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采用QuEChERS-超高效液相色谱-串联质谱技术同时测定乳制品中磺胺类和喹诺酮类抗生素残留。样品加乙腈提取,经分散固相萃取净化后,采用WatersC18色谱柱分离,以乙腈和0.1%的甲酸水溶液为流动相进行梯度洗脱,采用电喷雾-正离子多反应监测模式,内标法定量。在1～200μg/L的质量浓度范围内,磺胺类和喹诺酮类抗生素的相关系数均大于0.9965,该方法的检出限在0.3～2.5μg/kg之间,定量限在1.0～7.5μg/kg之间。添加10、20、50μg/kg3个浓度水平,磺胺类和喹诺酮类抗生素的平均回收率在71.6%～120.7%之间,相对标准偏差在0.1%～7.2%之间。将该技术应用于市售多种类乳制品的测试,结果表明,该方法简便、快速、灵敏度高,适用于乳制品中磺胺类和喹诺酮类抗生素残留的同时测定。
Simultaneous Determination of Sulfonamides and Quinolones Residues in Dairy Products by QuEChERS - Ultra Performance Liquid Chromatography - Tandem Mass Spectrometry. The sample was extracted with acetonitrile and purified by dispersive solid-phase extraction. The residue was separated on a Waters C18 column by gradient elution with acetonitrile and 0.1% formic acid in water as the mobile phase. The electrospray ionization-positive ion multiple reaction monitoring . The correlation coefficient between sulfonamides and quinolone antibiotics was more than 0.9965 in the range of 1 ~ 200μg / L, the detection limit of this method was between 0.3 ~ 2.5μg / kg and the limit of quantification was 1.0 ~ 7.5μg / kg between. The average recoveries of sulfonamides and quinolones antibiotics were between 71.6% and 120.7% with relative standard deviations between 0.1% and 7.2% at the concentrations of 10, 20 and 50 μg / kg, respectively. The technology is applied to the testing of various types of dairy products on the market. The results show that the method is simple, rapid and sensitive. It is suitable for the simultaneous determination of sulfonamides and quinolone antibiotics residues in dairy products.