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Proposed guidelines for sample preparation and ESI-MS analysis of humic substances to avoid self-esterification

机译:为避免自酯化而对腐殖质进行样品制备和ESI-MS分析的拟议指南

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摘要

Standard humic substances (HS) were stored in C-13-labelled methanol, ethanol, 2-propanol and d(3)-methanol to investigate whether they underwent self-esterification with the solvents or not. Data from stable carbon isotope analysis: C-13 NMR spectroscopy and electrospray ionisation mass spectrometry (ESI-MS) showed that significant self-esterification of carboxyl groups began immediately after dissolution. The major implication is that data collected in previous studies using these solvents in conjunction with HS are likely to be compromised. Self-esterification was minimised by varying parameters such as % water, temperature, concentration, storage time and buffer. Solvent reactivity was found to be: ethanol > 2-propanol > methanol. The study proposes preliminary guidelines for the preparation and storaqe of HS and their analysis by ESI-MS. The primary recommendation is to avoid the use of these solvents and use alternatives such as acetonitrile and water. (c) 2004 Elsevier Ltd. All rights reserved.
机译:将标准腐殖质(HS)储存在C-13标记的甲醇,乙醇,2-丙醇和d(3)-甲醇中,以调查它们是否与溶剂自酯化。稳定碳同位素分析的数据:C-13 NMR光谱和电喷雾电离质谱(ESI-MS)表明,溶解后,羧基立即开始显着自酯化。主要含义是,先前使用这些溶剂与HS结合进行的研究收集的数据可能会受到损害。通过改变诸如水的百分比,温度,浓度,储存时间和缓冲液等参数,可将自酯化反应降至最低。发现溶剂反应性为:乙醇> 2-丙醇>甲醇。该研究为HS的制备和储藏以及通过ESI-MS进行分析提供了初步指南。首要建议是避免使用这些溶剂,而使用乙腈和水等替代品。 (c)2004 Elsevier Ltd.保留所有权利。

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