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超声波萃取-GC/MS法测定软体家具材料中的溴化阻燃剂
引用本文:梁莹,梁金玲,张志辉,刘卓钦,蚁乐洲,李丹.超声波萃取-GC/MS法测定软体家具材料中的溴化阻燃剂[J].家具,2013(6):87-90.
作者姓名:梁莹  梁金玲  张志辉  刘卓钦  蚁乐洲  李丹
作者单位:广东出入境检验检疫局,广州510623
基金项目:质检公益性科研项目(编号:2012104020).
摘    要:建立了超声波萃取-GC/MSN时测定软体家具材料多溴阻燃剂的方法,分析物包括10种多溴联苯和10种多溴二苯醚。将破碎后的样品用正己烷和二氯甲烷的混合溶剂进行超声波萃取,萃取液经固相硅胶净化、浓缩定容后,采用GC/MS测定多溴联苯和多溴二苯醚的含量,外标法定量。优化了样品前处理条件,包括前处理方式、萃取溶剂的选择、萃取温度和时间。结果表明在(0.15~2.00)mg/L范围内相关系数均大于0.99.定量下限2.0mg/kg,相对标准偏差(n=6)在5.16%~9.18%之间,回收率在80.5%~113.5之间。该方法操作简便、分析迅速、结果准确,可以满足软体家具材料对多溴联苯和多溴二苯醚的定性和定量分析。

关 键 词:软体家具材料  溴化阻燃剂  超声波萃取  气相色谱-质谱法

Determination of the Banned Polybromobiphenyls and Polybromobiphenyl Ethers in Upholstered Furniture Materials by Ultrasonic Extraction GC-MS Method
LIANG Ying,LIANG Jinling,ZHANG Zhihui,LIU Zhuoqin,YI Lezhou,LI Dan.Determination of the Banned Polybromobiphenyls and Polybromobiphenyl Ethers in Upholstered Furniture Materials by Ultrasonic Extraction GC-MS Method[J].Fumiture,2013(6):87-90.
Authors:LIANG Ying  LIANG Jinling  ZHANG Zhihui  LIU Zhuoqin  YI Lezhou  LI Dan
Affiliation:( Guangdong Entry- Exit Inspection & Quarantine Bureau, Guangzhou 510623, China)
Abstract:A ultrasonic extraction-gas chromatography-mass spectrometric method was established for the determination of the banned polybromobiphenyls ( PBBs ) and polybromobiphenyl ethers ( PBBEs ) in upholstered furniture materials. The pretreatment conditions including extraction method, extractant, extraction time and temperature were optimized. Under the optimum separation and detection condition, PBBs and PBBEs were confirmed and determined with external standard method. Linear relationship between area of peak and concentration of acetophenone was kept with r above 0.99 in the range of 0.15-2.00 mg/L, and the method examination limit was 2.0 mg/kg. The recoveries were in the range of between 80.5% and 113.5%, and the values of RSD (n=6) were between 5.16% and 9.18%.
Keywords:upholstered furniture material  bromide flame retardant  ultrasonic extraction  GC-MS
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