液相色谱-串联质谱法检测蜂蜜中氟苯尼考及其代谢物残留量

Determination of florfenicol and its metabolite residues in honey by liquid chromatography-tandem mass spectrometry

中文关键词:  液相色谱-串联质谱法  氟苯尼考  氟苯尼考胺  蜂蜜

英文关键词:liquid chromatography-tandem mass spectrometry  florfenicol  florfenicol amine  honey

中文摘要:

      目的 建立液相色谱-串联质谱法检测蜂蜜中氟苯尼考及其代谢物残留量的分析方法。方法 样品经氨化乙酸乙酯提取, 通过DPC-2固相萃取柱净化, 采用Poroshell 120 EC-C18柱分离, 以10 mmol/L乙酸铵溶液-乙腈为流动相进行梯度洗脱, 电喷雾正/负离子切换, 多反应监测模式检测, 同位素内标法定量。结果 氟苯尼考在0.2~30 μg/L时具有良好的线性关系, 相关系数大于0.999, 检出限为0.05 μg/kg, 回收率为85.5%~116.3%, 相对标准偏差小于10%。氟苯尼考胺在1~30 μg/L时具有良好的线性关系, 相关系数大于0.999, 检出限为0.3 μg/kg, 回收率为85.6%~113.5%, 相对标准偏差小于10%。结论 该方法快速、准确、灵敏, 适用于蜂蜜中氟苯尼考及其代谢物残留量的测定。

英文摘要:

      Objective To establish a method for determination of florfenicol and its metabolite florfenicol amine in honey by liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with ammoniated ethyl acetate, and cleaned with DPC-2 SPE column. The target analytes were separated on a Poroshell 120 EC-C18 column with gradient elution using a mobile phase consisting acetonitrile and 10 mmol/L ammonium acetate solution. The samples were determined by mass spectrometry with electrospray ion source in the positive and negative mode, monitored by the multiple reaction monitoring mode, and then quantified by the matrix matching of internal standard calibration. Results Florfenicol had a good linear relationship at 0.2-30 μg/L, and the correlation coefficient was greater than 0.999. The limits of detection were 0.05 μg/kg, the recoveries were 85.5%?116.3%, and the relative standard deviations were less than 10%. The florfenicol amine had a good linear relationship at 1? 30 μg/L, and the correlation coefficient was greater than 0.999. The limits of detection were 0.3 μg/kg, the recoveries were 85.6%?113.5%, and the relative standard deviations were less than 10%. Conclusion The method is rapid, sensitive and accurate, and suitable for the determination of florfenicol and its metabolites in honey.