LC-MS/MS测定牛奶中氯霉素和四环素类抗生素

Chloramphenicol and Tetracyclines in Milk by LC-MS/MS

建立了超高效液相色谱-串联质谱法（UPLC-MS/MS）同时测定牛奶中四环素、土霉素、金霉素、强力霉素和氯霉素残留量的方法。牛奶样品用EDTA-2Na-Mcllvaine缓冲液提取,经Pro Elut PLS固相萃取柱富集净化后,用10%甲醇-乙酸乙酯洗脱。采用Thermo Hypersil Gold色谱柱（100 mm×2.1 mm×1.9μm）分离,ESI正负离子切换扫描模式分段采集测定。样品的加标回收率为81.5%~115.1%,相对标准偏差（RSD）不大于10%（n=6）。氯霉素的检出限为0.01μg/kg,四环素类的检出限为1~2μg/kg。该方法灵敏、可靠、准确,可用于同时检测牛奶中的氯霉素和四种四环素类药物残留。

A method for simultaneous determination of tetracycline, oxytetracycline, chlortetracycline, doxycycline and chloramphenicol in milk sample was developed by ultra performance liquid chromatography-electrospray tandem mass spectrometry. Milk samples were extracted by EDTA-2Na-Mcllvaine buffer. Sample solution, which was concentrated and purified by Pro Elut PLS solid-phase extraction column, was eluted by 10% methanol-ethyl acetate. The separation was performed on a Thermo Hypersil Gold（100 mm×2.1 mm×1.9 μm） column, and was determinated by periodic polarity-swithing. The recovery rates of the spiked sample in the range of 81.5%~115.1% with the relative standard deviation（RSD） were less than 10%（n=6）. The detection limits were 0.01 μg/kg for chloramphenicol and 1~2 μg/kg for tetracyclines. This method was sensitive, reliable, accurate, and could be successfully applied to the simultaneous detection for chloramphenicol and four kinds of tetracyclines in milk.