液质联用检测鱼肉中氟苯尼考和氟苯尼考胺的残留量.PDF

※分析检测 食品科学 2010, Vol. 31, No. 12 219 李莹莹，宋永青，赵 榕，牛晋阳，郭文萍 ( 中国肉类食品综合研究中心，北京 100068) ：建立同时测定鱼肉中氟苯尼考和氟苯尼考胺的液质联用检测方法(HPLC-MS/MS) 。样品采用碱性乙酸乙 酯提取，正己烷脱脂，电喷雾离子源正负模式切换，多反应监测(MRM) ，内标法定量。检出限分别为氟苯尼考 1 μg/kg ，氟苯尼考胺5 μg/kg 。低、中、高3 水平的加标回收率在87.0%～110.4% 之间，相对标准偏差均小于 6 . 2 % 。该方法前处理简便快速，分s 析速度快，灵敏度高。 ：氟苯尼考；氟苯尼考胺；液质法；鱼肉 HPLC-MS/MS Determination of Florfenicol and Florfenicol Amine Residues in Fish LI Ying-ying ，SONG Yong-qing，ZHAO Rong ，NIU Jin-yang ，GUO Wen-ping (China Meat Research Center, Beijing 100068, China) Abstract：A HPLC-MS/MS method was established for the simultaneous determination of florfenicol (FF) and florfenicol amine (FA) residues in fish. Samples were extracted with alkalinified ethyl acetate and cleaned up by liquid-liquid extraction with n-hexane. Both positive and negative electrospray ionization sources were selected and multiple reaction monitor (MRM) mode was used. Internal standard method was used for quantification. The limits of detection of the method established were 1 μg/kg for FF and 5 μg/kg for FA. Average recovery rates for FF and FA spiked at low, medium and high levels ranged from 87.0% to 110.4%, with a relative standard deviation of less than 6.2%. The method is simple, fast, efficient and highly selective. Key words ：florfenicol ；florfenicol amine ；HPLC-MS/MS method ；fish 中图分类号：O657.63 文献标识码：A 文章编号：1002-6630(2010)12-0219-04 氟苯尼考又称氟甲砜霉素，是氯霉素的第三代产 有很多报道[7-11] ，但关于同时测定氟苯尼考和氟苯尼考胺 品，广泛用于猪、牛、鱼及禽类等多种动物的感染性 残留的国内外报道较少，报道的方法主要有液相色谱紫 [12] [13] [14-15] [16-17] 疾病的防治，具有抗菌谱广、抗菌活性强等良好的药 外法 、液相色谱荧光法 、气质