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第23卷,第6期Vol.23,No.6 20化学分析计量 2014年11月CHEMICALANALYSISANDMETERAGENov.2014 doi:10.3969/j.issn.1008–6145.2014.06.006 固相萃取–气相色谱–串联质谱法测定塑料食品 包装材料中3种抗氧化剂的残留量* 姚帮本,王道俊,储大勇 (安徽省产品质量监督检验研究院,合肥230051) 摘要建立了气相色谱–串联质谱法测定塑料食品包装材料中抗氧化剂二丁基羟基甲苯(BHT)、丁基羟基茴香 醚(BHA)和特丁基对苯二酚(TBHQ)残留量的分析方法。样品采用环己烷–乙酸乙酯混合溶剂超声萃取,经固相 萃取法富集和净化,采用气相色谱–串联质谱在多反应监测模式下进行测定。结果表明,3种抗氧化剂质量浓度在 0.05~20mg/L范围内线性关系良好,线性相关系数大于0.999;BHT,BHA,TBHQ的检出限分别为0.005,0.01,0.03 mg/kg;平均添加回收率为88.7%~104.0%;测定结果的相对标准偏差小于5.5%(n=6)。该方法操作简便,灵敏度高, 重复性好,可用于塑料食品包装材料中抗氧化剂BHT,BHA,TBHQ残留量的测定。 关键词固相萃取;气相色谱–串联质谱法;抗氧化剂;塑料食品包装材料 中图分类号:O657文献标识码:A文章编号:1008–6145(2014)06–0020–05 DeterminationofThreeAntioxidantResiduesinFoodPlasticPackagingMaterials bySolidPhaseExtraction–GasChromatography–TandemMassSpectrometry YaoBangben,WangDaojun,ChuDayong (AnhuiProvinceProductQualitySupervision&InspectionInstitute,Hefei230051,China) AbstractAnewmethodforthesimultaneousdeterminationofthreeantioxidantresidues(butylatedhydroxytoluene, butylatedhydroxyanisole,tertiarybutylhydroquinone)infoodplasticpackagingmaterialsbysolidphaseextraction–gas chromatography–tandemmassspectrometry(GC–MS/MS)wasdeveloped.Theantioxidantswereextractedfromthe sampleswithcyclohexane-ethylacetateintheassistantofultrasonicextraction,andthenenrichedandcleaned-upwithsolid phaseextractiononasilicacolumn.ThedetectionwascarriedoutbyGC–MS/MSinthesingle-reactionmonitoring(SRM) mode.Thecalibrationcurvesshowedgoodlinearityintherangeof0.05–20mg/Lwiththecorrelationcoefficientsmore than0.999.Thedetectionlimitswere0.005,0.01and0.03mg/kgforBHT,BHAandTBHQ,respectively.Theaverage recoveriesofthethreeantioxidantsincommercialfoodplasticpackagingmaterialswere88.7%–104.0%,therelative standarddeviationswerelessthan5.5%(n=6).Thismethodissimple,sensitive,highlyreproducible,andsuitablefor determinationofthreeantioxidantresiduesinfoodplasticpackagingmaterials. Keywordssolidphaseextraction(SPE);gaschromatography–tandemmassspectrometry(GC–MS/MS); antioxidants;plasticfoodpackagematerial 食品接触材料作为食品的贴身衣,其安全性直是油脂类食品,会通