超高效液相色谱快速测定水产品中孔雀石绿.docVIP

PAGE 4 食品安全质量检测学报 第8卷第3期 刘少彬, 等: 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 PAGE 5第8卷 第3期 食品安全质量检测学报 Vol. 8 No. 32017年3月 Journal of Food Safety and Quality Mar. , 2017 基金项目: 东莞市科技计划项目(K10017K)Fund: Supported by the Scientific and Technological Project of Dongguan (K10017K)*通讯作者: 刘少彬, 助理工程师, 主要研究方向为食品检测。E-mail: lsb@dg.cn*Corresponding author: LIU Shao-Bin, Assistant Engineer, Dongguan Marine and Fishery Environment Monitoring Station, Dongguan 523079, China. E-mail: lsb@dg.cn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 建立超高效液相色谱(ultra performance liquid chromatography, UPLC)测定水产品中孔雀石绿、结晶紫的含量。方法 样品经加酸性氧化铝净化、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 孔雀石绿和结晶紫在0.5~500 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: 超高效液相色谱法; 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 0.5~5