超高效液相色谱-串连质谱法同时测定牛奶中7种四环素和14种喹诺酮类药物残留

Simultaneous determination of tetracyclines and quinolones residues in milk by ultra performance liquid chromatography-tandem mass spectrometry

目的采用超高效液相色谱-电喷雾串连四极杆质谱,正离子多反应监测(MRM)模式同时测定牛奶中7种四环素和14种喹诺酮残留。方法试样经EDTA-McIlvaine(pH=4.0)缓冲溶液提取,用HLB固相萃取柱浓缩和净化,Waters ACQUITY UPLCTMBEH C18色谱柱分离,以甲醇-乙腈混和液和含0.2%甲酸的水溶液为流动相梯度洗脱,进行测定。结果该方法的平均回收率为89.2%～119.1%,相对标准偏差为1.8%～19.0%,方法的定量限介于0.1～0.5μg/kg。结论该方法灵敏度高,重现性良好,适用于牛奶中多种抗生素的检测。

Objective A comprehensive analytical method based on ultra performance liquid chromatography-electrospray tandem mass spectrometry（UPLC-MS/MS） with positive mode has been developed for the simultaneous determination of seven tetracyclines and fourteen quinolones in milk.Methods Milk samples were extracted by EDTA-McIlvaine（pH=4.0） buffer solution and then purified and enriched by Oasis HLB solid phase extraction cartridges.The separation was performed on a Waters ACQUITY UPLCTM BEH C18 column（100 mm×2.1 mm i.d.,1.7μm） with gradient elution using methanol-acetontrile and water（containing 0.2% formic acid） at a flow rate of 0.2 ml/min.Results The average recoveries of this method for fortified samples were ranged from 89.2% to 119.1%,with relative standard deviations between 1.8% to 19.0%.The limits of quantification（LOQ） were ranged from 0.1 to 0.5 μg/kg.Conclusion Due to its high sensitivity and reproducibility,the method is suitable for the determination of seven tetracyclines and fourteen quinolones in milk samples.