固相萃取-高效液相色谱法测定水产品中喹乙醇

Determination of olaquindox in aquatic products by HPLC using SPE

建立了固相萃取-高效液相色谱法测定水产品中喹乙醇的方法。匀浆后的水产品试样经甲醇溶液提取、正己烷除脂、固相萃取小柱直接净化浓缩后,以体积分数15%的甲醇溶液作为流动相,流速：1.0 m L/min,采用Symmetryshield TM RP18色谱柱进行分离,紫外检测器检测,外标法定量。方法的检出限和定量限分别为0.02 mg/kg和0.05 mg/kg,浓度在0.05~1.00 mg/L范围内,线性良好（r=0.9999）。添加浓度在0.05~1.00 mg/kg时,不同品种水产品的回收率在78%~99.6%之间,相对标准偏差小于7.7%。方法适合于水产品样品的成批定量检测。

A high performance liquid chromatographic（ HPLC） method was developed for the simultaneous determination of olaquindox in aquatic products. The olaquindox residues in samples were extracted by methanol aqueous solution,and degreased with hexane. The extract was cleanup by liquid-liquid extraction and solid phase extraction. A HPLC column of SymmetryshieldTMRP18（ 25 × 4. 6 mm i. d.,5 μm） was used with elution（ 1. 0 m L/min） by methanol-H2O（ 15 ＋ 85,V / V） and detection by HPLC-UV. The detection limit of0. 02 mg / kg,low limit of determination of 0. 05 mg / kg,concentration in the range of 0. 05 to 1. 00 mg / L（ r =0. 9999）,recoveries of 78% ~ 99. 6% were obtained for the method. RSD（ relative standard deviation） was less than 7. 7%. The method is easy to be operated,and has a good linear relationship,low detection limit. In addition,the recoveries conform to the determination of olaquindox in aquatic products. So the method is suitable for the batch quantitative detection of the aquatic products sample.