实验旨在建立水样中孔雀石绿测定的液相色谱-荧光检测方法．水样中孔雀石绿采用二氯甲烷为溶剂超声波辅助提取，提取液离心分离后经MCX柱净化，并用5％氨水甲醇溶液洗脱，以Develosil C18色谱柱为分析柱，0．05 mol／L的乙酸铵（pH 4．5）-乙腈（20：80，V／V）为流动相，采用荧光检测器分析，外标法定量．结果表明：孔雀石绿在0．05μg～1．0μg／mL范围内线性良好，相关系数为0．9993，检出限为0．5μg／L．空白水样在加标孔雀石绿含量分别为1．0μg、2．5μg、5．0μg时，孔雀石绿的平均加标回收率为72．0％～86．4％，相对标准偏差为5．4％～7．5％．该方法准确度高、精密度良好，适用于水产养殖用水中孔雀石绿的测定．%A gradient high performance liquid chromatography ( HPLC) coupled with fluorescence detection was developed for the detection of malachite green from water .Methylene chloride was used as extracting solvent assisted with ultrasonic method , the malachite green extract was purificated by MCX column after centrifuged , then eluted by 5%ammonia solution in methanol elution , Develosil C18 column was used as analytical column , 0.05 mol/L ammonium acetate (pH 4.5) -acetonitrile (20:80, v/v) as mobile phase, analyzed by fluores-cence detector , quantified by external standard method .The results showed that the linear range of malachite green was 0.05 μg/mL~1.0 μg/mL( r2 =0.9993), and the detection limit was 0.5 μg/L.When the added quality of malachite green in blank water was 1.0 μg, 2.5 μg, 5.0 μg, respectively, the average recovery ranged from72.0%to 86.4%, and the relative standard deviation was 5.4% ~7.5%.This method was precise and accurate , and suitable for determination of malachite green in aquaculture water .
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