Simpson Andre J, Tseng Li-Hong, Simpson Myrna J, Spraul Manfred, Braumann Ulrich, Kingery William L, Kelleher Brian P, Hayes Michael H B
Department of Physical and Environmental Sciences, University of Toronto, Scarborough Campus, Toronto, ON, Canada.
Analyst. 2004 Dec;129(12):1216-22. doi: 10.1039/b408064e. Epub 2004 Oct 15.
Non-living natural organic matter (NOM) is ubiquitous in the oceans, atmosphere, sediments, and soils, and represents the most abundant organic carbon reserves on earth. However, a large proportion is considered to be "molecularly uncharacterized" because the inherent complexity of NOM is problematic when applying conventional analytical techniques. This manuscript presents initial applications of LC-NMR (1H) and LC-SPE-NMR (1H) to the studies of NOM isolated from water and soil. LC-NMR is applied to dissolved natural organic matter (DNOM) collected from freshwater environments, and both LC-NMR and LC-SPE-NMR are applied to an alkaline soil extract. The polar and complex nature of the DNOM samples limits conventional reversed phase separation, which can be partially overcome with the use of an ion pair reagent, although such an approach further complicates the NMR detection. LC-SPE-NMR of the soil alkaline extract was encouraging, and specific components in the mixture could be assigned. This work demonstrates that it is both possible to separate and concentrate specific components in NOM such that NMR detection is possible. As NMR information will be critical in unraveling the novel and/or complex structures in NOM this represents a key analytical hurdle in this area.
非生物天然有机物(NOM)广泛存在于海洋、大气、沉积物和土壤中,是地球上最丰富的有机碳储备。然而,很大一部分被认为是“分子特征不明的”,因为在应用传统分析技术时,NOM固有的复杂性存在问题。本文介绍了液相色谱-核磁共振(1H)和液相色谱-固相萃取-核磁共振(1H)在从水和土壤中分离出的NOM研究中的初步应用。液相色谱-核磁共振应用于从淡水环境中收集的溶解态天然有机物(DNOM),液相色谱-核磁共振和液相色谱-固相萃取-核磁共振都应用于碱性土壤提取物。DNOM样品的极性和复杂性限制了传统的反相分离,使用离子对试剂可部分克服这一问题,尽管这种方法会使核磁共振检测进一步复杂化。土壤碱性提取物的液相色谱-固相萃取-核磁共振结果令人鼓舞,混合物中的特定成分可以被鉴定出来。这项工作表明,在NOM中分离和浓缩特定成分并进行核磁共振检测是可行的。由于核磁共振信息对于揭示NOM中的新结构和/或复杂结构至关重要,这代表了该领域的一个关键分析障碍。