期刊
ANALYTICAL CHEMISTRY
卷 86, 期 22, 页码 11255-11262出版社
AMER CHEMICAL SOC
DOI: 10.1021/ac5038957
关键词
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资金
- CAPES (Coordenacao de Aperfeicoamento de Pessoal de Nivel Superior) [BEX 0495/13-1]
- Italian Ministry for the University and Research (MIUR) within the National Operative Project Hi-Life Health Products from the Industry of Foods [ID PON01_01499]
In this work, two analytical liquid chromatography methods were developed and compared for the characterization of aqueous phases from pyrolysis of lignocellulosic biomasses. NanoLC electron ionization-mass spectrometry (E1-MS) represents a novel and useful tool for a both separation and identification of semi/nonvolatile and a thermolabile molecules. The use of nanoscale flow rates, the highly reproducibility, and high detailed information on El spectra are the principal advantages of this technique. On the other hand, comprehensive 2D-LC, providing a two-dimen- 5 sional separation, increases the overall peak capacity lowering the occurrence of peak coelutions. Despite the use of reversed phase modes in both dimensions, a satisfactory degree of orthogonality was achieved by the employment of a smart design of gradient elution strategies in the second dimension incombination with photodiode array detection (PDA) and atmospheric pressure chemical ionization-mass spectrometry (APCIMS). Because of the absence of the preliminary extraction procedure, the fingerprint obtained for these samples results is independent of the extraction yield or contamination contrary to the gas chromatography-mass spectrometry (GC-MS) approach where a liquid liquid extraction of the water phase is necessary. The main classes of identified compounds were phenols, ketones, furans, and alcohols. The synergistic information on the two powerful analytical approaches, e.g., NanoLC El-MS and LC X LC, in the identification of such complex samples has never been investigated and fully benefit on the one hand from the superior degree of mass spectral information from El-MS and on the other hand from enhanced LC X LC compound separation.
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