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固相萃取小柱-超高效液相串联质谱测定牛奶中氯霉素
Determination of Chloramphnicol in Milk by SPE-Ultra Performance Liquid Chromatography/Triple Qudrupole Tandem Mass Spectrometry
【摘要】 建立可靠的前处理方法,采用超高效液相色谱-串联质谱法检测牛奶中氯霉素。样品经乙酸乙酯提取,分析了分别经C18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。结果表明,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0.01、0.25、1.00μg/kg 3个加标水平下回收率分别为71.0%、53.8%、50.4%。本法灵敏度高、重复性好,可满足牛奶样品中痕量氯霉素残留的测定。
【Abstract】 To establish a reliable pretreatment method for chloramphnicol in milk with ultra performance liquid chromatography/triple qudrupole tandem mass spectrometry. The sample was extracted by ethyl acetate, then the results was analysed after C18 and MCS cartridge purification. The objective compounds were separated using Syncronis C18 column(100×2.1 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). The results showed that MCS cartridge had good recovery rate. The detection limit of chloramphnicol was 0.004μg/kg, limit of quantitation was 0.01μg/kg, the average recoveries for spiked levels of 0.01, 0.25, 1.00μg/kg were 71.0%, 53.8%, 50.4%. The method is suitable for the detection of chloramphnicol residual in milk.
【Key words】 chloramphnicol; solid phase extraction colum; ultra performance liquid chromatography/triple qudrupole tandem mass spectrometry; milk;
- 【文献出处】 中国乳品工业 ,China Dairy Industry , 编辑部邮箱 ,2020年03期
- 【分类号】O657.63;TS252.7
- 【被引频次】7
- 【下载频次】180