采用高效液相色谱同时检测水产品中孔雀石绿、结晶紫及无色孔雀石绿和无色结晶紫的残留量,样品经提取、净化处理后所得残渣用乙腈溶解后,通过采用C18色谱柱,以乙腈(A)和pH 3.0的0.02 mol·L-1磷酸二氢钾缓冲溶液(B)按不同比例混合进行梯度淋洗,实现孔雀石绿、结晶紫及其代谢物的分离.用自制的二氧化铅柱氧化无色孔雀石绿及无色结晶紫.在588 nm波长处,测定4种物质的质量浓度在0.3~6.0 mg·L-1范围内与其峰面积呈线性关系,相对标准偏差(n=6)小于2.5%,检出限(3S/N)小于1.9 μg·kg-1,分析时间20 min.以凤尾鱼罐头为基体进行回收试验,方法的回收率在71.5%~88.6%范围.

HPLC was applied to the simultaneous determination of residual amounts of malachite green,crystal violet and their leuco-products in aquatic products.The sample was extracted with acetonitrile and purified by extraction with CH2Cl2 and passing through SPE column of acidic aluminum oxide.The column was eluted with acetonitrile,and the eluate was evaporated to near dryness by rotary evaporation.The residue was taken up with 1.0 mL of acetonitrile which was used for HPLC analysis.The C18 column was used as the stationary phase,and solutions of acetonitrile (A) and 0.02 mol·L-1 KH2PO4 (adjusted to pH 3.0 with H3PO4) (B) mixed in different ratio by volume were used as the mobile phase in gradient elution.A self-made PbO2 oxidation column was used for on-line oxidation of the leuco bases of malachite green and crystal violet.Linear relationships between values of peak area and mass concentration of the 4 compounds were found in the same range of 0.3-6.0 mg·L-1,with their detection limits (3S/N) less than 1.9 μg·kg-1.Array diode detection at 588 nm was adopted,values of RSD′s (n=6) found for the 4 compounds were all less than 2.5%.Sample of canned archovies was analyzed by this method,and test for recovery was made on this matrix by standard addition method giving results in the range of 71.5% to 88.6%.