超高效液相色谱-串联质谱法测定鸡肉、鸡蛋中氟苯尼考和氟苯尼考胺残留

Determination of florfenicol and florfenicol amine residues in chicken and hen eggs by ultra performance liquid chromatography tandem mass spectrometry

中文关键词:  氟苯尼考  氟苯尼考胺  鸡肉  鸡蛋  超高效液相色谱-串联质谱法

英文关键词:florfenicol  florfenicol amine  chicken  hen eggs  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-串联质谱准确测定鸡肉、鸡蛋中氟苯尼考和氟苯尼考胺残留的分析方法。方法 鸡肉和鸡蛋样品加入D5-氯霉素内标, 经氨化乙酸乙酯混合溶液超声离心提取, 提取液减压蒸馏浓缩后, C18固相萃取柱净化处理, 采用超高效液相色谱-串联质谱法对氟苯尼考和氟苯尼考胺同时进行检测。 结果 氟苯尼考线性范围为0.2~20 μg/L, 检出限为1.0 μg/kg, 定量限为3.0 μg/kg, 方法回收率为88.0%~108.0%, 相对标准偏差为4.7%~6.4%; 氟苯尼考胺线性范围为0.2~20 μg/L, 检出限为1.0 μg/kg, 定量限为3.0 μg/kg, 方法回收率为76.0%~93.1%, 相对标准偏差为4.1%~7.2%。结论 本方法精确、重现性好, 适用于鸡肉、鸡蛋中氟苯尼考和氟苯尼考胺残留量的测定。

英文摘要:

      Objective To establish a method for the determination of florfenicol and florfenicol amine residues in chicken and hen eggs by ultra performance liquid chromatography-tandem mass spectrometry. Methods Chicken and hen eggs samples were added to the internal standard of D5-chloramphenicol and extracted by ultrasonic centrifugation with ammoniated ethyl acetate mixed solution. After the extract was concentrated under reduced pressure, purified by the C18 solid-phase extraction column, florfenicol and florfenicol amine residues were simultaneous determined by ultra performance liquid chromatography tandem mass spectrometry. Results The linear range of florfenicol was 0.2–20 μg/L, the detection limit was 1.0 μg/kg, the limit of quantification was 3.0 μg/kg, the method recoveries were 88.0%–108.0%, and the relative standard deviations were 4.7%-6.4%. The linear range of florfenicol amine was 0.2–20 μg/L, the detection limit was 1.0 μg/kg, the limit of quantification was 3.0 μg/kg, the method recoveries were 76.0%–93.1%, and the relative standard deviations were 4.1%–7.2%. Conclusion The method is accurate and reproducible, and is suitable for the determination of florfenicol and florfenicol amine residues in chicken and hen eggs.