高效液相色谱-串联质谱测定塑料聚合物中有机磷阻燃剂DOPO的迁移量及其迁移规律研究  

Study on Analysis of Migration of Organophosphorus Flame Retardant DOPO in Plastic Polymers by HPLC-MS/MS and Its Migration Regularity

作　　者：林春梅 刘莹峰[1] 张子豪[1] 李全忠[1] 李丹[1] 翟翠萍[1] 肖前[1] 郑建国[1] IN Chun-mei;LIU Ying-feng;ZHANG Zi-hao;LI Quan-zhong;LI Dan;ZHAI Cui-ping;XIAO Qian;ZHENG Jian-guo(Guangdong Inspection and Quarantine Technology Center,Guangzhou 510623,China)

机构地区：[1]广东出入境检验检疫局技术中心,广东广州510623

出　　处：《分析测试学报》2019年第3期277-282,共6页Journal of Instrumental Analysis

基　　金：国家重点研发计划(2016YFF0203705);广东检验检疫局科研项目(2018GDK22)

摘　　要：采用高效液相色谱-串联质谱(HPLC-MS/MS)技术建立了塑料聚合物中9,10-二氢-9-氧-10-磷杂菲-10-氧化物(DOPO)迁移量的测定方法,并对不同浸泡模拟物、不同温度和时间下DOPO的迁移规律进行研究。样品采用欧盟(EU)2017/752法规中的食品模拟物浸泡。水基模拟物直接过滤,橄榄油模拟物用含38%甲醇的乙腈溶液萃取后,经C_(18)色谱柱分离,以甲醇-2 mmol/L醋酸铵水溶液(含0.1%甲酸)为流动相,采用多反应监测模式进行检测。水基模拟物(3%乙酸、10%乙醇、50%乙醇)中DOPO的定量下限为0.10 ng/mL,橄榄油模拟物中的定量下限为1.0 ng/g。样品加标回收率为85.3%～110%,相对标准偏差(RSD,n=6)不大于7.3%。该方法快速简便、灵敏度高、准确性好,适用于塑料聚合物中DOPO迁移量的测定。A method of high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) was established for the determination of migration of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide(DOPO)in plastic polymers.The migration regularity of the analyte in different simulants,temperatures and times were studied.Samples were soaked with the food simulants according to(EU)2017/752.The water-based simulated sample was directly filtered,and the olive oil simulated sample was extracted with acetonitrile solution containing 38% methanol.The samples were separated on a C18 column with methanol-2 mmol/L ammonium acetate containing 0.1% formic acid as mobile phases,and analyzed under multiple reaction monitoring mode.The quantitation limits of the method for water-based simulant(3% acetic acid,10% alcohol,50% alcohol)and olive oil simulant were 0.10 ng/mL and 1.0 ng/g,respectively.The spiked recoveries ranged from 85.3% to 110% with relative standard deviations(RSD)not more than 7.3%.This method was rapid,precise and convenient,and was appropriate for the determination of DOPO migration in plastic polymers.

关 键 词：塑料 有机磷阻燃剂 迁移量 DOPO 高效液相色谱-串联质谱(HPLC-MS/MS) 

分 类 号：O657.7[理学—分析化学] TQ320.74[理学—化学]