分析化学2012，Vol.40Issue(11)：1758-1763,6.DOI:10.3724/SP.J.1096.2012.20523
手性气相色谱质谱法测定莲藕及底泥中的多氯联苯对映体
Determination of Polychlorinated Biphenyls Enantiomers in Lotus Root and Sediment by Chiral Gas Chromatography-Mass Spectrometry
摘要
Abstract
An enantioselective method was developed for separation and determination of six chiral polychlorinated biphenyls (PCBs) including PCB 91, 95, 136, 149, 176 and 183 in lotus root, stem, leal and sediment by GOMS. After optimizations of instrumental parameters for enantiomeric separation and investigations of sample preparations including accelerated solvent extraction (ASE) parameters, extraction solvents and cleanup methods, PCBs enantiomers were extracted from samples by ASE with n-hcxane/acetone (1:1, V/V) at 100 ℃ and 10. 3 MPa for 10 min. The extracts were orderly sulphonated by sulfuric acid, purified by Florisil solid phase extraction column, reconstituted with isooctane after being concentrated, and respectively detected by GC-MS with Chirasil-Dex and BGB-172 columns. For all PCBs enantiomers, good linearities were obtained in the concentration range of 0. 5 - 100 μg/L, and recoveries of spiked samples at 0. 25, 2. 5 and 25 μg/kg levels were 82. 8% - 117. 0% with relative standard deviations (RSD) of 1. 5% - 13. 6%. Limits of detection (LOD) and limits of quantification (LOQ) were 0. 01-0. 02 μg/kg and 0. 025 - 0. 04 μg/kg, respectively. The real samples analysis showed that chiral PCBs were not detected in lotus roots from markets, but higher concentrations were found in lotus root and sediment from contaminated area. The concentrations of PCB 91-2, PCB 95-1 and ( + )- PCB 136 in lotus root, stem and leaf were respectively higher than those of their enantiomers, while no significant differences between two enantiomers of PCB 149, 176 and 183.关键词
多氯联苯/对映体/气相色谱质谱/加速溶剂萃取/莲藕/底泥Key words
Polychlorinated biphenyls/ Enantiomer/ Gas chromatography-mass spectrometry/ Accelerated solvent extraction/ Lotus root/ Sediment引用本文复制引用
戴守辉,赵桦林,王敏,Charles S.Wang,柴婷婷,杨曙明,邱静..手性气相色谱质谱法测定莲藕及底泥中的多氯联苯对映体[J].分析化学,2012,40(11):1758-1763,6.基金项目
本文系国家自然科学基金(No.20907073)资助项目 （No.20907073）
