超高效液相色谱法快速测定水产品中孔雀石绿、结晶紫的含量.docVIP

超高效液相色谱快速测定水产品中孔雀石绿、结晶紫 刘少彬, 胡浩光, 谢翠美, 莫炯怀 东莞市海洋与渔业环境监测站东莞523079) 摘 要: 目的 超高效液相色谱(ultra performance liquid chromatographyUPLC)测定水产品中孔雀石绿、结晶紫的。方法 加酸性氧化铝净化、乙腈旋涡振荡、硼氢化钾还原, 超声提取, 提取液真空浓缩近干后用乙腈溶解残渣。残渣液过串联酸性氧化铝AL-A柱和丙磺酸PRS柱, 净化过程中在移除AL-A柱后, 用3 mL水淋洗PRS柱, 最后用乙酸铵和乙腈1:1, V:V)洗脱, 过滤供UPLC测定。结果 μg/L浓度范围内呈现良好的线性关系。GB/T 20361-2006经改进后, 回收率和重复性均满足国标方法的要求。结论 该方法简便、准确、高效, 适用于水产品中孔雀石绿和结晶紫残留量的快速检测。 关键词超高效液相色谱; 孔雀石绿; 结晶紫; 水产品 Rapid determination of malachite green and crystal violet in aquatic products by ultra performance liquid chromatographyLIU Shao-Bin*, HU Hao-Guang, XIE Cui-Mei, MO Jiong-Huai (Dongguan Marine and Fishery Environment Monitoring Station, Dongguan 523079, China) ABSTRACT: Objective To establish a method for determination of malachite green and crystal violet in aquatic product by ultra performance liquid chromatography (UPLC). Methods Samples were cleaned with acidic alumina, vortex oscillated with acetonitrile, processed with potassium borohydride reduction and ultrasonic extraction. The extract was vacuum concentrated until near dry and the residue was dissolved with acetonitrile. The residue liquid passed series AL-A and PRS columns for purification process, 3 mL water was used to leach PRS column after the removal of AL-A, and finally ammonium acetate and acetonitrile(1:1, V:V) were used for elution. and then the filtrate was determined by UPLC. Results Malachite green and crystal violet had good linear relationships in the range of 0.5~500 μg/L. After the improvement of GB/T 20361-2006, the recovery and repeatability of the method could meet the requirements of the national standard method. Conclusion The established method is simple, accurate and efficient, which is suitable for rapid detection of malachite green and crystal violet residues in aquatic product. KEY WORDS: ultra performance liquid chromatography; malachite green; crystal violet; aquatic products 1 引 言 孔雀石绿(malachite green, MG)属于三苯甲烷类染料, 自20世纪30年代早期, 孔雀石绿就在养殖场作为常用抗感染药物使用[1]。结晶紫(crystal