液相色谱-串联质谱法同时测定蜂蜜中4种四环素族抗生素及其3种差.PDF

232 2011, Vol. 32, No. 10 食品科学 ※分析检测 - 4 3 1 , 2 2 2 1 , 刘蓉蓉 ，吴黎明 ，周金慧 ，曾明华 * (1.安徽农业大学动物科技学院，安徽 合肥 230036 ；2. 中国农业科学院蜜蜂研究所，北京 100093) 采用液相色谱 - 质谱联用技术，建立同时测定蜂蜜样品中 4 种四环素族抗生素及其 3 种差向异构体的方法。 蜂蜜样品中残留的药物用 EDTA-McIlvaine 缓冲液提取，提取液依次经 OASIS HLB 及羧酸弱阳离子柱固相萃取柱富 集、净化后，用流动相洗脱。洗脱液经微孔滤膜过滤，用流动相甲酸水 - 乙腈梯度分离，电喷雾- 串联质谱进行 测定。在多反应监测模式下，22min 内7 种药物基本实现分离以及定性定量。样品在 10～500 μg/kg 添加范围内， 回收率均在64.9%～91.0% 之间，相对标准偏差(RSD)不大于 10.5%。土霉素及差向土霉素、四环素及差向四环素 的检测限为 1μg/kg ，金霉素及差向金霉素、强力霉素的检测限为2 μg/kg 。本方法灵敏、可靠，可用于蜂蜜中7 种 四环素类抗生素的同时检测(其中包括 3 种毒性代谢产物) 。 液相色谱 - 串联质谱法；蜂蜜；四环素类抗生素；差向异构体 Simultaneous Determination of 4 Tetracyclines and 3 Epimers in Honey by HPLC Coupled with Tandem MS 1,2 2 2 1, LIU Rong-rong ，WU Li-ming ，ZHOU Jin-hui ，ZENG Ming-hua * (1. School of Animal Science and Technology, Anhui Agricultural University, Hefei 230036, China； 2. Bee Research Institute, Chinese Academy of Agricultural Sciences, Beijing 100093, China) Abstract ：A method for simultaneous determination of 4 tetracyclines and 3 epimers in honey samples was developed by high performance liquid chromatography coupled with tandem mass spectrometry. The residues in honey samples were extracted by EDTA-Mcllvaine buffer, and cleaned up and condensed by OASIS hydrophilic-liphophilic balance (HLB) column and weak cation exchange (WCX and carboxylic acid) sequentially. Sample solution eluted from the WCX SPE column by mobile phase was filtered by micro-pours membrane, separated by LC-MS/MS with gradient elution using acetonitrile-formic acid solution as