食品研究与开发:2026,47(1):134-144
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通过式固相萃取净化-超高效液相色谱-串联质谱法快速测定部分动物源性食品中46种杀虫剂残留
肖泳,曾小明,李政,袁列江,邓航,谢叔娥,潘照
(湖南省产商品质量检验研究院,湖南 长沙 410007)
Rapid Determination of 46 Insecticide Residues in Animal-Derived Food by Pass-Through Solid-Phase Extraction-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry
XIAO Yong, ZENG Xiaoming, LI Zheng, YUAN Liejiang, DENG Hang, XIE Shu′e, PAN Zhao
(Hunan Provincial Institute of Product and Goods Quality Inspection, Changsha 410007, Hunan, China)
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投稿时间:2024-09-29    
中文摘要: 该研究建立通过式固相萃取结合超高效液相色谱-串联质谱法快速测定部分动物源性食品中46种杀虫剂残留的分析方法。样品加水分散后,用乙腈提取,HMR-Lipid固相萃取柱净化,经XSelect HSS T3色谱柱分离,以甲醇和水为流动相进行梯度洗脱,基质匹配标准曲线外标法定量。结果 表明,46种杀虫剂在各自线性范围内线性关系良好,相关系数大于0.995,定量限为1.0~10.0 μg/kg;以猪肉、猪肾、鸡蛋、牛奶为基质,在定量限、10倍定量限、50倍定量限加标水平下的回收率为65%~110%,相对标准偏差为1.9%~10.6%。该方法高效便捷,定量准确,适用于畜禽肉及内脏、蛋类、生乳等动物源性食品中46种杀虫剂残留的快速定量检测。
Abstract:A method for determining 46 insecticide residues in animal-derived food by pass-through solidphase extraction-ultra high performance liquid chromatography-tandem mass spectrometry was established.The animal-derived food samples were dispersed with water, extracted with acetonitrile, and purified with HMR-Lipid solid-phase extraction column. The analytes were separated on a XSelect HSS T3 column by gradient elution with methanol and water as the mobile phases. Then, quantification of the analytes was performed by the matrix-matched standard curve external standard method. The results showed that the 46 insecticides had good linear relationships within their respective ranges, with the correlation coefficients greater than 0.995. The limits of quantification (LOQ) of the method for the insecticides were 1.0-10.0 μg/kg. With pork,pig kidney, egg, and milk as matrixes, the recovery rates at three spiking levels (LOQ, 10 LOQ, and 50 LOQ) ranged from 65% to 110%, with relative standard deviations of 1.9% to 10.6%. The established method was efficient, simple, and accurate, thus being suitable for rapid quantitation of 46 insecticide residues in animal-derived food products such as livestock and poultry meat, offal, eggs, and raw milk.
文章编号:202601017     中图分类号:    文献标志码:
基金项目:湖南省自然科学基金-市场监督管理局联合项目(2022JJ90031)
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