 0.999 28. The limits of detection (LODs) ranged from 0.01 to 0.10 mg·kg−1. The recovery tests were carried out by setting three spiking levels: the spiked concentrations of the target compounds were 0.01, 0.04, 0.10 mg·kg−1, while separate gradients of 0.10, 0.40 and 1.00 mg·kg−1 were set for cyhalothrin and permethrin. The spiked recoveries of all components were in the range of 80.01%−90.34%, and the relative standard deviations (RSDs) were 4.28%−9.88%. This method had the advantages of simple pre-processing steps, excellent purification efficiency and low detection cost, which was suitable for batch monitoring of topical insecticide residues in poultry and egg products by grassroots testing institutions.

       

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