食用油脂中挥发性卤代烃的HS_SPME_GC联用分析.docxVIP

食用油脂中挥发性卤代烃的HS-SPME-GC联用分析赵鸿雁1，郭莹莹1，李磊1,*，乙小娟2，孙建刚2，陈君义2(1.南京医科大学公共卫生学院，江苏南京210029；2.张家港出入境检验检疫局，江苏张家港215600)摘要：目的：建立进出口油脂中挥发性卤代烃(VHHs)的顶空-固相微萃取-气相色谱(HS-SPME-GC)联用分析方法。方法：采用Supelco公司5种SPME纤维头对食用油脂进行顶空萃取，比较不同萃取纤维的萃取效率，分别考察萃取温度、时间、顶空体积等对萃取效果的影响。用毛细管色谱柱分离萃取成分、气相色谱-电子捕获检测器(GC-ECD)进行检测。结果：优选的SPME纤维头为75μm碳分子筛-聚二甲基硅氧烷(CAR/PDMS)。于15mL顶空萃取瓶中加入9mL食用油，在60℃恒温水浴中萃取30min后，290℃解吸3min进行GC分析。方法检测限为0.02～1.4ng/mL，回收率在89%～105%之间，相对标准偏差(RSD)小于8.5%(n=5)。结论：该方法具有操作简便、快捷、灵敏度高、检测限低、不使用有机溶剂等特点，适合于食用油脂中挥发性卤代烃的检测。关键词：食用油脂；顶空-固相微萃取-气相色谱(HS-SPME-GC)；挥发性卤代烃；气相色谱；联用技术DeterminationofVHHsinEdibleOilsbyHS-SPMEfollowedbyGC-ECDZHAOHong-yan1，GUOYing-ying1，LILei1,*，YIXiao-juan2，SUNJian-gang2，CHENJun-yi2(1.SchoolofPublicHealth,NanjingMedicalUniversity,Nanjing210029,China；2.ZhangjiagangEntry-exitInspectionandQuarantineBureau,Zhangjiagang215600,China)Abstract：Objective:Toestablishamethodfortheextractionanddeterminationoffivevolatilehalogeneratedhydrocarbons(VHHs)inedibleoilbyheadspacesolid-phasemicroextraction(HS-SPME)andgaschromatography-electroncapturedetector(GC-ECD).Methods:Samplesweresubjectedtoheadspaceextractionwith5typesoffiber(SupelcoInc.).Extractionefficienciesofdifferentfiberswerecompared,andtheeffectsofextractiontemperature,extractiontime,andsolventvolumewereinvestigated.Thechromatographicseparationwascarriedoutonacapillarycolumnequippedtoagaschromatographysystemwithelectroncapturedetector.Results:CAR/PDMSfiberof75μmwastheselectedfiber.Afterpouring9mLofedibleoilina15mLvial,theextractionwasconductedattheequilibriumtemperatureof60℃andextractiontimeof30min.Thedesorptionoffiberwasperformedat290℃for3min.Thedetectionlimitoftheestablishedmethodrangedfrom0.02(tetrachloroethylene)to1.4ng/mL(trichloroethane).Theaveragerecoveryratewasintherangeof89%－105%witharelativestandardderivation(RSD)oflessthan8.5%.Conclusion:Thismethodissimple,practical,andsensitive,whichissuitableforthedeterminationofVHHsinedibleoil.Keywords：edibleoil；headspacesolid-phasemicroextraction；volatilehalogeneratedhydrocarbons；gaschromatog