超高效液相色谱串联飞行时间质谱法测定水产品中18种磺胺类化合物

采用超高效液相色谱串联飞行时间质谱(UPLC-QTOF-MS)结合QuEChERS净化处理,对淡水产品中18种磺胺类化合物进行准确的鉴定。Chromalynx XS软件将化合物的保留时间以及一级母离子精确质量数作为定性依据,筛查样品中阳性化合物,对疑似阳性化合物进行人工比对二级碎片离子信息,以进一步确证阳性化合物。本实验对草鱼、黄鳝、螃蟹3种淡水产品基质效应进行考察,基质匹配外标法定量,结果表明,在50~1000μg/kg浓度范围内,18种目标化合物线性关系良好,方法检出限为2~20μg/kg,对3种基质在200、400、800μg/kg 3个添加水平的18种磺胺类化合物进行测定,回收率在70.0~124.6%之间。

Determination of 18 sulfonamides in fish products by UPLC-QTOF-MS

The accurate mass and retention time were utilized to screen the positive compounds by Chromalynx XS.The suspected sulfonamides were evaluated using artificial comparison of MS2 ions for the futher identifying.The matrix effects in three kinds of typical foods were investigated and the quantification was carried out by matrix-matched with external standard method.The results demonstrated that the linear ranges were from 50μg/kg to 1000μg/kg with good correlation coefficients.The method detection limits were in the range of 2μg/kg to 20μg/kg.The average recoveries at three spiked levels were in the range of 70.0%-124.6% for grass carp,ricefield eel and crab.