超高效液相色谱-串联质谱法测定乳饼中的氯霉素

Determination of chloramphenicol in rubing by ultra performance liquid chromatography/triple quadrupole tandem mass spectrometry

目的建立一种超高效液相色谱-串联质谱法(ultra high performance liquid chromatography tandem mass spectrometry,UPLC-MS/MS)检测乳饼中氯霉素的分析方法。方法样品经乙酸乙酯提取,分析了分别经C18(100 mm×2.1 mm,1.7μm)及MCS固相萃取柱净化、富集的结果;以乙腈-0.05%氨水为流动相,经C18色谱柱分离,采用多反应检测负离子模式进行定性及定量分析。结果MSC固相萃取柱具有较好的回收率,氯霉素的方法检出限为0.004μg/kg,方法定量限为0.01μg/kg,在0.10、0.50、1.00、10.00 ng 4个加标水平下回收率分别为76.4%、101%、62.4%、61.1%。结论本方法灵敏度高、重复性好,可满足乳饼样品中痕量氯霉素残留的测定。

Objective To establish a analysis method for chloramphenicol in rubing with ultra performance liquid chromatography/triple quadrupole tandem mass spectrometry.Methods The sample was extracted by ethyl acetate,then the results were analysed after C18 column and MCS cartridge purification.The objective compounds were separated using syncronis C18 column(100 mm×2.1 mm,1.7μm)with acetonitrile-water(0.05%ammonia)as mobile phase and analyzed by mass spectrometry in the negative electrospray ionization under multiple reaction monitoring mode(MRM).Results The results showed that MCS cartridge had good recovery rate.The detection limit of chloramphenicol was 0.004μg/kg,the limit of quantitation was 0.01μg/kg,the average recoveries for spiked levels of 0.10,0.50,1.00,10.00μg/kg were 76.4%,101%,62.4%,61.1%,respectively.Conclusion This method is sensitive and repeatable,which is suitable for the detection of chloramphenicol residual in rubing.