摘要
建立了气相色谱-质谱法测定REACH法规相关的15种邻苯二甲酸酯的分析方法。在0.5 g样品中加入10 mL四氢呋喃,60℃下超声提取60 min,正己烷沉淀絮凝高聚物,经0.45μm有机系过滤膜过滤后,采用气相色谱-质谱法进行测定。11种邻苯二甲酸酯(DIBP、DBP、DIPP、nPIPP、DPP、DIHXP、DHP/DnHP、BBP、DCHP、DEHP和DNOP)的线性范围为0.2 mg·L^(-1)~10 mg·L^(-1)(r≥0.999),其余4种邻苯二甲酸酯(DMEP、DIHP、DINP和DIDP)的线性范围为1 mg·L^(-1)~50 mg·L^(-1)(r≥0.999)。15种邻苯二甲酸酯的检出限为0.011 mg·L^(-1)~0.232 mg·L^(-1),3个添加浓度水平的加标回收率范围在90.7%~103.2%,相对标准偏差(RSD,n=7)小于5.0%。该方法高效、简便、快速,已应用于REACH法规相关的15种邻苯二甲酸酯的测定。
A method for the determination of 15 phthalate esters restricted by REACH by gas chromatography-mass spectrometry was established.10 mL tetrahydrofuran was added to 0.5 g sample,and the sample was extracted by ultrasonic at 60℃for 60 min.The polymer was precipitated and flocculated by n-hexane.The extract was filtered by 0.45μm organic filter membrane,and determined by gas chromatography-mass spectrometry.The linear range of 11 phthalates(DIBP,DBP,DIPP,nPIPP,DPP,DIHXP,DHP/DnHP,BBP,DCHP,DEHP and DnOP)was 0.2 mg·L^(-1)~10 mg·L^(-1)(r≥0.999),and that of the other four phthalates(DMEP,DIHP,DINP and DIDP)was 1 mg·L^(-1)-50 mg·L^(-1)(r≥0.999).The detection limits of 15 phthalates were 0.011 mg·L^(-1)~0.232 mg·L^(-1).The recoveries ranged from 90.7%to 103.2%,and the relative standard deviation(RSD,n=7)was less than 5.0%.The method was efficient,simple,rapid,and suitable for determining 15 phthalates in REACH.
作者
高欢
卫碧文
付饶
张烨雯
GAO Huan;WEI Bi-wen;FU Rao;ZHANG Ye-wen(Technical Center for Mechanical and Electrical Product Inspection and Testing of Shanghai Customs District,Shanghai 200135,China)
出处
《化学研究与应用》
CAS
CSCD
北大核心
2021年第11期2262-2268,共7页
Chemical Research and Application
基金
2018年国家标准计划项目(20183155-T-607)资助。
