超高效液相色谱-串联质谱法测定猪肉中氯霉素类兽药残留量

Determination of chloramphenicol residues in pork by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  猪肉  氯霉素  甲砜霉素  氟苯尼考

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  pork  chloramphenicol  thiamphenicol  florfenicol

中文摘要:

      目的 建立超高效液相色谱-串联质谱法同时测定猪肉中氯霉素、甲砜霉素、氟苯尼考3种氯霉素类兽药残留量的分析方法。方法 样品用氨化乙酸乙酯超声提取, 提取液蒸干后用水复溶, 采用电喷雾离子化, 负离子扫描和多反映监测模式(multi reaction monitor, MRM)检测, 以保留时间和特征离子对定性, 外标法定量。结果 氯霉素和氟苯尼考在0.05~1.50 ng/mL, 甲砜霉素在0.25~7.50 ng/mL的范围内呈现良好的线性关系, 相关系数(r)均大于0.99; 方法检出限为0.1~0.5 μg/kg; 3种氯霉素类药物添加水平为0.1~5.0 μg/kg时, 平均回收率为90.8%~108.2%, 相对标准偏差为2.4%~9.8% (n=6)。结论 本方法样品前处理简单, 准确性、精密度和灵敏度均较好, 适用于猪肉中氯霉素类药物残留检测。

英文摘要:

      Objective To establish a method for the determination of 3 chloramphenicol compounds (chloramphenicol, thiamphenicol, florfenicol) in pork by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted with adding ammonia ethylacetate, and the extract was evaporated and re-dissolved with water. The target compounds were detected under ESI-and MRM mode, identified by retention time and the ration of characteristic ions, and quantified by external standard method. Results Chloramphenicol and florfenicol showed a good linearity in the range of 0.05 ng/mL to 1.50 ng/mL and thiamphenicol was in the range of 0.25 ng/mL to 7.50 ng/mL. The correlation coefficients of the 3 compounds were above 0.99. The limit of detection was in the range from 0.1 μg/kg to 0.5 μg/kg. The average recoveries of pork samples at spiked levels from 0.1 μg/kg to 5.0 μg/kg were between 90.8% and 108.2% , and the relative standard deviations (n=6) were between 2.4% and 9.8%. Conclusion This method is simple, accurate, precise and sensitive, and suitable for detecting chloramphenicol residue in pork.