高效液相色谱法测定水产品中孔雀石绿残留量方法的改进

水产品中残留的隐色孔雀石绿经后氧化铅柱氧化为显色孔雀石绿,采用高效液相色谱-紫外检测器对显色孔雀石绿进行了检测.样品提取净化采用乙腈在乙酸铵缓冲溶液条件下提取,10 000 r/min离心,上清液转入50 mL离心管,再加入15 mL蒸馏水,10 000 r/min离心,取上清液过固相萃取柱,再用3mL蒸馏水洗柱,1 ...

Improving Method of Determination of Residual Amounts of Malachite Green in Fishery Products by High Performance Liquid Chromatography

The leuco-malachite green residues(LMG)in fishery products were transformed to malachite green(MG) by the post-column of PbO2,and determined by high performance liquid chromatography-visible wavelength detector(HPLC-VWD).MG and LMG was extracted from samples with acetonitrile in an acetate buffer medium of pH 4.5,10 000 r/min centrifugation,the supernatant was transferred to another 50 mL centrifuge tube,then added 15 mL of distilled water,10 000 r/min centrifugation,and the supernatant over solid-phase extraction column,3 mL distilled water washes column,1 mL elution(acetic acid: acetonitrile = 92∶8) eluted.Linear relationship between the values of peak area and mass concentration of MG was obtained in the range of 0.01 μg /mL-1.0 μg /mL,with detection limit(3 S/N) of 2.0 μg/kg.The recoveries and relative standard deviation were in ranges of 78.9%-88.8% and 0.6%-5.2%.The results showed that malachite green into LMG conversion rate greater than 99.3%.