Determination of 14 Kinds of Flame Retardants in Leather by Solid Phase Extraction Combined with GC-MS Method

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Determination of 14 Kinds of Flame Retardants in Leather by Solid Phase Extraction Combined with GC-MS Method

- Determination of 14 Kinds of Flame Retardants in Leather by Solid Phase Extraction Combined with GC-MS Method
- Vol. 35, Issue 12, Pages: 1548-1553(2016)
- 作者机构：
  
  广州质量监督检测研究院国家皮革制品质量监督检验中心,广州
- 作者简介：
- 基金信息：
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Determination of 14 Kinds of Flame Retardants in Leather by Solid Phase Extraction Combined with GC-MS Method. [J]. 35(12):1548-1553(2016)
DOI：

Determination of 14 Kinds of Flame Retardants in Leather by Solid Phase Extraction Combined with GC-MS Method. [J]. 35(12):1548-1553(2016) DOI：

摘要

采用固相萃取结合气相色谱-质谱(GC-MS)技术，建立了皮革中14种多氯联苯及磷酸三酯类阻燃剂(TEP，TBP，TCEP，PCB18，TCPP，PCB101，PCB153，PCB138，TPhP，TEHP，PCB180，o-TTP，m-TTP，p-TTP)的高通量检测方法。皮革样品经乙腈超声提取后，采用Florisil 固相萃取柱净化，经DB-5MS色谱柱分离，GC-MS的选择离子监测(SIM)模式监测，以保留时间和特征离子比值定性，外标法定量。14种阻燃剂在一定浓度范围内线性关系良好，相关系数(r2)均大于0.998，方法检出限为25.0~50.0 μg/kg，平均回收率为82.0%~112.8%，相对标准偏差(RSD，n=6)为2.1%~9.4%。方法的前处理简单快速，灵敏度高，适用于皮革中14种阻燃剂的同时测定。

Abstract

A new method was established to determine 14 kinds of polychlorinated biphenyls(PCBs) and organophosphate esters(OPEs) flame retardants(including TEP，TBP，TCEP，PCB18，TCPP，PCB101，PCB153，PCB138，TPhP，TEHP，PCB180，o-TTP，m-TTP and p-TTP) in leather by solid phase extraction(SPE) coupled with gas chromatography-mass spectrometry(GC-MS).The samples were ultrasonically extracted with acetonitrile，and purified with a Florisil solid phase extracting column.Analytes were successfully separated on a DB-5MS capillary column,and detected by GC-MS in selected ion monitoring mode(SIM).Analytes were qualitatively analyzed via retention time and abundance ratio of characteristic ions，and quantified by the external standard method.14 flame retardants presented favorable linearity in the respective linear ranges，with correlation coefficients(r2) more than 0.998.The detection limits(S/N=3) ranged from 25.0 μg/kg to 50.0 μg/kg，the average recoveries(n=6) were in the range of 82.0%-112.8%，and the relative standard deviations(RSDs，n=6) were 2.1%-9.4%.The method is accurate，rapid and sensitive,and is suitable for the determination of 14 flame retardants in leather samples.

关键词

皮革阻燃剂固相萃取气相色谱-质谱

Keywords

leatherflame retardantsolid phase extraction(SPE)gas chromatography-mass spectrometry(GC-MS)

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Related Institution

School of Environment，Hangzhou Institute for Advanced Study，UCAS

University of Chinese Academy of Sciences

State Key Laboratory of Environmental Chemistry and Ecotoxicology，Research Center for Eco-Environmental Science，Chinese Academy of Sciences

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