QuEChERS-超高效液相色谱-串联质谱法快速测定鱼肉中22种磺胺类药物残留  

Rapid Determination of 22 Sulfonamide Residues in Fish by QuEChERS-UPLC-MS/MS

作　　者：张晓强[1] 张波 方萍[1] 林慧[1] 颜春荣[1] 

机构地区：[1]江苏省产品质量监督检验研究院,南京210007 [2]山东省环保技术服务中心,济南250101

出　　处：《理化检验（化学分册）》2015年第3期369-374,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：江苏省质量技术监督局科技项目(KJ122701)

摘　　要：结合QuEChERS前处理技术,提出了测定鱼肉中22种磺胺类残留的超高效液相色谱-串联质谱法。样品用含0.1%(体积分数,下同)甲酸的乙腈溶液提取后,经QuEChERS试剂盒净化。净化液在Agilent ZORBAX Eclipse Plus C18色谱柱上分离,以0.1%甲酸溶液-甲醇为流动相进行梯度洗脱。采用电喷雾正离子源及计划式多反应监测模式进行测定,以内标法定量。磺胺硝苯、磺胺、磺胺喹噁啉的线性范围为0.5~50μg·L-1,检出限(3S/N)为0.5μg·L-1;其他19种磺胺类兽药的线性范围为0.1~50μg·L-1,检出限(3S/N)为0.1μg·L-1。加标回收率在78.2%~118%之间,测定值的相对标准偏差(n=6)在3.4%~19%之间。方法用于鱼肉中多种磺胺类药物残留的快速测定,结果与标准方法测定结果一致。A method of QuEChERS-UPLC-MS/MS was proposed for rapid determination of 22 sulfonamide residues in fish.The sample was extracted with a mixture of acetonitrile with 0.1%(φ)formic,and the extract was purified by QuEChERS method.The target analytes were separated on an Agilent ZORBAX Eclipse Plus C18 column,using a mixture of methanol and 0.1%(φ)formic solution as mobile phase for gradient elution.ESI+and schedule MRM were adopted in MS/MS,quantification was carried out by the internal standards method.The linear ranges of sulfanilamide,sulfaquinoxaline and sulfanitran were 0.5-50μg·L-1 with detection limits(3S/N)of0.5μg·L-1.For the other 19 sulfonamides,the detection limits(3S/N)were 0.1μg·L-1 and the linear ranges were 0.1-50μg·L-1.The recovery rate measured by standard addition method was in the range of 78.2%-118%,with RSD′s(n=6)in the range of 3.4%-19%.The method was used for rapid determination of 22 sulfonamide residues in fish,giving results in agreement with those obtained by the standard method.

关 键 词：QUECHERS 超高效液相色谱-串联质谱法 鱼肉 磺胺类药物残留 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]