论文部分内容阅读
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 To determine the residues of seven tetracyclines and 14 quinolones in milk by ultra performance liquid chromatography-electrospray tandem mass spectrometry (ESI-MS / MS / MS) and positive ion multiple reaction monitoring (MRM) Methods The samples were extracted with EDTA-McIlvaine (pH = 4.0) buffer solution, concentrated and purified by HLB solid phase extraction column and separated on a Waters ACQUITY UPLC TMBEH C18 column. The mobile phase consisted of methanol-acetonitrile mixture and 0.2% formic acid in water Gradient elution, the determination. Results The average recoveries of this method ranged from 89.2% to 119.1% with relative standard deviations of 1.8% to 19.0%. The limits of quantification for this method ranged from 0.1 to 0.5 μg / kg. Conclusion The method has high sensitivity and reproducibility and is suitable for the detection of multiple antibiotics in milk.