超高效液相色谱串联质谱法测定液态奶中氯霉素、甲砜霉素和氟苯尼考含量

Determination of chloramphenicol, thiamphenicol and florfenicol in milk by ultra performance liquid chromatography-tandem mass spectrometry

目的建立超高效液相色谱串联质谱法测定液态奶中氯霉素、甲砜霉素和氟苯尼考的检测方法。方法样品经乙酸乙酯提取,用Oasis MCX柱净化。然后用WATERS ACQUITY UPLC BEH C18(2.1 mm×100 mm,1.7μm)进行分离,采用同位素内标法定量。结果在优化条件下,该方法中氯霉素的最低检出限为0.05μg/kg,定量限为0.1μg/kg,甲砜霉素和氟苯尼考的最低检出限为0.1μg/kg,定量限为0.3μg/kg,平均回收率为80.4%~105.4%,相对标准偏差为2.8%~8.4%。结论该方法灵敏度高、回收率好,具有良好的净化效果,提升检测效率,适用于液态奶中氯霉素、甲砜霉素和氟苯尼考的同时检测。

Objective To establish a method for the determination of chloramphenicol, thiamphenicol and florfenicol in milk by ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with ethyl acetate, followed by clean-up with Oasis MCX column, and then separated by WATERS ACQUITY UPLC BEH C18(2.1 mm×100 mm, 1.7 μm). Internal standard method was used to quantify. Results Under optimal conditions, the minimum detection limit of chloramphenicol was 0.05 g/kg, the quantitative limit was 0.15 g/kg, the minimum detection limits of thiamphenicol and florfenicol were 0.1 g/kg, and the quantitative limits were 0.3 g/kg. The average recoveries were 80.4%-105.4%, and the relative standard deviations were 2.8%-8.4%. Conclusion This method has high sensitivity, good recovery rate, good purification effect and improves the detection efficiency. It is suitable for the simultaneous detection of chloramphenicol, sulfoxycin and fluorophenicol in liquid milk.