超高效液相色谱-串联质谱法测定鸡肉和猪肉中利尿剂残留量

薛颖; 花锦; 高浩; 杜利君; 徐瑶; 黄立亭; 王嘉妮

doi:10.13386/j.issn1002-0306.2020050206

超高效液相色谱-串联质谱法测定鸡肉和猪肉中利尿剂残留量

Determination of Residues of Diuretics in Chicken and Swine by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

摘要

摘要: 目的：建立测定鸡肉和猪肉中违禁添加物呋塞米、螺内酯和布美他尼含量的超高效液相色谱-串联质谱法。方法：样品用乙酸乙酯提取后，经C₁₈粉净化。色谱柱为Hypersil GOLD C₁₈（1.9 μm，2.1 mm×50 mm），流动相为乙腈和0.1%甲酸水，梯度洗脱，流速为0.4 mL/min，柱温为40℃。采用电喷雾正负离子同时扫描，多反应监测模式（MRM）进行质谱检测。结果：3种利尿剂在1.0~500.0 μg/L浓度范围内线性关系良好（r>0.996）；平均加标回收率67.3%~111.6%，方法检出限均为0.5 μg/kg，定量限均为1.0 μg/kg。结论：该方法简便、准确，可作为鸡肉和猪肉中利尿剂快速检测的方法。

Abstract: Objective:An ultra-high performance liquid chromatography-tandem mass spectrometry method for detection of furoxime,spironolactone and bumetanilan in chicken and swine,which were banned in animal-derived foods,was established. Methods:The samples were purified with C₁₈ powder after the extraction of ethyl acetate. The chromatographic column was Hypersil GOLD C₁₈(1.9 μm,2.1 mm×50 mm).Mobile phase was acetonitrile and 0.1% formic acid water. The flow rate was 0.4 mL/min,and the column temperature was 40 ℃. The electrospray was operated in both positive and negative mode at the same time and the samples were detected by multiple reaction monitoring(MRM).Results:The liner relations of the three diuretics were good within the concentration range of 1.0~500.0 μg/L(r>0.996). The average standard recovery rate was 67.3%~111.6%. Limits of detection of the method were 0.5 μg/kg and limits of quantification were 1.0 μg/kg. Conclusion:This method is simple and accurate,and can be used as a rapid method for detection of diuretics in chicken and swine.