分子印迹-固相萃取-高效液相色谱法测定鱼肉中的孔雀石绿

Determination of Malachite Green in Fish by HPLC Coupled with Molecular Imprinting Solid-Phase Extraction

以本体聚合法制备孔雀石绿(MG)分子印迹聚合物,并以此为填料,制作针对孔雀石绿的分子印迹固相萃取小柱。鱼肉样品经乙腈超声提取,提取液过分子印迹固相萃取小柱,用甲醇-乙酸(9+1)混合液洗脱,洗脱液采用Eclipse Plus C18色谱柱分离,以50mmol·L-1乙酸盐缓冲溶液-乙腈(4+6)混合液为流动相进行洗脱,检测波长为620nm。孔雀石绿的线性范围为1.00~50.0μg·L-1,检出限(3S/N)为0.62μg·kg-1。对空白鱼肉样品进行加标回收试验,回收率在86.6%~95.4%之间,测定值的相对标准偏差(n=5)在3.6%~6.8%之间。

Molecularly imprinted polymer for malachite green(MG)was synthesized by bulk polymerization and used as the absorbent for the solid phase extraction(SPE)column.The fish sample was extracted with acetonitrile.The extract was purified on the molecularly imprinted SPE column and eluted with a mixture of methanol and acetic acid.The eluent was separated on Eclipse Plus C18 column using a mixture of acetonitrile and50mmol·L-1 of acetate buffer solution as mobile phase.The detection wavelength was 620 nm.The linear range of MG was 1.00-50.0μg·L-1,with detection limit(3S/N)of 0.62μg·kg-1.The recovery rates measured by adding standard samples to blank fish sample were in the range of 86.6%-95.4% with RSD(n=5)in the range of and 3.6%-6.8%.