摘要
采用QuEChERS结合超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)法建立了同时测定鱼肉制品中磺胺二甲嘧啶、磺胺脒、结晶磺胺等24种磺胺类抗生素的分析方法。通过对色谱、质谱条件和QuEChERS前处理技术的优化,确定了最佳的实验条件。样品采用乙腈超声提取,上清液经C18和无水硫酸镁净化,过0.20μm滤膜后经UPLC-MS/MS检测。以乙腈-0.1%甲酸水溶液为流动相,经Eclipse XDB-C18色谱柱(4.6 mm×100 mm,1.8μm)进行分离,在电喷雾电离源(electrospray ionization source,ESI)正离子模式下,进行多反应监测(multiple reaction monitoring,MRM),基质匹配外标法定量。结果表明,在各自线性范围内24种磺胺类抗生素具有良好的线性关系,相关系数(r)大于0.999,在5、10、50μg/kg 3个加标浓度水平下的平均加标回收率为80.0%~116.4%,相对标准偏差(relative standard deviation,RSD)为0.8%~9.4%(n=7)。方法检出限为0.01~0.48μg/kg,定量限为0.02~1.59μg/kg,所测样品均未检出磺胺类抗生素。该方法简单快速、选择性好、灵敏度高,适用于鱼肉制品中24种磺胺类抗生素的高通量检测。
A method for the simultaneous determination of 24 sulfonamide antibiotics including sulfamethazine,sulfaguanidine,sulfanilamide and so on in fish products was established by QuEChERS coupled with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The optimal experimental conditions were determined by optimizing the chromatographic and mass spectrometric conditions and the QuEChERS pre-treatment technique.The samples were extracted by acetonitrile under ultrasonication,and then purified by C18 and anhydrous MgSO4.The solvent was detected by UPLC-MS/MS after filtering through 0.20 μm microporous membrane.The separation was performed on an Eclipse XDB-C18 column(4.6 mm × 100 mm,1.8 μm) using acetonitrile-0.1% formic acid aqueous solution as the mobile phase,and determined with positive ion mode of electrospray ionization(ESI) under multiple reaction monitoring(MRM).Then the matrix matching external standard method was used for quantitative analysis.The results indicated that the 24 sulfonamide antibiotics showed good linearity in the respective linear range with the correlation coefficients(r)higher than 0.999.The average recoveries at three spiked levels of 5,10 and 50 μg/kg ranged from 80.0% to 116.4% with the relative standard deviation(RSD) of 0.8%~9.4%(n=7).Moreover,the limits of detection(LOD) were 0.01~0.48 μg/kg and the limits of quantification(LOQ) were 0.02~1.59 μg/kg.The method was simple,rapid,selective and sensitive for the high-throughput detection of 24 sulfonamide antibiotics in fish products.
作者
李朔
张璨
马玲
王可
杨莉丽
花中霞
张梦妍
LI Shuo;ZHANG Can;MA Ling;WANG Ke;YANG Lili;HUA Zhongxia;ZHANG Mengyan(College of Chemistry and Materials Science,Hebei Normal University,Shijiazhuang 050024,China;Shijiazhuang Center for Disease Control and Prevention,Shijiazhuang Technology Innovation Center for Chemical Poison Detection and Risk Early Warning,Shijiazhuang 050011,China)
出处
《食品工业科技》
CAS
北大核心
2022年第9期301-308,共8页
Science and Technology of Food Industry
基金
国家自然科学基金项目(81903322)
石家庄市科学技术研究与发展指导计划项目(191460733)。
