色谱2011，Vol.29Issue(8)：731-736,6.DOI:10.3724/SP.J.1123.2011.00731
微波辅助萃取-气相色谱-串联质谱法同时测定纺织品中6种有机磷阻燃剂
Simultaneous determination of six organophosphorous flame retardants in textiles by gas chromatography-tandem mass spectrometry combined with microwave assisted extraction
摘要
Abstract
An effective method was established for the simultaneous determination of six banned organophosphorous flame retardants in textiles by gas chromatography-tandem mass spectrometry (GC-MS/MS) combined with microwave assisted extraction (MAE). By investigating the extraction efficiency of 12 different extraction solvents for the target analytes, the optimal conditions were that the sample was extracted by microwave assisted extraction using acetone as the solvent at 76 ℃ for 30 min. Then the extract was analyzed by GC-MS/MS in multiple reaction monitoring (MRM) mode, and the concentration of each analyte was calibrated by external standard method. The linear ranges of tris-( 1-aziridinyl) phosphine oxide (TEPA), tris-( 2-chloroethyl) phosphate ( TCEP ), tris-( 1, 3-dichloropropyl) phosphate (TDCP), bis-(2,3-dibromopropyl) phosphate (DDBPP), tri-o-cresyl phosphate (TOCP) and tris-( 2,3-dibromopropyl) phosphate (TEIS) were 9. 17 -366.80, 0.95 -75.98, 1.04 -83.20, 41.60-832.00, 3.80 -75.90, and 40.48 -809.60 μg/L, respectively, the correlation coefficients were not less than 0. 997 5 , while the limits of quantification ( LOQ) (S/N = 10) were 3.0, 0.2, 0.3, 25.0, 2.5 and 29.0 μg/kg, respectively. The spiked recoveries varied from 82. 62% to 96. 88% with the relative standard deviations of 3. 80% to 8. 79%. The proposedmethod was successfully applied to the determination of organophosphorous flame retardants in eight commercial textiles. The experimental results demonstrated that the method developed is simple, rapid, sensitive and accurate, which could satisfy the demand of the analysis of banned organophosphorous flame retardants in textiles.关键词
微波辅助萃取/气相色谱-串联质谱/有机磷阻燃剂/纺织品Key words
microwave assisted extraction (MAE)/ gas chromatography-tandem mass spec-trometry (GC-MS/MS)/ organophosphorous flame retardants/ textiles分类
化学化工引用本文复制引用
王成云,李丽霞,谢堂堂,张伟亚,刘彩明,褚乃清..微波辅助萃取-气相色谱-串联质谱法同时测定纺织品中6种有机磷阻燃剂[J].色谱,2011,29(8):731-736,6.基金项目
深圳出入境检验检疫局科技计划项目(SZ2010014)和国家认监委科研制标项目(2011B238k) （SZ2010014）
