水产品中己烷雌酚_己烯雌酚与双烯雌酚残留的毛细管电泳测定

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1、第29卷第1期分析测试学报Vol129No112010年1月FENXICESHIXUEBAO(JournalofInstrumentalAnalysis)55～58水产品中己烷雌酚、己烯雌酚与双烯雌酚残留的毛细管电泳测定林子俺,庞纪磊,黄慧,郑江南,张兰(福州大学化学化工学院食品安全分析与检测教育部重点实验室,福建福州350002)摘要:建立了毛细管电泳-紫外检测法测定水产品中己烷雌酚(HXS)、己烯雌酚(DES)及双烯雌酚(DIES)残留的新方法。研究了缓冲体系的酸度、浓度、添加剂、分离电压、进样时间及温度等对组分分离的影响。在检测波长为200nm,分离电压为20kV,运行缓冲液为50mm

2、ol/L硼砂-25mmol/L氢氧化纳(pH1213,含30%的N,N2二甲基甲酰胺)的条件下,3种目标组分在14min内达到基线分离。HXS、DES与DIES的质量2浓度与峰面积分别在210～120、110～100、110～100mg/L范围内呈良好线性,相关系数(r)分别为019998、019992、019994,检出限为013～019mg/L。将该方法用于鲫鱼中3种雌酚类激素的检测,结果令人满意。关键词:毛细管电泳;水产品;己烷雌酚;己烯雌酚;双烯雌酚中图分类号:O65718;R97711文献标识码:A文章编号:1004-4957(2010)01-0055-04doi:1013969/

3、j1issn11004-4957120101011013DeterminationofHexestrol,DiethylstibestrolandDienestrolResiduesinAquaticProductbyCapillaryElectrophoresisLINZi2an,PANGJi2lei,HUANGHui,ZHENGJiang2nan,ZHANGLan(KeyLaboratoryofAnalysisandDetectionforFoodSafety,MinistryofEducation,DepartmentofChemistry,FuzhouUniversity,Fuzho

4、u350002,China)Abstract:Afacilemethodwasdevelopedforsimultaneousdeterminationofhexestrol(HXS),dieth2ylstibestrol(DES)anddienestrol(DIES)residuesinaquaticproductbasedoncapillaryelectrophore2siscoupledwithultravioletdetection.Theinfluencesofsomeimportantfactorssuchasadditive,acidityandconcentrationofr

5、unningbuffer,separationvoltage,injectiontimeandtemperatureweresystemicallyinvestigated.Atthedetectionwavelengthof200nm,agoodbaselineseparationofthreeanalyteswasobtainedwithin14minbyusing50mmol/Lborax-25mmol/LNaOH(pH1213)withadditiveof30%(byvolume)DMFasrunningbufferand20kVasanappliedvoltage.Thecalib

6、ra2tioncurveswerelinearintherangeof210-120mg/LforHXSand110-100mg/LforDESandDIES,withcorrelationcoefficientsof019998,019992and019994,respectively.Thelimitsofdetection(S/N=3)ofHXS,DESandDIESwere019,014and013mg/L,respectively.Theav2eragerecoveriesfromsamplesatspikedconcentrationlevelof50mg/Lwereranged

7、from92%to98%withRSDsof213%-319%.Themethodshowedagoodrepeatabilityandhighsensitivity,andwasappliedinthedeterminationofthreeanalytesinrealsamplewithsatisfactoryresult.Keywords:capillaryelectrophoresis;aquatic