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气相色谱-质谱法测定玩具中的4种阻燃剂
引用本文:马强,白桦,王超,张庆,刘茜,席海为,王烨,陈云利.气相色谱-质谱法测定玩具中的4种阻燃剂[J].分析试验室,2010,29(4).
作者姓名:马强  白桦  王超  张庆  刘茜  席海为  王烨  陈云利
作者单位:1. 中国检验检疫科学研究院,北京,100123
2. 北京中医药大学中药学院,北京,100102
基金项目:质检公益性行业科研专项计划(200810953);;国家认证认可监督管理委员会计划(2007B268)项目资助
摘    要:建立了玩具中三(2-氯乙基)磷酸酯、磷酸三邻甲苯酯、2,2′,4,4′,5-五溴联苯醚、2,2′,3,3′,4,4′,6,6′-八溴联苯醚等4种阻燃剂的气相色谱-质谱分析方法。玩具样品以V(正己烷):V(二氯甲烷)=1:1混合溶液为提取溶剂,超声提取30min,提取液以DB-5HT石英毛细管色谱柱(15m×0.25mm×0.10μm)分离后进行选择离子监测模式下的定性及定量分析。4种阻燃剂的定量限为0.1mg/kg,在低、中、高3个添加水平范围内,4种阻燃剂的平均回收率为93.5%~97.3%,相对标准偏差在2.4%~4.1%之间。

关 键 词:气相色谱-质谱  玩具  阻燃剂  

Determination of 4 flame retardants in toys by GC-MS
MA Qiang,BAI Hua,WANG Chao,ZHANG Qing,LIU Xi,XI Hai-wei,WANG Ye,CHEN Yun-li.Determination of 4 flame retardants in toys by GC-MS[J].Chinese Journal of Analysis Laboratory,2010,29(4).
Authors:MA Qiang  BAI Hua  WANG Chao  ZHANG Qing  LIU Xi  XI Hai-wei  WANG Ye  CHEN Yun-li
Institution:1.Chinese Academy of Inspection and Quarantine;Beijing 100123;2.Beijing University of Chinese Medicine;Beijing 100102
Abstract:An analytical method based on gas chromatography-mass spectrometry has been developed for the simultaneous determination of 4 flame retardants (tris (2-chloroethyl) phosphate, tri-o-cresyl phosphate, 2, 2', 4, 4', 5-pentabromodiphenyl ether and 2, 2', 3, 3', 4, 4', 6, 6'-octabromophenyl ether) in toys. Toy samples were extracted under ultrasonication for 30 min with n-hexane-dichloromethane (1∶1, V/V). The filtrate was injected into GC-MS and separated on a DB-5HT (15 m×0.25 mm×0.10 μm) chromatographic column. Qualitative and quantitative analysis was conducted under selected ion monitoring (SIM) mode. The limits of quantitation (LOQ) were 0.1 mg/kg for 4 flame retardants. The recoveries and relative standard deviations were 93.5%~97.3% and 2.4%~4.1%, respectively.
Keywords:GC-MS  Toys  Flame retardants  
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