摘要
建立了超高效液相色谱-串联质谱（UPLC-MS/MS）同时测定猪肌肉中13种喹诺酮类药物残留的方法.样品用Na2 EDTA-Mcllvaine缓冲溶液及磷酸盐缓冲液超声提取,HLB柱固相萃取,在电喷雾正离子模式下,以多反应监测（MRM）方式采集数据进行定性与定量分析.在5～200 μg/kg浓度范围内线性良好,相关系数均大于0.990;所检测的13种药物在5.0、50.0、100.0 μg/kg 3个浓度水平添加,回收率在64.55％～117.62％之间,日内变异系数小于14.28％,日间变异系数小于12.81％,检测限均为1.0 μg/kg,定量限均为5.0 μg/kg.本方法简便快速、灵敏可靠,适用于猪肌肉中喹诺酮类药物多残留的同时快速定性与定量测定.
A method was developed for the simultaneous determination of 13 quinolone （QNs） antibiobtics in swine muscle by ultra performance liquid chromatography tandem mass spectrometry （UPLC-MS/MS）.The analytes were extracted from the sample using Na2 EDTA-Mcllvaine buffer solution and phosphate buffer with ultrasonic bath and purified by solid-phase extraction （SPE） cartridge.Sample was analyzed in electrospray positive ion and multiple reaction monitoring（MRM） mode.Satisfied recoveries （64.55%-117.62%） of all the drugs are demonstrated in 5.0,50.0 and 100.0 μg/kg spiked levels with the RSD for intra-day and inter-day of 13 analytes less than 14.28% and 12.81%.Limit of detection （LOD） and limit of quantitation （LOQ） are 1.0 μg/kg and 5.0 μg/kg.The method is simple,accurate,sensitive and suitable for the determination of 13 quinolone（QNs） antibiobtics in swine muscle.
出处
《质谱学报》
EI
CAS
CSCD
北大核心
2014年第2期185-192,共8页
Journal of Chinese Mass Spectrometry Society
基金
北京农业职业学院院级课题(XY-YF-12-18)
食品质量安全"主动"控制技术项目(201203069-2)资助
