固相萃取-高效液相色谱法测定水产品中的苯巴比妥

建立水产品中苯巴比妥残留量测定的固相萃取-高效液相色谱方法。样品经乙酸乙酯提取，正己烷脱脂，通过C18固相萃取小柱富集和净化，高效液相色谱仪进行检测。苯巴比妥在0.05～4.0μg/mL内线性范围良好，相关系数为0.9999。当添加量在30～200μg/kg时，加标回收率在80.49%～102.42%，相对标准偏差为1.52%～10.15%，方法检出限10μg/kg，定量限30μg/kg。研究结果表明本方法操作简单、准确度高，能满足水产品中苯巴比妥残留量的测定及确证工作的需要。

Determination of Phenobarbital Residues in Fishery Products by SPE-HPLC

A solid phase extraction (SPE) coupled with high performance liquid chromatography (HPLC) method has been developed for the determination of phenobarbital residues in fishery products. Samples were extracted with ethyl acetate, defatted with n-hexane, and cleaned up on a C18 solid phase extraction cartridge before HPLC analysis. Over the concentration range of 0.05－4.0 μg/mL, a good linear response was observed for the fitted calibration curve of phenobarbital, with a coefficient of correlation of 0.9999. The average recovery rate of phenobarbital in four types of aquatic products varied from 80.49%－102.42% with relative standard deviation (RSD) of 1.52%－10.15%. The detection limit and quantification limit of this method was 10 μg/kg and 30 μg/kg, respectively. This method was simple and accurate and could meet the requirements for the determination and confirmation of phenobarbital residues in fishery products.