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建立了高效液相色谱-串联质谱法(HPLC-MS~/MS)同时检测7种动物源性食品(鸡肉、牛肉、鸡蛋、鱼肉、牛奶、脂肪、猪肝)中三氟苯嘧啶、氟嘧啶、乙基多杀菌素J、双丙环虫酯、四唑虫酰胺、氟唑环菌胺和苯嘧虫噁烷7种新型农药残留的分析方法。对样品前处理和色谱、质谱条件进行优化,结果显示,样品经90%乙腈水超声提取和分散固相萃取净化,采用HPLC-MS~/MS测定,7种农药在0.10～10 ng~/m L质量浓度范围内有良好的线性关系,相关系数r≥0.99,定量限(S~/N>10)为0.50～5.0_μg~/kg,样品在3个不同加标浓度水平下的回收率均在62.73%～117.62%之间,精密度和重复性测试的相对标准偏差(n=5)均在20%以内。该方法前处理操作快速简便,检测结果灵敏度高、准确性好,可满足动物源性食品中7种新型农药残留的检测要求。
Abstract：In this study,a high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) method was established for the simultaneous detection of seven new pesticide residues(triflumezopyrim,flupyrimin,spinetoram-J,afidopyropen,tetraniliprole,sedaxane,and benzpyrimoxan) in seven animal-derived foods(chicken,beef,eggs,fish,milk,fat,and pork liver).Sample pretreatment,chromatographic,and mass spectrometric conditions were optimized.The samples were extracted with 90% acetonitrile and cleaned up with ultrasonic extraction and dispersive solid-phase extraction,and then determined by HPLC-MS/MS.Good linearity was observed for the seven pesticides over the concentration range of 0.10-10 ng/m L,with correlation coefficients r≥0.99.The limits of quantification(LOQs) of the method were in the range of 0.50-5.0 μg/kg(S/N>10).The sample recoveries at three different spiked concentrations ranged from 62.73% to 117.62%.Relative standard deviations for precision and reproducibility were within 20%(n=5).This method features rapid and simple pretreatment,high sensitivity,and excellent accuracy,meeting the requirements for the detection of seven new pesticide residues in animal-derived foods.
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基本信息:
DOI：10.13526/j.issn.1006-6144.2025.08017
中图分类号:TS207.53;O657.63
引用信息:
[1]孙千然,陈均,陈祥贵,等.高效液相色谱-串联质谱法测定动物源性食品中7种新型杀虫剂和杀菌剂[J].分析科学学报().DOI:10.13526/j.issn.1006-6144.2025.08017.
基金信息:
国家重点研发计划项目(2022YFF1100804)
2026-08-11
2026-08-11
2026-08-11