高效液相色谱-电喷雾质谱法测定牛肉中3种氟喹诺酮药物残留

Determination of Fluoroquinolone Residues in Beef by High Performance Liquid Chromatography-Electrospray Ionization Mass Spectrometry

采用高效液相色谱-电喷雾质谱(HPLC-ESI-MS)建立牛肉中3种氟喹诺酮类药物(环丙沙星、恩诺沙星和沙拉沙星)残留的分析测定方法。试样经酸化甲醇萃取后直接用于分析,内标法定量。在1～20pg/μl范围内,3种氟喹诺酮药物的线性相关系数均大于0.992。在16.7～50.0μg/kg添加水平内,3种化合物的加标回收率为75.2%～96.3%,相对标准偏差为2.5%～8.3%,检出限为8～19μg/kg。这一检测限远低于我国农业部、JECFA以及欧盟等规定的牛肉组织中氟喹诺酮类药物的最大残留限量(MRL)。该方法简便、快速,可用作动物可食性产品中氟喹诺酮类药物残留分析确证的参考。

A method for analyzing three fluoroquinolone drug residues （ciprofloxacin, enrofloxacin and sarafloxacin） in beef was developed by high performance liquid chromatography-electrospray ionization mass spectrometry （HPLC-ESI-MS）. Samples were extracted with acidified methanol and quantified with the addition of internal standards. An excellent linear was revealed in the range from 1 to 20 pg/μl for three fluoroquinolones with a correlation coefficient of over 0.992. The average spike recovery rates at the levels from 16.7 to 50.0μg/kg were in the range of 75.2%-96.3% with a relative standard deviation of 2.5%-8.3%. In addition, the detection limit was 8- 19μg/kg, which was much lower than the maximum residue limit （MRL） in beef issued by the Ministry of Agriculture of China, the Department of JECFA and the European Union. This method is simple, rapid and can be used as the reference for the identification and quantification of fluoroquinolone drug residues in edible animal-derived products.