分析化学Issue(3)：430-436,7.DOI:10.11895/j.issn.0253-3820.150739
多次溶剂萃取-气相色谱/串联质谱法测定热熔胶中的多环芳烃
Determination of Polycyclic Aromatic Hydrocarbons in Hot Melt Adhesive by Multiple Solvent Extraction Coupled with Gas Chromatography-Tandem Mass Spectrometry
摘要
Abstract
A method for multiple solvent extraction coupled with gas chromatography-tandem mass spectrometry ( GC-MS/MS ) was established for the simultaneous determination of 16 polycyclic aromatic hydrocarbons ( PAHs) in hot melt adhesive. The extraction conditions, purification conditions, chromatogphic conditions and tandem MS conditions of analysis were critically examined. The results were also compared with those obtained by gas chromatography-mass spectrometry ( GC-MS ) . The sample was extracted by ultrasonic extraction with n-hexane as solvent at 60℃. Then, the extract was purified by centrifugation after freezing treatment, twice extraction with dimethyl sulfoxide, twice re-extraction with n-hexane in turn. The purified extract was determined by gas chromatography-tandem mass spectrometry under multiple reaction monitoring (MRM) mode. The linear correlation coefficients were above 0. 9969, the limits of detection (LOD) ranged from 1. 0 μg/kg to 10 μg/kg, the relative standard deviations (RSDs) were below 6. 3%, and the recoveries ranged from 80. 4% to 117. 6% at three spiked levels. The matrix effects of tandem MS were studied, but there was no significance. Compared with GC-MS methods, the established method outperformed the GC-MS methods in LOD, which ranged from 23 μg/kg to 94 μg/kg for GC-MS, and could greatly enhance the accuracy of the qualitative and quantitative analysis of PAHs. The results indicated that the method was sensitive, accurate and reproducible, and suitable for the simultaneous determination of 16 PAHs in hot melt adhesive.关键词
多环芳烃/溶剂萃取/气相色谱-串联质谱/热熔胶Key words
Polycyclic aromatic hydrocarbons/Solvent extraction/Gas chromatography-tandem mass spectrometry/Hot melt adhesive引用本文复制引用
司晓喜,朱瑞芝,张凤梅,刘春波,徐艳群,李中昌,何沛,刘志华..多次溶剂萃取-气相色谱/串联质谱法测定热熔胶中的多环芳烃[J].分析化学,2016,(3):430-436,7.基金项目
本文系中国烟草总公司标准项目(No.2013QB015)和云南中烟工业有限责任公司科技开发项目(No.2015JC06)资助@@@@This work was supported by the standards project of China National Tobacco Company (No.2013QB015) and the Technological development projects of China Tobacco Yunnan Industrial Co., Ltd.(No.2015JC06) （No.2013QB015）
