牛奶和奶粉中氟胺烟酸残留量测定方法的研究

Research on Determination Method of Flunixin Residue in Bovine Milk and Milk Powder by HPLC-UV

研究了牛奶和奶粉中氟胺烟酸残留量的液相色谱-紫外分析方法。样品在酸性条件下酶解用乙腈提取后,经固相萃取柱净化,用配有紫外检测器的高效液相色谱测定,外标法定量。方法的最低检出限牛奶为5mg/kg,奶粉为40mg/kg;在2.5～160.0mg/kg浓度范围内,线性关系良好,相关系数r=0.9996,添加水平牛奶5.0～40mg/kg时,奶粉40.0～100mg/kg时,回收率在86.86%～100.32%,相对标准偏差(RSD)为1.986%～2.295%。

The method for the determination of flunixin residues in aquatic products is studied by HPLC-UV. Bovine milk is digested using β-glucuronidase.The enzyme digestion was extracted using acetonitrile,cleaned up with SPE col- umn.The solution was analyzed by LC-UV using external standard method. The detection limit of this method is 5μg/kg for bovine mill and 40mg/kg for mill power .The results showed a good linear （r=0.9996） in the concentration range of 2.5-160.0μg/kg,the average recoveries for spiked standards （5.0μg/kg-40μg/kg）and（40.0μg/kg-100.0μg/kg） were 86.86%- 100.32%,the relative standard deviations were 1.986%-2.295% in bovine mill and mill powder.