内标液相色谱-串联质谱法测定蜂蜜中氯霉素、甲砜霉素和氟苯尼考残留

Determination of chloramphenicol, sulfoxycin and fluorphenicol residues in honey by liquid chromatography-tandem mass spectrometry with interior label

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

英文关键词:honey  chloramphenicol  thiamphenicol  fluorphenicol  liquid chromatography tandem mass spectrometry

中文摘要:

      目的 建立液相色谱-串联质谱法测定蜂蜜中氯霉素、甲砜霉素和氟苯尼考的分析方法。方法 以氯霉素-D5为内标, 样品用乙酸乙酯提取, 提取液在45 ℃氮气吹至近干, 残渣用2 mL水溶解, 溶解液过Oasis HLB柱净化, 洗脱液在45 ℃氮气吹干, 50%甲醇水溶液定容, 后经正己烷脱色脱脂、PSA粉末吸附净化, 高速离心过膜后用串联四极杆检测。样液经过Agilent Eclipse XDB?C18色谱柱分离, 甲醇-水流动相梯度洗脱, 多反应监测扫描模式检测。采用内标法定量。结果 氯霉素在0.1~4.0 μg/kg、甲砜霉素和氟苯尼考在0~40.0 μg/kg呈良好的线性关系, 相关系数大于0.999, 回收率为93.7%~109.7%, RSD为0.7%~11.4%, 检出限为0.03~ 0.09 μg/kg, 定量限为0.1~0.3 μg/kg。结论 该方法准确、检出限低、重现性好, 适用于蜂蜜中氯霉素、甲砜霉素和氟苯尼考残留的检测。

英文摘要:

      Objective To establish a method for determination of chloramphenicol, sulfoxycin and fluorophenicol in honey by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods Chloramphenicol-D5 was used as the internal standard. The honey sample was extracted with ethyl acetate, the extract was blown to near dry at 45 ℃ with nitrogen, and the residue was dissolved with 2 mL water. The solution was purified by OASIS HLB column, the eluent was dried at 45 ℃ with nitrogen, and the volume was fixed with 50% methanol solution. The eluent was decolorized and degreased with N-hexane, and purified with PSA powder adsorption. The sample was separated by Agilent Eclipse XDB-C18 chromatographic column, and eluted by methanol-water mobile phase gradient. The eluent was detected by MRM scanning mode of ESI ion source. Chloramphenicol was quantified by internal standard method. Results Chloramphenicol showed a good linear relationship between 0.1?4.0 g/kg, as well assulfoxycin and flufenicol ranged from 1.0 g/kg to 40.0 g/kg. The correlation coefficient was greater than 0.999, recoveries were 93.7%?109.7%, RSDs were 0.7%?11.4%, the limits of detection were 0.03?0.09 μg/kg, and the limits of quantitative were 0.1?0.3 μg/kg. Conclusion This method is accurate, has low limit of detection and good reproducibility, and is suitable for the determination of chloramphenicol, sulfoxamicol and florfenicol residues in honey.