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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 method for the determination of olaquindox in aquatic products by solid phase extraction and high performance liquid chromatography was established. The homogenized aquatic samples were extracted with methanol solution and degreased with n-hexane. The solid phase extraction cartridge was directly purified and concentrated. The mobile phase was methanol solution with a volume fraction of 15%, the flow rate was 1.0 m L / min and Symmetryshield TM RP18 column separation, UV detector detection, external standard quantitative. The limit of detection (LOD) and limit of quantitation (LOQ) of the method were 0.02 mg / kg and 0.05 mg / kg, respectively. The linearity was good (r = 0.9999) in the range of 0.05-1.00 mg / L. The recoveries of different aquatic products ranged from 78% to 99.6% at the concentration of 0.05-1.00 mg / kg with the relative standard deviation of less than 7.7%. The method is suitable for batch quantitative detection of aquatic products samples.