超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法测定牛奶中19种喹诺酮类抗生素

建立基于超高效液相色谱-四极杆/静电场轨道阱高分辨质谱筛查和确证牛奶中19种喹诺酮类抗生素的方法.牛奶样品经酸化乙腈提取并沉淀蛋白,PRiME HLB固相萃取柱净化,用Waters Acquity BEH C18柱(2.1 mm×100 mm,2.5μm)分离,以乙腈和0.1％甲酸水溶液进行梯度洗脱,在全扫描(full...

Determination of 19 Kinds of Quinolones in Milk by Ultra Performance Liquid Chromatography/ Quadrupole Obitrap High Resolution Mass Spectrometry

A rapid method was presented for the determination of 19 quinolone antibiotics in milk by ultra high performance liquid chromatography/quadrupole orbitrap high resolution mass spectrometry.Milk samples were extracted by acidified acetonitrile and purified by PRiME HLB solid phase extraction column,then separated by Waters Acquity BEH C18 column(100 mm×2.1 mm,2.5μm)using a binary solvent system composed of acetonitrile and water(0.1%formic acid)by gradient elution.The analytes were determined by quadrupole-orbitrap high resolution mass spectrometry in full-MS and data-dependent scan(ddMS2)mode.The results showed that mass accuracy error of the 19 quinolones were lower than 3.0×10-6,linear relationships were well in the range of 0.2-200 ng/mL for 19 antibiotics,and correlation coefficients were higher than 0.998.The LODs were in the range of 0.1-0.5μg/kg and the LOQs were in the range of 0.2-1.0μg/kg.With spike levels in the range of 0.2-10.0μg/kg,recovery of the method was in range of 62.1%-100.4%and relative standard deviations were lower than 10%.The method is simple,rapid,accurate,which is suitable for the rapid screening and quantitative analysis of 19 kinds of quinolones antibiotics in milk sample.