在线净化LC-MS-MS测定淡水鱼中孔雀石绿及隐性孔雀石绿.pdfVIP

Vo l. 27 No.l 常州大学学报{自然科学版) 第 27 卷第 1 期 Journal of Changzhou University(Natural Science Edition) Jan.2015 2015 年 1 月 文章编号:2095-0411 (2015)01-0071-05 在线净化/LC-MS-MS 测定淡水鱼中孔雀石绿及 隐性孔雀石绿 墙燕毡，罗满涟，吴冬梅，王博超，王洁琼 (常州市农畜水产品质量监督检验测试中心，江苏常州 213002) 摘要:研究了一种在线净化/LC-M5-MS 联用技术测定淡水鱼中孔雀石绿(MG)及隐性孔雀石绿(LMG)残留的方法.样品加内 标，经乙崩涡旋提取、离心，提取液经在线净化柱(Cyclone P) 净化，以 10mmol/ L 乙酸镀-乙蔚溶液将目标物洗脱至 C18 柱上，用 LC-MS-MS检测.方法在 O. 1-1O，_.g/kg 质量浓度范围内有良好的线性关系.MG、 LMG 的检出限为，0. l ，..g/峙.3 个浓度加标回 收率为 84.5%-99.6%.相对标准偏差为 2.7%-5.3%. 该方法前处理简便快速、试剂用量少、回收率高、灵敏度和重现性好，适 用于水产品中孔雀石绿及其代谢物残留量分析. 关键词:在线净化，LC-M5-MS，孔雀石绿s 测定 中图分类号:0657.6 文赋标识码:A 1101 ,10. 3969/j. issn. 2095-0411. 2015. 01. 014 Determination of Malachite Green 缸ld Leucomalachite Green in Freshwater Fish by Online Purification and LC-MS-MS DU Yan-yu , LUO Yi-lian , WU Dong-mei , WANG Bo-chao , WANG Jie-qiong (Agriculture Beast and Fishing Product Quality Supervision Inspection and Test Center of Changzhou , Changzhou 213002 ,China) Abstract: A method was established for determination of malachite green (MG) and leucomalachite green (LMG) residues in freshwater fish by online purification and LC-MS-MS technology. The samples were vortex extracted and centrifuged with acetonitrile after adding internal standard. The extract was purified by online column(Cyclone P) , and then the target compound was eluted to C18 column with 10mmol/L ammonium acetate-acetonitrile solution for further detection by LC-MS-MS. The method has a good line- arity concentration range from o. 1 to 10pg/kg, and the detection li