Rapid, Quantitative Nuclear Magnetic Resonance Test for Oxygen-17 Enrichment in Water
Rapid, Quantitative Nuclear Magnetic Resonance Test for Oxygen-17 Enrichment in Water
复制标题
水中 O-17 富集度的快速定量核磁共振测试
DOI：
10.1021/acs.analchem.2c00081
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发表时间：
2022
影响因子：
7.4
通讯作者：
Harper, James K.
中科院分区：
文献类型：
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作者：
Peterson, Joshua W.;Burt, Scott R.;Yuan, Yu;Harper, James K.
涉及~(17)O的核磁共振研究在分子生物学、材料科学和其他学科中越来越重要。这些研究中有大量使用H_(17)O作为17O的来源，由于H_(17)O的高成本，这种依赖可能是有限的。为了克服这一限制，最近的一项研究提出了一种蒸馏方案，能够以低成本生产大量的H_217O。虽然这种方法被报道是有效的，但所提出的量化17O浓缩百分比的反应要么是时间密集型的，要么是由于同位素效应而有误差的风险。在这里，描述了一种替代的反应方案来测量17O水，最终生成含有SOL17O的产品苯甲酸甲酯。建议的反应在室温下在几分钟内完成，只产生一个17O产物，不需要净化步骤。在溶液核磁共振中观察到的13C═16O和13C═17O共振之间的大同位素位移允许单个峰的整合。这种13C核磁共振分析被发现在广泛的浓缩范围内具有很高的精确度，大多数核磁共振光谱学家都可以使用。
Nuclear magnetic resonance (NMR) studies involving17O are increasingly important in molecular biology, material science, and other disciplines. A large number of these studies employ H217O as a source of17O, and this reliance can be limiting because the high cost of H217O. To overcome this constraint, a recent study proposed a distillation scheme capable of producing significant quantities of H217O at a low cost. Although this method is reported to be effective, the reactions proposed to quantify percent of17O enrichment are either time intensive or have a risk of errors due to the isotope effect. Here, an alternative reaction scheme is described to measure17O water that ultimately creates methyl benzoate as the sole17O-containing product. The proposed reaction is completed in a matter of minutes at room temperature, produces only one17O product, and requires no clean-up step. The large isotope shift observed in solution NMR between the13C═16O and13C═17O resonances allows for integration of the individual peaks. This13C NMR analysis is found to be highly accurate over a wide enrichment range and is accessible to most NMR spectroscopists.