Katelyn Downey, Wolfgang Bermel, Ronald Soong, Daniel H. Lysak, Kiera Ronda, Katrina Steiner, Peter M. Costa, William W. Wolff, Venita Decker, Falko Busse, Benjamin Goerling, Agnes Haber, Myrna J. Simpson, Andre J. Simpson
{"title":"低场,而不是低质量:1D简化、选择性检测和异核2D实验,用于改进环境和生物样品的低场NMR光谱。","authors":"Katelyn Downey, Wolfgang Bermel, Ronald Soong, Daniel H. Lysak, Kiera Ronda, Katrina Steiner, Peter M. Costa, William W. Wolff, Venita Decker, Falko Busse, Benjamin Goerling, Agnes Haber, Myrna J. Simpson, Andre J. Simpson","doi":"10.1002/mrc.5401","DOIUrl":null,"url":null,"abstract":"<p>Understanding environmental change is challenging and requires molecular-level tools to explain the physicochemical phenomena behind complex processes. Nuclear magnetic resonance (NMR) spectroscopy is a key tool that provides information on both molecular structures and interactions but is underutilized in environmental research because standard “high-field” NMR is financially and physically inaccessible for many and can be overwhelming to those outside of disciplines that routinely use NMR. “Low-field” NMR is an accessible alternative but has reduced sensitivity and increased spectral overlap, which is especially problematic for natural, heterogeneous samples. Therefore, the goal of this study is to investigate and apply innovative experiments that could minimize these challenges and improve low-field NMR analysis of environmental and biological samples. Spectral simplification (JRES, PSYCHE, singlet-only, multiple quantum filters), selective detection (GEMSTONE, DREAMTIME), and heteronuclear (reverse and CH<sub>3</sub>/CH<sub>2</sub>/CH-only HSQCs) NMR experiments are tested on samples of increasing complexity (amino acids, spruce resin, and intact water fleas) at-high field (500 MHz) and at low-field (80 MHz). A novel experiment called Doubly Selective HSQC is also introduced, wherein <sup>1</sup>H signals are selectively detected based on the <sup>1</sup>H and <sup>13</sup>C chemical shifts of <sup>1</sup>H–<sup>13</sup>C J-coupled pairs. The most promising approaches identified are the selective techniques (namely for monitoring), and the reverse and CH<sub>3</sub>-only HSQCs. Findings ultimately demonstrate that low-field NMR holds great potential for biological and environmental research. The multitude of NMR experiments available makes NMR tailorable to nearly any research need, and low-field NMR is therefore anticipated to become a valuable and widely used analytical tool moving forward.</p>","PeriodicalId":18142,"journal":{"name":"Magnetic Resonance in Chemistry","volume":"62 5","pages":"345-360"},"PeriodicalIF":1.9000,"publicationDate":"2023-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Low-field, not low quality: 1D simplification, selective detection, and heteronuclear 2D experiments for improving low-field NMR spectroscopy of environmental and biological samples\",\"authors\":\"Katelyn Downey, Wolfgang Bermel, Ronald Soong, Daniel H. Lysak, Kiera Ronda, Katrina Steiner, Peter M. Costa, William W. Wolff, Venita Decker, Falko Busse, Benjamin Goerling, Agnes Haber, Myrna J. Simpson, Andre J. Simpson\",\"doi\":\"10.1002/mrc.5401\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p>Understanding environmental change is challenging and requires molecular-level tools to explain the physicochemical phenomena behind complex processes. Nuclear magnetic resonance (NMR) spectroscopy is a key tool that provides information on both molecular structures and interactions but is underutilized in environmental research because standard “high-field” NMR is financially and physically inaccessible for many and can be overwhelming to those outside of disciplines that routinely use NMR. “Low-field” NMR is an accessible alternative but has reduced sensitivity and increased spectral overlap, which is especially problematic for natural, heterogeneous samples. Therefore, the goal of this study is to investigate and apply innovative experiments that could minimize these challenges and improve low-field NMR analysis of environmental and biological samples. Spectral simplification (JRES, PSYCHE, singlet-only, multiple quantum filters), selective detection (GEMSTONE, DREAMTIME), and heteronuclear (reverse and CH<sub>3</sub>/CH<sub>2</sub>/CH-only HSQCs) NMR experiments are tested on samples of increasing complexity (amino acids, spruce resin, and intact water fleas) at-high field (500 MHz) and at low-field (80 MHz). A novel experiment called Doubly Selective HSQC is also introduced, wherein <sup>1</sup>H signals are selectively detected based on the <sup>1</sup>H and <sup>13</sup>C chemical shifts of <sup>1</sup>H–<sup>13</sup>C J-coupled pairs. The most promising approaches identified are the selective techniques (namely for monitoring), and the reverse and CH<sub>3</sub>-only HSQCs. Findings ultimately demonstrate that low-field NMR holds great potential for biological and environmental research. The multitude of NMR experiments available makes NMR tailorable to nearly any research need, and low-field NMR is therefore anticipated to become a valuable and widely used analytical tool moving forward.</p>\",\"PeriodicalId\":18142,\"journal\":{\"name\":\"Magnetic Resonance in Chemistry\",\"volume\":\"62 5\",\"pages\":\"345-360\"},\"PeriodicalIF\":1.9000,\"publicationDate\":\"2023-10-09\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Magnetic Resonance in Chemistry\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://onlinelibrary.wiley.com/doi/10.1002/mrc.5401\",\"RegionNum\":3,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q3\",\"JCRName\":\"CHEMISTRY, MULTIDISCIPLINARY\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Magnetic Resonance in Chemistry","FirstCategoryId":"92","ListUrlMain":"https://onlinelibrary.wiley.com/doi/10.1002/mrc.5401","RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q3","JCRName":"CHEMISTRY, MULTIDISCIPLINARY","Score":null,"Total":0}
Low-field, not low quality: 1D simplification, selective detection, and heteronuclear 2D experiments for improving low-field NMR spectroscopy of environmental and biological samples
Understanding environmental change is challenging and requires molecular-level tools to explain the physicochemical phenomena behind complex processes. Nuclear magnetic resonance (NMR) spectroscopy is a key tool that provides information on both molecular structures and interactions but is underutilized in environmental research because standard “high-field” NMR is financially and physically inaccessible for many and can be overwhelming to those outside of disciplines that routinely use NMR. “Low-field” NMR is an accessible alternative but has reduced sensitivity and increased spectral overlap, which is especially problematic for natural, heterogeneous samples. Therefore, the goal of this study is to investigate and apply innovative experiments that could minimize these challenges and improve low-field NMR analysis of environmental and biological samples. Spectral simplification (JRES, PSYCHE, singlet-only, multiple quantum filters), selective detection (GEMSTONE, DREAMTIME), and heteronuclear (reverse and CH3/CH2/CH-only HSQCs) NMR experiments are tested on samples of increasing complexity (amino acids, spruce resin, and intact water fleas) at-high field (500 MHz) and at low-field (80 MHz). A novel experiment called Doubly Selective HSQC is also introduced, wherein 1H signals are selectively detected based on the 1H and 13C chemical shifts of 1H–13C J-coupled pairs. The most promising approaches identified are the selective techniques (namely for monitoring), and the reverse and CH3-only HSQCs. Findings ultimately demonstrate that low-field NMR holds great potential for biological and environmental research. The multitude of NMR experiments available makes NMR tailorable to nearly any research need, and low-field NMR is therefore anticipated to become a valuable and widely used analytical tool moving forward.
期刊介绍:
MRC is devoted to the rapid publication of papers which are concerned with the development of magnetic resonance techniques, or in which the application of such techniques plays a pivotal part. Contributions from scientists working in all areas of NMR, ESR and NQR are invited, and papers describing applications in all branches of chemistry, structural biology and materials chemistry are published.
The journal is of particular interest not only to scientists working in academic research, but also those working in commercial organisations who need to keep up-to-date with the latest practical applications of magnetic resonance techniques.