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 analytical method combining streamlined sample pretreatment, gas chromatography-electron capture detection(GC-ECD)and external standard quantitation was established for the simultaneous detection of 8 topical insecticide residues — fipronil and its metabolites, plus four pyrethroid compounds — in Zhongshan muscovy duck meat and duck egg by-products. Following purification using Waters Oasis PRiME HLB solid-phase extraction cartridges, sample analysis showed that all 8 target analytes exhibited excellent linearity over the concentration range of 0.04–0.4 mg·L−1, with all correlation coefficients(r2)above 0.99928, and the limits of detection(LODs)ranged from 0.01 to 0.10 mg·kg−1. Recovery tests were performed at three spiking levels: 0.01, 0.04 and 0.10 mg·kg−1 for most analytes, 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 fell within 80.01%–90.34%, with relative standard deviations(RSDs)of 4.28%–9.88%. Featuring simple operation, satisfactory purification efficiency and low testing cost, this method is suitable for batch monitoring of topical insecticide residues in poultry and egg products by grassroots testing institutions.

       

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