水中孔雀石绿的高效液相色谱测定法

Determination of Malachite Green in Water by High Performance Liquid Chromatography

目的建立淡水中孔雀石绿含量的高效液相色谱法测定分析方法。方法采用ZORBAXSB-C18(250mm×4.6mm,5μm)色谱柱,二氧化铅柱后氧化柱,流动相为0.1mol/L(pH=4.5)的乙酸铵溶液∶乙腈(体积比为20∶80),流速为1.5ml/min,紫外检测器波长为588nm。结果该方法在孔雀石绿浓度范围在0.1～4.0μg/ml时,r=0.99972。以峰面积(x)对质量浓度(y)做标准曲线,得到线性方程为:y=40.25x+1.99。根据3倍信噪比计算,最低检测限为0.02μg/L。向不含孔雀石绿的水样中分别加入2.0、10.0μg/L的孔雀石绿溶液进行高效液相色谱法的精密度、准确度试验,结果显示,平均回收率分别为98.5%,97.8%,RSD分别为11.2%,8.0%。结论本方法操作简单,回收率稳定,灵敏度高,适用于淡水中的孔雀石绿含量的检测,但不适用于无色孔雀石绿的检测。

Objective To develop a sensitive HPLC method for the determination of malachite green in fresh water. Methods The HPLC column of ZORBAX SB-C18 (250 mm×4.6 mm, 5 μm) was employed and acetonitrile and acetate buffer (0.1 mol/L, pH=4.5, V∶V=80∶20) were taken as the mobile phase. The samples were tested at wave length of 588 nm after post-column oxidation with PbO2 flowed at 1.5 ml/min. Results The average recovery rate were 98.5% and 97.8% respectively at the water concentration of 2.0 μg/L and 10.0 μg/L,the relative standard deviations (RSD) were 11.2% and 8.0%,the least detection limit was 0.02 μg/L. Conclusion The method is stable,sensitive and suitable for the detection of malachite green in water.