液相色谱-串联质谱法同时测定水产品中10种喹诺酮类药物残留

Simultaneous Determination of 10 Quinolones Aquatic Products by Liquid Chromatography-tandem Mass Spectrometry

目的:建立通过高效液相色谱-串联质谱法分析方法测定水产品中10种喹诺酮类药物残留的分析方法。方法:样品加入1%甲酸-乙腈后,使用漩涡混合和超声波提取,经EclipsePlus C18色谱柱(RRHD 50 mm×2.1 mm,1.8μm)分离后,采用0.1%甲酸水(A)、甲醇(B)和乙腈(C)作为流动相进行梯度洗脱,质谱(ESI+)采用多反应离子监测模式。结果:10种喹诺酮类药物在2~100μg·L-1范围内线性关系良好,r>0.9981,检出限为0.5~1.0μg·kg-1,定量限为1.5~2.5μg·kg-1,不同加标水平的平均回收率为81.2%~112.6%,相对标准偏差为2.8%~8.6%。结论:该方法准确度高、重复性好,可满足水产品中喹诺酮的检测需求。

Objective:To establish a method for the determination of 10 quinolones residues in aquatic products by HPLC-MS/MS.Methods:1%formic acid acetonitrile was added into the sample,and then the sample was extracted by vortex mixing and ultrasonic extraction.After separation on an eclipse plus C18 column(RRHD 50 mm×2.1 mm,1.8μm),gradient elution was performed with 0.1%formic acid water(A),methanol(B)and acetonitrile(C)as mobile phases.Mass spectrometry(ESI+)was monitored by multiple reaction ions.Results:The linear range of 10 quinolones was 2~100μg·L-1,R>0.9981,the detection limit was 0.5~1.0μg·kg-1,and the limit of quantification was 1.5~2.5μg·kg-1.The average recoveries were 81.2%~112.6%and the relative standard deviations were 2.8%~8.6%.Conclusion:The method has high accuracy and good repeatability,which can meet the detection requirements of quinolone in aquatic products.