分析测试学报2012,Vol.31Issue(9):1146-1150,5.DOI:10.3969/j.issn.1004-4957.2012.09.022
生物样品中手性多氯联苯对映体的分离测定
Enantiomer Separations of Chiral Polychlorinated Biphenyls in Biological Samples
摘要
Abstract
A method was developed for the separation and determination of 12 chiral polychlorinated biphenyls(PCBs), i.e. CB 45, CB 84, CB 91, CB 95, CB 131, CB 132, CB 136, CB 149, CB 171, CB 174, CB 176 and CB 183, in biological samples. The target chemicals were Soxhlet extracted , cleaned up by gel permeation chromatography and multi-layer silica alumina column, and were further fractioned with a Florisil column. The chiral PCBs were identified and quantified by gas chromatography - mass spectrometry with electron impact ion source (GC -EI/MS). The peak resolutions of these chiral congeners ranged from 0. 5 to 2. 1. The relative standard deviations of the calculated enantiomeric fractions ( EFs) in triplicates were less than 2% . The enantiomers of CBs 84, CB 91 and CB 174 in the standard solutions were separated by two different chiral columns. There was a slight discrepancy in the calculated EFs between the two columns, with relative standard deviations of 1. 2% , 0. 2% and 0. 2% for CB 84, CB 91 and CB 174, respectively, suggesting the high degree of accuracy and efficiency of the established method.a关键词
气相色谱-质谱联用/多氯联苯/生物样品/手性/对映体/分离Key words
gas chromatography - mass spectrometry/ polychlorinated biphenyl/ biological sample/chiral/ enantiomer/ separation分类
化学化工引用本文复制引用
张荧,吴江平,罗孝俊,佘雅哲,莫凌,向同寿,麦碧娴..生物样品中手性多氯联苯对映体的分离测定[J].分析测试学报,2012,31(9):1146-1150,5.基金项目
国家重点基础研究发展计划项目(2009CB421604) (2009CB421604)
国家自然科学基金项目(41073081,41103054,40821003) (41073081,41103054,40821003)