气相色谱内标法测定水产品中五氯苯酚-上海海洋大学学报.DOC

固相萃取-气相色谱串联质谱法测定 水产品中扑草净残留( 朱晓华1,2,3，王凯1,2,3，张燚4，杨洪生1,2,3，谭秀慧1,2,3，1,2,3 （1. 江苏省水产质量检测中心，江苏 南京 210017； 2. 江苏省淡水水产研究所，江苏 南京 210017； 3. 农业部渔业产品质量监督检验测试中心（南京），江苏 南京 210017； 4. ，）摘 要：通过对前处理提取溶剂、溶剂用量、固相萃取小柱对回收率影响的比较研究和二级质谱检测参数的确定，建立了鳕鱼、草鱼、斑点叉尾鮰、克氏螯虾和紫菜中扑草净残留量的固相萃取-气相色谱串联质谱法。样品中的扑草净残留由乙腈提取，经Envi-Carb串联LC-NH2固相萃取小柱净化后，通过TR-5MS毛细管色谱柱分离，采用电子轰击离子源选择反应监测模式进行质谱测定，以d14-扑草净作为内标物，内标法定量。结果表明，该方法在5～100 μg/L范围内线性关系良好，相关系数r2=0.999，在加标水平为5.0、10.0、25.0 μg/kg，内标为10.0 μg/kg，加标样品回收率为82.0～111.2 %，RSD为1.2～6.0 %，最低检测限为0.5 μg/kg。 关键词：扑草净；气相色谱-串联质谱；水产品；固相萃取；残留；内标法选择鳕鱼、草鱼、斑点叉尾鮰、克氏螯虾、紫菜等5种典型水产品种作为试验对象，可以有效去除样品复杂背景的干扰，具有高选择性、高灵敏度。 中图分类号：TS254.7 文献标志码：A as chromatography-tandem mass spectrometry determination of prometryn residue in aquatic products with solid phase extraction ZHU Xiaohua1,2,3, WANG Kai1,2,3 , ZHANG Yi4, YANG Hongsheng1,2,3 , TAN Xiuhui1,2,3, GAO Yuyi1,2,3 （1. Aquatic Products Analysis and Testing Center of Jiangsu Province, Nanjing 210017,China; 2. Freshwater Fishery Research Institute of Jiangsu Province, Nanjing 210017,China； 3. Fishery Products Quality Supervision and Testing Center (Nanjing), Ministry of Agriculture, Nanjing 210017,China； 4., Beijing 100193, China） Abstract：Residue of prometryn in edible tissues of codfish, grass crap, channel calfish, crayfish, laver were determined by gas chromatography-tandem mass spectrometry (GC- MS/MS) using internal standard method. Such factors as extraction solvent, solvent dosage and choice of solid-phase extraction ( SPE ) columns were compared in this paper. The target compound was extracted two times with acetonitrile，purified by solid-phase extraction ( SPE ) Envi-Carb column and LC-NH2 colunn. and analyzed with GC-MS/MS. TR-5MS capillary chromatographic column was used for separation, and the selected reaction monitoring(SRM) with electron impact ionization source was adopted in MS. This method chooses d14- prometryn as internal standard substance. The working curve were linear (r2=0.999) in the range of 5～100 μg/L