提出了固相微萃取-高效液相色谱法测定水中孔雀石绿的含量。为使固相微萃取达到更高的效率,选择85 μm的聚丙烯酸酯(PA)涂层萃取纤维,萃取时间为15 min。以Shim-pack VP-ODS C18色谱柱为固定相分离,用pH 4.5的50 mmol·L-1乙酸铵溶液与乙腈按体积比为20比80混合的溶液为流动相进行洗脱,在波长595 nm处进行测定。孔雀石绿的质量浓度在0.05~2 mg·L-1范围内呈线性,检出限(3S/N)为0.003 mg·L-1。以鱼塘水为基体进行回收试验,方法的回收率在98.1%~109.6%之间。

HPLC with sample treatment by solid phase micro-extraction (SPME) was applied to the determination of malachite green in water samples. To attain a higher efficiency in SPME, the 85 μm PA coating was applied to the micro-extractor, and the extraction was carried out for 15 min. The Shim-pack VP-ODS C18 column was used as the stationary phase, and a mixture of 50 mmol·L-1 ammonium acetate solution of pH 4.5 and acetonitrile (20+80) was used as the mobile phase for elution. Detection at 595 nm was adopted. Linearity range of malachite green was kept in the range of 0.05-2 mg·L-1, with detection limit (3S/N) of 0.003 mg·L-1. A sample of fish pond water was analyzed by this method, and test for recovery was made on this sample as matrix by standard addition method giving results in the range of 98.1%-109.6%.