固相萃取-高效液相色谱法测定禽蛋中斑蝥黄

Determination of cantharidate in eggs by SPE-high performance liquid chromatography

研究建立高效液相色谱测定禽蛋中斑蝥黄的方法,样品通过超声提取,过硅胶固相萃取柱净化,采用C18色谱柱(4.6mm×250mm,5μm)分离,用乙腈-0.1%甲酸(v/v=98∶2)等度洗脱,高效液相色谱法测定,外标法定量。在优化后色谱条件下,斑蝥黄在0.5mg/L^20mg/L浓度范围内,线性关系良好,相关系数R=0.9996,方法检出限可达0.05mg/kg,样品加标回收率为89.4%~97.2%,相对标准偏差(RSD)为2.36%~4.45%。本方法便捷、准确、灵敏,可以满足禽蛋中斑蝥黄的测定。

A HPLC method for the determination of cantharidate in eggs was established.The samples were extracted by ultrasound,purified by silica gel SPE column,separated by C18 column(4.6mm×250mm,5μm),eluted by acetonitrile-0.1%formic acid(v/v=98∶2),determined by HPLC,and quantified by external standard method.Under optimized chromatographic conditions,cantharidate had a good linear relationship in the concentration range of 0.5mg/L^20 mg/L,and the correlation coefficient was R=0.9996.The detection limit was 0.05mg/kg,the standard recovery of samples was 89.4%~97.2%,and the relative standard deviation(RSD)was 2.36%~4.45%.This method is convenient,accurate and sensitive,and can be used for the determination of cantharidin in eggs.