煤吡啶抽提过程中柱色谱与索氏提取法对富集物组成的影响  

Influence of Column Chromatography and Soxhlet Extraction on the Composition of Coal Pyridine Soluble

作　　者：李文英[1] 叶翠平[1] 冯杰[1] 谢克昌[1] 

机构地区：[1]太原理工大学煤科学与技术教育部和山西省重点实验室,太原030024

出　　处：《分析化学》2006年第7期905-909,共5页Chinese Journal of Analytical Chemistry

基　　金：长江学者和创新团队发展计划;国家自然科学基金(No.20476068;No.90410018);山西省自然科学青年基金(No.20041008);教育部科学技术研究重点项目(No.204021);973项目(No.2004CB2176002)共同资助

摘　　要：为考察柱色谱分离和索氏提取两种固体样品提取方法对提取物组成的影响,探索操作条件温和、溶剂使用量经济的固体样品提取方法.本研究以吡啶为溶剂,对准葛尔黑岱沟、平朔、潞安常村3种不同变质程度的煤样进行了柱色谱分离和索氏抽提.提取物用凝胶色谱、电喷雾质谱和同步荧光光谱进行分析,比较和确定不同提取方法对煤提取物中组分分子量分布和结构的影响.分析发现,柱色谱分离与索氏提取相比,抽提率略有增加,但柱色谱提取物组分中缺失了提取样品中结构稳定的超大分子结构片断;质谱结果显示柱色谱抽提物中主要存在5个组分,提取物组分相对于索氏提取物单一、富集度高;同步荧光显示柱色谱提取物中芳香化合物的基本组成为3～5个环的芳香化合物.实验结果表明：如仅分析质量数小于1000 amu的化合物,柱色谱法可替代索氏提取法.This study discussed the composition of coal pyridine soluble from column-chromatography （CC） and the Soxhlet extraction method. A, B and C coal samples were extracted by pyridine using CC and Soxhlet extraction methods at 25~C and 120~C, respectively. Gel permeation chromatography （GPC） coupled with photo diode array （PDA） detector was applied to determine molecular weight （MW） distribution and structure characteristics within the range of 210 -400 nm. Electrospray ionization mass spectrometer （ESI-MS） and synchronous fluorescence spectroscopy with constant wavenumber were employed to investigate the detailed structure features and poly-aromatic property. Results showed that the pyridine extraction ratio of CC was higher than that of Soxhlet method although some compounds with ultra high MW were filtered by silica gel used in CC. The extracts from CC could present better S/N （signal to noise） diagram in MS spectra, five individual compounds had been identified that mainly consist of 3 -5 aromatic rings. Nevertheless, there are lots of impurity information from Soxhlet extracts in MS spectra and difficult to make further structure analysis. In conclusion, CC would be a better substitute of Soxhlet extraction if we just concern the compounds with less than 1000 ainu MW.

关 键 词：煤吡啶提取物 柱色谱 索氏抽提 凝胶渗透色谱 电喷雾质谱 同步荧光 

分 类 号：TQ533[化学工程—煤化学工程]