Determination of Lignin in Marine Sediment Using Alkaline Cupric Oxide Oxidation-Solid Phase Extraction-on-Column Derivatization-Gas Chromatography

查看全文 作　　者：ZHANG [1]Ting;LI [1]Xianguo;SUN [1]Shuwen;LAN [1]Haiqing;DU [1]Peirui;WANG [1]Min

机构地区：[1]Key Laboratory of Marine Chemistry Theory and Technology,Ministry of Education Ocean University of China

出　　处：《Journal of Ocean University of China》索引2013年第12卷第1期,共7页

基　　金：supported by the National Basic Research Program of China (973 Program, Grant No. 2010CB428901);the National Natural Science Foundation of China (NSFC, Grant No. 41020164005,41276067);the team of 973 Program Grant No. 2010CB428701 for the help during sampling 摘　　要：Lignin serves as one of the most important molecular fossils for tracing Terrestrial Organic Matters (TOMs) in marine environment. Extraction and derivatization of lignin oxidation products (LOPs) are crucial for accurate quantification of lignin in marine sediment. Here we report a modification of the conventional alkaline cupric oxide (CuO) oxidation method, the modification consisting in a solid phase extraction (SPE) and a novel on-column derivatization being employed for better efficiency and reproducibility. In spiking blanks, recoveries with SPE for the LOPs are between 77.84% and 99.57% with relative standard deviations (RSDs) ranging from 0.57% to 8.04% (n=3), while those with traditional liquid-liquid extraction (LLE) are from 44.52% to 86.16% with RSDs being from 0.53% to 13.14% (n=3). Moreover, the reproducibility is greatly improved with SPE, with less solvent consumption and shorter processing time. The average efficiency of on-column derivatization for LOPs is 100.8% ± 0.68%, which is significantly higher than those of in-vial or in-syringe derivatization, thus resulting in still less consumption of derivatizing reagents. Lignin in the surface sediments sampled from the south of Yangtze River estuary, China, was determined with the established method. Recoveries of 72.66% to 85.99% with standard deviation less than 0.01mg/10g dry weight are obtained except for p-hydroxyben-zaldehyde. The lignin content Σ8 (produced from 10 g dry sediment) in the research area is between 0.231 and 0.587 mg. S/V and C/V ratios (1.028 ± 0.433 and 0.192 ± 0.066, respectively) indicate that the TOMs in this region are originated from a mixture of woody and nonwoody angiosperm plants; the high values of (Ad/Al) v suggest that the TOMs has been highly degraded. 关键词：衍生化气相色谱木质素含量海洋沉积物固相萃取柱氧化铜碱性相对标准偏差测定

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Determination of Lignin in Marine Sediment Using Alkaline Cupric Oxide Oxidation-Solid Phase Extraction-on-Column Derivatization-Gas Chromatography

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