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超高效液相色谱-串联三重四极杆质谱法测定鸭肉中26种兽药残留

超高效液相色谱-串联三重四极杆质谱法测定鸭肉中26种兽药残留

ISSN:2095-0381
2025年第16卷第11期
2025年专题:食品中有毒有害物质分析与监测
孙思1, 杨梅2, 刘太阳2, 刘文锋2, 汪忠荣3 SUN Si1, YANG Me1, LIU Tai-Yang1, LIU Wen-Feng2, WANG Zhong-Rong3

目的 建立超高效液相色谱-串联三重四极杆质谱法同时测定鸭肉中磺胺类、四环素类、氟喹诺酮类,共3类26种兽药残留的分析方法。方法 采用0.1%的甲酸-乙腈提取, QuEChERS净化剂除杂,经45℃水浴氮吹至近干后0.1%甲酸水-乙腈(1:1,V:V)定容,通过超高效液相色谱-串联三重四极杆质谱仪进行定性及定量检测分析。结果 26种兽药在2.0~300.0 ng/mL质量浓度范围内线性关系良好(r2≥0.9996),检出限为0.28~6.02μg/kg,定量限为11.28~15.03μg/kg。在不同浓度添加水平(5.0、50.0、300.0μg/kg)下26种兽药的平均回收率为75.08%~112.35%(n=15),相对标准偏差(relative standard deviations, RSDs)为1.25%~7.88%(n=15)。结论 该方法前处理操作简便,效率高,试剂耗材用量小,适用于大批量鸭肉样品中此3类26种兽药残留的初筛检测。

Objective To establish a method for the simultaneous determination of 26 kinds of veterinary drug residues in 3 categories including sulfonamide, quinolones and tetracyclines based on duck meat by ultra performance liquid chromatography-tandem triple quadrupole mass spectrometry. Methods The 0.1% formic acid acetonitrile extraction was used , QuEChERS purification agent was used to remove impurities. After nitrogen blowing in a 45 ℃ water bath to near dryness, the mixture was diluted with 0.1% formic acid water acetonitrile (1:1, V:V) and analyzed qualitatively and quantitatively using ultra performance liquid chromatography-tandem triple quadrupole mass spectrometry. Results The 26 kinds of veterinary drugs showed good linearity in the range of 2.0-300.0 ng/mL (r2>0.996), the limits of detection were 0.28 ~ 6.02 μg/kg, the limits of quantification were 11.28 ~ 15.03 μg/kg. The average recovery rates of 26 kinds of veterinary drugs at different concentration levels (5.0, 50, 300.0 μg/kg) were 75.08% ~ 112.35% (n=15), and the relative standard deviation (RSD) was 1.25% ~ 7.88% (n=15). Conclusion This method features simple pretreatment operations, high efficiency, and low consumption of reagents and materials. It is suitable for the preliminary screening and detection of 26 kinds of veterinary drug residues in 3 categories for large quantities of duck meat samples.

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ISSN:2095-0381
2025年第16卷第11期
2025年专题:食品中有毒有害物质分析与监测

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