超高效液相色谱_质谱法测定儿童玩具中氯系有机磷酯类阻燃剂.docx

氯系有机磷酯类阻燃剂欣1*，郑如兰1，戴传云2，苏小东2，雷绍荣3高(1．北京出入境检验检疫局，北京100029;2．重庆科技学院化学化工学院，重庆401331;3．四川省农科院分析测试中心，四川成都610066)摘要:建立了超声辅助萃取技术提取，高效液相色谱－质谱联用技术同时测定玩具中三(2-氯乙基)磷酸酯、三(1，3-二氯丙基)磷酸酯和磷酸三氯丙酯3种氯系有机磷酸酯类阻燃剂的分析方法，并考察了萃取溶剂、萃取时间和不同流动相对实验体系的影响。结果表明，以丙酮为萃取溶剂，萃取时间为25min，水(含0.05%甲酸)－乙腈为流动相，利用SIM模式定量分析时，三(2-氯乙基)磷酸酯、三(1，3-二氯丙基)磷酸酯和磷酸三氯丙酯的浓度分别在1.0～500、10～500、10～500μg/L范围内与峰面积成正比，相关系数大于0.997，其定量下限分别为0.5、8.0、6.0μg/kg。加标回收率为83.4%～98.9%，相对标准偏差为4.0%～7.7%。该方法简单、灵敏、准确，可用于市售塑料和毛绒儿童玩具样品的测定。关键词:超声提取;高效液相色谱－质谱;玩具;有机磷酸酯类阻燃剂中图分类号:O657.63;TQ314.248文献标识码:文章编号:1004－4957(2013)12－1507－04Adoi:10.3969/j.issn.1004－4957.2013.12.019SimultaneousDeterminationofOrganophosphorousFlameＲetardantsinChildrensToysbyHighPerformanceLiquidChromatography－MassSpectrometryGAOXin1*，ZHENGＲu-lan1，DAIChuan-yun2，SUXiao-dong2，LEIShao-rong3(1．BeijingEntry－ExitInspectionandQuarantineBureau，Beijing100029，China;2．DepartmentofChemistryandChemicalEngineer，ChongqingUniversityofScienceandTechnology，Chongqing401331，China;3．AnalysisandDeterminationCenter，SichuanAcademyofAgriculturalSciences，Chengdu610066，China)Abstract:Aneffectivemethodwasestablishedforthesimultaneousdeterminationofthreekindsoforganophosphorousflameretardantsincludingtris-(2-chloroethyl)-phosphate(TCEP)，tris-(1，3-di-chlorepropyl)-phosphate(TDCP)andtris(chloro-2-propyl)phosphate(TCPP)inchildrenstoys，basedonultrasonicassistedextractioncoupledwithhighperformanceliquidchromatography－massspectrometry．Effectsofextractionsolventtype，extractiontimeandmobilephaseonextractioneffi-ciencieswereinvestigated．Theoptimalconditionswereasfollows:extractionsolvent:acetone，ex-tractiontime:25min，mobilephase:watercontaining0.05%formicacid－acetonitrile．Undertheoptimalconditions，thecalibrationcurveswerelinearintherangesof1.0－500μg/LforTCEP，10－500μg/LforTCPPand10－500μg/LforTDCP，respectively，withcorrelationcoefficientsmorethan0.997，ThequantitationlimitsforTCEP，TCPPandTDCPwere0.5，8.0，6.0μg/kg，re-spectively．Thespikedrecoveriesvariedfrom83.4%to98.9%withrelativestandarddeviationsof4.0%－7.7%．Theproposedmetho