超声萃取/HPLC-MS检测电子电气产品聚合物中的六溴环十二烷  

Determination of Hexabromocyclododecanes in Polymers of Electrical and Electronic Products Using Ultrasonic Extraction Followed by LC-MS

作　　者：陈琼[1] 黄秋鑫[1] 姜涛[1] 丑天姝 方亮[1] 吴琴[1] 

机构地区：[1]工业和信息化部电子第五研究所中国赛宝环境评估与监测中心信息产业电子信息产品污染控制赛宝检验中心,广东广州510610

出　　处：《分析测试学报》2017年第7期929-932,共4页Journal of Instrumental Analysis

基　　金：国家标准研制项目(20132270-T-469);广东省省级科技计划项目(2016A040403039)

摘　　要：通过优化超声萃取时间、萃取次数、萃取溶剂类型等条件,建立了电子电气产品中六溴环十二烷(含α,β,γ3种同分异构体)的高效液相色谱-质谱(HPLC-MS)测定方法。经条件优化,采用甲苯超声萃取样品,重复萃取3次,每次15 min,离心取上清液,合并后经氮气吹干,用甲醇-水溶液重新溶解定容后进行检测。六溴环十二烷各同分异构体的线性范围为50~5 000μg/L,线性相关系数均大于0.999,方法检出限为1 mg/kg,样品加标回收率为88.3%~104.5%。该方法快速、简便、准确、稳定,用于实际样品的检测,阳性样品均为发泡聚苯乙烯材料。A high performance liquid chromatography -mass spectrometric（HPLC-MS） method was developed for the determination of hexabromocyclododecanes （HBCDDs, including alpha, beta, gamma, three isomers） in electrical and electronic products, by optimization of ultrasonic extraction time, extraction cycle and extraction solvent.In the optimal conditions,the sample was ultrasonically extracted with toluene for three times and each took 15 min.The extracts were combined and concentrated to dryness under nitrogen, then redissolved with methanol water solution.The calibration curves of HBCDDs were linear in the range of 50-5 000 μg/L, with correlation coefficients more than 0.999.The detection limits were all 1 mg/kg.The spiked recoveries were in the range of 88.3%-104.5%.The method was proved to be quick,simple,accurate and stable.It was successfully applied in the determination of HBCDDs in real samples, of which the detected samples were polystyrene.

关 键 词：电子电气产品 六溴环十二烷 超声萃取 高效液相色谱-质谱法 

分 类 号：O657.63[理学—分析化学] TQ314.248[理学—化学]