2014年5月Vol.32No.5May2014ChineseJournalofChromatography524~528技术与应用DOI:10.3724/SP.J.1123.2014.01008*通讯联系人.Tel:(010)58619221,E-mail:yunh@bjciq.gov.cn.基金项目:科技部质检公益行业科研专项(201210029);国家高技术研究发展计划(“863”计划)项目(2012AA101603).收稿日期:2014-01-06超高效液相色谱-串联质谱法测定动物源性食品中的磺胺增效剂高洋洋1,张朝晖1,刘鑫1,卢晓宇1,严华1,何悦1,杨大进2,云环1*(1.北京出入境检验检疫局技术中心,北京100026;2.国家食品安全风险评估中心,北京100021)摘要:建立了一种超高效液相色谱-串联质谱(UPLC-MS/MS)测定多种基质(鸡肉、鱼肉、鸡肝、鸡蛋和牛奶)中三甲氧苄氨嘧啶、二甲氧苄胺嘧啶和二甲氧甲基苄胺嘧啶的分析方法。样品用甲酸-乙腈(1∶9,v/v)溶液提取,正己烷除脂净化,AcquityUPLCBEHC18柱(50mm×2.1mm,1.7μm)分离,以甲醇和5mmol/L醋酸铵(含0.1%(v/v)甲酸)作为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测。考察了3种提取溶液的提取效率,优化了净化条件和浓缩条件,并对流动相、柱温和固相萃取柱进行了优化。结果表明:三甲氧苄氨嘧啶、二甲氧苄胺嘧啶和二甲氧甲基苄胺嘧啶在1.25~30.0μg/L范围内线性关系良好(r≥0.99)。方法的定量限(S/N=10)为5.0μg/kg,在5.0、10.0、20.0μg/kg的添加浓度的回收率为61.2%~108.5%,相对标准偏差(RSD,n=6)为1.1%~9.8%。该方法快速、灵敏、准确,适合于多种基质中磺胺增效剂的测定。关键词:超高效液相色谱-串联质谱;磺胺增效剂;动物源性食品中图分类号:O658文献标识码:A文章编号:1000-8713(2014)05-0524-05Determinationofsulfonamidepotentiatorsinanimaloriginfoodsbyultraperformanceliquidchromatography-tandemmassspectrometryGAOYangyang1,ZHANGZhaohui1,LIUXin1,LUXiaoyu1,YANHua1,HEYue1,YANGDajin2,YUNHuan1*(1.TechnologyCenterofBeijingEntry-ExitInspectionandQuarantineBureau,Beijing100026,China;2.ChinaNationalCenterforFoodSafetyRiskAssessment,Beijing100021,China)Abstract:Amethodforthedeterminationofsulfonamidepotentiators,trimethoprim(TMP),diaveridine(DVD)andormetoprin(OMP),indifferentanimaloriginfoodmatrices(includingchickenmuscle,fishmuscle,chickenliver,eggandmilk)hasbeendevelopedbyultraperformanceliquidchromatography-tan-demmassspectrometry(UPLC-MS/MS).Thesamplewasextractedbyformicacid-acetonitrile(1∶9,v/v),cleaned-upbyhexane,separatedonanAcquityUPLCBEHC18column(50mm×2.1mm,1.7μm)withgradientelution.Thedeterminationwascarriedoutwithelectrosprayionsourceundertheposi-tivemodeandmultiplereactionmonitoring(MRM)mode.Theextractionrecoveriesofthreeextractionsolventswereobserved.Thepurificationconditionandconcentrationconditionwereoptimized.Inaddi-tion,themobilephase,columntemperatureandsolidphaseextractioncolumnwerestudied.Thecalibra-tioncurvesshowedagoodlinearityintherangeof1.25-30.0μg/L,andthecorrelationcoefficients(r)werehigherthan0.99.Thelimitsofquantification(LOQ,S/N=10)ofthethreepotentiatorswere5.0μg/kg.Atthespikedlevelsof5.0,10.0and20.0μg/kg,therecoveriesofthethreepotentiatorswererangedfrom61.2%to108.5%,andtherelativestandarddeviations(RSD,n=6)rangedfrom1.1%to9.8%.Theresultsindicatethatthemethodissimple,rapid,sensitiveandsuitableforthequalitativeandquantitativeanalysisofthethreepotentiatorsinmultiplematrices.第5期高洋洋,等:超高效液相色谱-串联质谱法测定动物源性食品中的磺胺增效剂Keywords:ultraperformanceliquidchromatography-tandemmassspectrometry(UPLC-MS/MS);sul-fonamidepotentiators;animaloriginfoods磺胺增效剂是指含有5-取代苄基-2,4-二氨基嘧啶的一类化合物,包括三甲氧苄氨嘧啶(trime-thop...