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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
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作者单位
陈琼,黄秋鑫,姜涛,丑天姝,方亮,吴琴 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 
基金项目:国家标准研制项目(20132270-T-469);广东省省级科技计划项目(2016A040403039)
中文摘要: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,γ 3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50~5 000 μg/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。
中文关键词: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
 
Determination of Hexabromocyclododecanes in Polymers of Electrical and Electronic Products Using Ultrasonic Extraction Followed by LC-MS
Abstract: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
Key Words:electrical and electronic products  hexabromocyclododecanes(HBCDDs)  ultrasonic extraction  high performance liquid chromatography -mass spectrometry(HPLC-MS)
引用本文:陈琼,黄秋鑫,姜涛,丑天姝,方亮,吴琴.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[J].分析测试学报,2017,36(7):929-932.
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