Simultaneous determination of 12 sulfonamides residues in caviar by solid phase extraction-high performance liquid chromatography tandem mass spectrometry
Simultaneous determination of 12 sulfonamides residues in caviar by solid phase extraction-high performance liquid chromatography tandem mass spectrometry
陈玉娇 1江利兵 1谢俊 1郑婷 1朱子健 1许源1
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作者信息
1. 衢州海关 浙江衢州 324003
折叠
摘要
首次建立了一种同时测定鱼子酱中磺胺嘧啶、磺胺二甲基嘧啶、磺胺二甲基异恶唑和磺胺间甲氧嘧啶等12种磺胺类药物残留的固相萃取-高效液相色谱-串联质谱分析方法.根据鱼子酱脂溶性的特点,试样采用正己烷溶剂预溶解,用乙酸乙酯提取2次后经混合型阳离子交换固相萃取柱(MCX)净化,用InertSustain Swift C18柱(150 mm×4.6 mm,5 μm)分离,多反应监测(MRM)模式串联质谱进行测定,以内标法定量.结果显示,磺胺类药物在1.00～20.00 ng/mL范围内12种测定物均具有较好的线性关系,相关系数均≥0.99,方法定量限(S/N＞10)为1.0 μg/kg.对阴性鱼子酱在3个添加水平下(1.0 μg/kg、2.0μg/kg和5.0 μg/kg)分别进行加标回收试验,实际样品中12种测定物质的平均回收率在72.9％～119.0％之间,相对标准偏差(RSD,n=6)在0.9％～11.0％之间.应用本方法对2018-2020年采集的320个鱼子酱样品进行检测,结果表明均为未检出磺胺类药物残留.本方法快速、灵敏、准确,适用于日常大批量鱼子酱样品中磺胺类药物及其代谢物残留的定性、定量分析.
Abstract
First establish a solid phase extraction(SPE)-high performance liquid chromatography(HPLC)-tandem mass spec-trometry method for the simultaneous determination of sulfadiazine,sulfamethazine,sulfadimethyl Isoxazole and sulfamonomethox-ine residues in Caviar.According to the fat soluble characteristics of Caviar,the sample was pre dissolved with n-hexane solvent,extracted twice with ethyl acetate,purified with mixed cation exchange solid phase extraction column(MCX),and separate with InertSustain Swift C18 column(150 mm×4.6 mm,5 μm),multi reaction monitoring(MRM)mode tandem mass spectrometry for determination,internal standard method for quantification.The results showed that there was a good linear relationship between the 12 analytes of sulfonamide drugs in the range of 1.00-20.00 ng/mL,with a correlation coefficient greater than 0.99,and a method quantification limit(S/N＞10)of l.0μg/kg.For negative Caviar,at 3 addition levels(1.0μg/kg,2.0 μg/kg and 5.0 μg/kg)were subjected to spiked recovery tests,and the average recovery rates of the 12 measured sub-stances in the actual samples ranged from 72.9％to 119.0％,with a relative standard deviation(RSD,n=6)is between 0.9％and 11％.This method was used to detect 320 Caviar samples from 2018 to 2020,and the results showed that no sulfon-amides residues were detected.This method is rapid,sensitive and accurate,and is suitable for qualitative and quantitative analysis of sulfonamides and their metabolites residues in daily mass Caviar samples.
关键词
鱼子酱/固相萃取/高效液相色谱-串联质谱/磺胺类药物/残留量
Key words
Caviar/Solid phase extraction/High performance liquid chromatography tandem mass spectrometry/Sulfonamides/Residues
维普
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