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固相萃取法提取典型溶解有机质及其红外谱和固态13C核磁共振表征
武奕鑫1, 王孝聪2, 周振淞1, 何晨3, 潘良浩4, 宋桂雪1
1.山东大学海洋研究院;2.中国石油大学北京理学院 北京;3.中国石油大学北京重质油国家重点实验室 北京;4.广西科学院红树林研究中心
摘要:
由于海水盐度大、有机质含量低,从海水中提取和纯化克级溶解性有机质(DOM)一直十分困难。本研究基于Bond Elut PPL固相萃取小柱法进行海水DOM固体样品提取的放大试验,建立DOM自动化调酸、PPL树脂吸附技术,最后形成提纯、冷冻干燥PPL-DOM完整工艺。采用元素分析、EEM荧光光谱、红外光谱和固态13C核磁共振(NMR)波谱法进行样品表征。结果表明:(1)该方法对近海表层海水DOM回收率稳定在50%以上,搭建的提取装置DOM日吸附量可达230 mg;(2)鳌山湾四个季节批次PPL-DOM整体分析结果表明,样品的元素组成和光谱特征相似,表明方法适用性和稳定性较好;(3)三种水生态环境的PPL-DOM13C NMR谱图显示样品的基本特征相似,以烷基碳、碳水化合物碳、芳香碳和羧基碳/酰胺碳为主,其中偶极去相(Dipolar dephasing)谱显示了DOM前体化合物来源的差异。
关键词:  海洋溶解性有机质,固相萃取,Bond Elut PPL, 13C NMR,FTIR
DOI:
分类号:
基金项目:国家重点研发计划项目(2018YFA0605800)
EXTRACTION OF REPRESENTATIVE MARINE DISSOLVED ORGANIC MATTER BY SOILD PHASE EXTRACTION AND CHARACTERIZATION BY INFRARED SPECTROMETRY AND SOLID-STATE 13C NUCLEAR MAGNETIC RESONANCE
WU Yi-Xin1, WANG Xiao-Cong2, ZHOU Zhen-Song1, HE Chen3, PAN Liang-Hao4, SONG Gui-Xue1
1.Institute of Marine Science and Technology,Shandong University,Qingdao Campus,Qingdao;2.College of Science,China University of Petroleum Beijing,Beijing;3.State Key Laboratory of Heavy Oil Processing,China University of Petroleum Beijing,Beijing;4.Guangxi Mangrove Research Center of Guangxi Academy of Sciences
Abstract:
Due to high salinity and low concentration of marine dissolved organic carbon, it is a great challenge to extract and purify representative marine DOM in a gram-scale. We carried out a scale-up experiment based on the solid phase extraction(Bond Elut PPL)from seawaters, developed a set of customer-made device and optimized the automatic procedure of SPE extraction and finally PPL-DOMs were purified and freeze-dried. Elemental analysis, Excitation Emission Matrix (EEM) fluorescence spectroscopy, Fourier Transformed Infrared spectroscopy and Solid-state 13C Nuclear Magnet Resonances (NMR) spectroscopy were used to characterize PPL-DOM samples. Results indicate that(1)the extraction method was reliable with DOC recovery of greater than 50% and about 230 mg of DOM could be absorbed per day using the developed extraction device;(2)the bulk analyses of elemental composition and spectral characteristics of DOM samples isolated from seawaters of Aoshan Bay in four seasons showed overall similarity , generally indicated that this was applicable and reliable;(3)the 13 C NMR spectra of PPL - DOM from three different aquatic ecosystems showed that to some extent the characteristics of samples were similar with the features of aliphatic C, carbohydrate, aromatics and carboxylic/amides. However, differences of the DD spectra due to different sources of precursor compounds in DOM were distinct.
Key words:  Marine DOM  Solid Phase Extraction  Bond Elut PPL  13C NMR  FTIR
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