通过式固相萃取净化-液相色谱-串联质谱法测定豆芽中10种喹诺酮类抗生素

Simultaneous determination of ten quinolones in bean sprouts by solid phase extraction purification and ultra performance liquid chromatography-tandem mass spectrometry

建立了超高效液相色谱-串联质谱(UPLC-Ms/Ms)快速检测豆芽中10种喹诺酮类抗生素(QNs)的方法。样品用乙腈-0.1%甲酸水溶液提取后,经PRiME HLB快速净化,氮吹浓缩后,用电喷雾离子源正离子-多反应监测(MRM)模式串联质谱进行检测。在0.25~100μg/L范围内,10种目标物的线性关系良好,其相关系数均大于0.997。方法对两种豆芽基质进行前处理并测定,检出限为1.0μg/kg和2.0μg/kg,定量限为3.0μg/kg和6.0μg/kg。回收率实验结果表明:10种目标物回收率范围为78.1%~106.4%,RSD<8.1%。方法能有效地避免杂质的干扰。

An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method coupled with PRi ME HLB solid phase extraction(SPE)for the simultaneous determination of ten quinolones(QNs)in bean sprouts was developed.The samples were extracted with 0.1%formic acid-acetonitrile,and cleaned by PRi ME HLB SPE.The samples were analyzed in electrospray positive ion mode and multiple reaction monitoring(MRM)mode.The linear relatimships of 10 QNs were good in the ramge of 0.25-100μg/L with correlation coefficients greater than 0.997.The limits of detection(LODs)were 1.0μg/kg and 2.0μg/kg,the limits of quantification(LOQs)were 3.0μg/kg and 6.0μg/kg,respectively.The recoveries at three spiked levels(2,200 and 100μg/kg)ranged from 78.1%to 106.4%with relative standard deviation(RSDs)between 1.1%and 8.1%.The established method can be applied to the determination of the 10 QNs in bean sprouts.