猪肉中15种喹诺酮类药物残留的高效液相色谱-串联质谱法研究  

Simultaneous determination of 15 quinolone residues in meat using high performance liquid chromatography-tandem mass spectrometry

作　　者：张志刚 张洁[2] 刘宗保[3] 

机构地区：[1]肉食品安全生产技术国家重点实验室,食品安全与营养协同创新中心,厦门银祥集团有限公司,福建厦门361100 [2]中国科学院城市环境研究所,福建厦门361100 [3]华南理工大学轻工与食品学院,广东广州510640

出　　处：《广东农业科学》2013年第24期91-95,共5页Guangdong Agricultural Sciences

基　　金："十二五"国家科技支撑计划项目(2012BAD28B 09);国家"973"计划项目(2012CB723705)

摘　　要：利用高效液相色谱-电喷雾串联质谱建立了猪肉中15种喹诺酮类药物残留的同时、快速分析方法。猪肉样品中残留药物用1％乙酸-乙腈均质提取，浓缩后用0．1％甲酸-乙腈定容，正己烷脱脂，用Kinetex C18色谱柱（100mm×2．1mm．2．6μm）分离，以0．1％甲酸-乙睛作为流动相梯度洗脱．采用基于正离子扫描的MRM监测模式，用保留时间和离子对（母离子和碎片离子）定性，响应值高的碎片离子作为定量离子，基质匹配外标法定量。结果表明，15种喹诺酮类药物在l～500μg／kg范围内具有良好的线性关系，定量限在1～8μg／kg之间。在3个添加水平下，加标回收率为60．1％-91.4％，相对标准偏差为0．42％～6．28％。该方法操作简便、灵敏度高、特异性好，可用于猪肉中喹诺酮类药物残留的高通量检测。A high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） method was developed for the simultaneous and fast determination of 15 representative quinolones in meat. The quinolone residues were extracted with acidic acetonitrile. The extract was concentrated and reconstituted with small volume of acidic acetonitrile, and then defatted using hexane, ready for HPLC-MS/MS analysis. Chromatographic separation was performed on a Kinetex C18 （100 mm×2.1 mm, 2.6 μm） column using a gradient elution with water （0.1% formic acid） and acetonitrile as mobile phases. Mass spectrometer was operated in multiple reaction monitoring of positive ionization mode. The qualitative analysis was done by using retention time and diagnostic ion pairs （parent ion and two daughter ions）. The daughter ion with high signal was used for quantitation analysis. The targeted quinolones presented good linearity from 1 to 500 μg/kg. The limits of quantitation ranged from 1 to 8 μg/kg. The average recoveries at three spiked levels ranged from 60.1% to 91.4% with relative standard deviations of 0.42% -6.28%. The developed method has high sensitivity and selectivity, and is easy to operate, therefore is suitable for the routine high throughput analysis of quinolones in meat.

关 键 词：猪肉 喹诺酮 液相色谱 质谱 残留 

分 类 号：O657.63[理学—分析化学]