固相萃取-气相色谱串联质谱法测定水产品中扑草净的残留  

Gas chromatography-tandem mass spectrometry determination of prometryn residue in aquatic products with solid phase extraction

作　　者：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] 高钰一[1,2,3] 

机构地区：[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,江苏南京210017 [4]中国农业科学院农产品加工研究所,北京100193

出　　处：《上海海洋大学学报》2015年第6期960-967,共8页Journal of Shanghai Ocean University

基　　金：江苏省农业科技自主创新资金(CX(15)1013;CX(15)1011);江苏省自然科学基金项目(BK20141500);江苏省属公益院所能力提升项目(BM2015018)

摘　　要：通过对前处理提取溶剂、溶剂用量、固相萃取小柱等因素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、克氏螯虾和紫菜中扑草净残留量的固相萃取-气相色谱串联质谱测定法。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5~100μg/L范围内线性关系良好,相关系数r2=0.999,在扑草净加标水平为5.0、10.0、25.0μg/kg,内标量为10.0μg/kg的条件下,加标样品回收率为82.0%~111.2%,RSD为1.2%~6.0%（n=6）,最低检测限为0.5μg/kg。方法满足残留检测的要求,适用于样品的定性确证与定量测定。Residues of prometryn in edible tissues of codfish, grass carp, channel calfish, catfish, 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 ） with Envi-Carb column and LC-NH2 column, 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. When spiked with 5. 0, 10.0, 25.0 μg/kg of prometryn and 10.0 μ1/kg d14- prometryn, the average recoveries were 82.0 % - 11 I. 2 % and the RSD were 1.2 % - 6.0 %. The detection limit was 0.5 μg/kg. The method could meet the requirements of the residul detection. It is suitable for qualitative and quantitative determination of samples.

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 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程]