QuEChERS净化-高效液相色谱串联质谱法快速筛查乳制品中10种喹诺酮类抗生素

Rapid Determination of 10 Quinolones in Dairy Products by QuEChERS Purification and High Performance Liquid Chromatography Tandem Mass Spectrometry

建立了乳制品中10种喹诺酮类抗生素的QuEChERS净化-高效液相色谱串联质谱快速筛查方法。将QuEChERS试剂加入待测乳制品中,旋涡混匀离心后将上清液转移至含无水硫酸镁及氯化钠的离心管中,取上层乙腈2.0 mL氮气吹干后用流动性初始比例定容,以0.1%甲酸水及甲醇-乙腈混合溶液为流动相梯度分离洗脱,电喷雾离子源正离子模式(ESI+)进行多反应监测扫描。结果显示10种喹诺酮类化合物在测定浓度范围内线性关系良好,各测定组分相关系数r≥0.998,空白样品在低、中、高3个浓度添加下测定方法平均回收率范围在63.2%~96.7%之间,精密度范围为4.32%~11.42%之间,10种喹诺酮化合物的方法检出限为1.0μg/kg,定量限为3.0μg/kg。该方法具有灵敏度高,精密度良好,相对于固相萃取净化方法具有前处理简单的特点,适用于乳制品中10中喹诺酮化合物的定量筛查检测。

To establish a method for analysis of 10 quinolones in dairy products by QuEChERS purification coupled with high performance liquid chromatography tandem mass spectrometry.The dairy products was purified by QuEChERS extraction.The supernatant was transferred to tube containing anhydrous magnesium sulfate and sodium chloride after vortex and centrifugation,then 2.0 mL acetonitrile was concentrated by nitrogen and redissolve with the initial mobile phase.Gradient elution was performed using 0.1%formic acid solution and methanol acetonitrile mixed solution and separated by Hypersil Gold column.Selective ion scanning detection was employed at positive electrospray ionization.The result showed good linear relationship between the concentration range,and the components correlation coefficient r≥0.998.Blank samples were added at three concentrations of low,medium and high,and the average recovery of the method was in the range of 63.2%-96.7%,precision range 4.32%-11.42%。The detection limits(LOD)of the method were 1.0μg/kg and the quantification limits(LOQ)was 3.0μg/kg.This method has high sensitivity and good precision,simple pretreatment compared with the SPE purification method and it is suitable for determination of 10 quinolones in dairy products。