Dr. Eul Hyun Suh, Dr. James Ratnakar, Dr. Jaspal Singh, Prof. Zoltan Kovacs
{"title":"77Se核的溶解动力学核极化","authors":"Dr. Eul Hyun Suh, Dr. James Ratnakar, Dr. Jaspal Singh, Prof. Zoltan Kovacs","doi":"10.1002/anse.202200086","DOIUrl":null,"url":null,"abstract":"<p><sup>77</sup>Se is a spin <math>\n \n <semantics>\n \n <mrow>\n <mn>1</mn>\n <mo>/</mo>\n <mn>2</mn>\n </mrow>\n \n <annotation>\n ${{ 1/2 }}$\n</annotation>\n </semantics>\n </math>\n, low sensitivity nucleus with a natural abundance of 7.6 %. Although <sup>77</sup>Se NMR is very useful in the characterization of selenium containing molecules including seleno-proteins, the detection of <sup>77</sup>Se is challenging in biological samples without enrichment. Therefore, the goal of this work was to establish whether the <sup>77</sup>Se signal could be enhanced in the liquid state by dissolution dynamic nuclear polarization (DNP) NMR without the need of enrichment. The dominant spin-lattice relaxation mechanism for <sup>77</sup>Se is via chemical shift anisotropy, which is highly dependent on the molecular symmetry. Here we tested three selenium compounds (sodium selenate, sodium selenite and selenocystine) with different molecular symmetries in dissolution DNP experiments and demonstrated that <sup>77</sup>Se DNP using commercially available hardware is feasible but the achieved NMR signal enhancements (1368-fold for selenate, 125-fold for selenite and no enhancement for selenocystine at 9.4 T) were strongly dependent on molecular symmetry.</p>","PeriodicalId":72192,"journal":{"name":"Analysis & sensing","volume":null,"pages":null},"PeriodicalIF":3.4000,"publicationDate":"2022-10-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Dissolution Dynamic Nuclear Polarization of the 77Se Nucleus\",\"authors\":\"Dr. Eul Hyun Suh, Dr. James Ratnakar, Dr. Jaspal Singh, Prof. Zoltan Kovacs\",\"doi\":\"10.1002/anse.202200086\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p><sup>77</sup>Se is a spin <math>\\n \\n <semantics>\\n \\n <mrow>\\n <mn>1</mn>\\n <mo>/</mo>\\n <mn>2</mn>\\n </mrow>\\n \\n <annotation>\\n ${{ 1/2 }}$\\n</annotation>\\n </semantics>\\n </math>\\n, low sensitivity nucleus with a natural abundance of 7.6 %. Although <sup>77</sup>Se NMR is very useful in the characterization of selenium containing molecules including seleno-proteins, the detection of <sup>77</sup>Se is challenging in biological samples without enrichment. Therefore, the goal of this work was to establish whether the <sup>77</sup>Se signal could be enhanced in the liquid state by dissolution dynamic nuclear polarization (DNP) NMR without the need of enrichment. The dominant spin-lattice relaxation mechanism for <sup>77</sup>Se is via chemical shift anisotropy, which is highly dependent on the molecular symmetry. Here we tested three selenium compounds (sodium selenate, sodium selenite and selenocystine) with different molecular symmetries in dissolution DNP experiments and demonstrated that <sup>77</sup>Se DNP using commercially available hardware is feasible but the achieved NMR signal enhancements (1368-fold for selenate, 125-fold for selenite and no enhancement for selenocystine at 9.4 T) were strongly dependent on molecular symmetry.</p>\",\"PeriodicalId\":72192,\"journal\":{\"name\":\"Analysis & sensing\",\"volume\":null,\"pages\":null},\"PeriodicalIF\":3.4000,\"publicationDate\":\"2022-10-31\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Analysis & sensing\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://onlinelibrary.wiley.com/doi/10.1002/anse.202200086\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q2\",\"JCRName\":\"CHEMISTRY, ANALYTICAL\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Analysis & sensing","FirstCategoryId":"1085","ListUrlMain":"https://onlinelibrary.wiley.com/doi/10.1002/anse.202200086","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"CHEMISTRY, ANALYTICAL","Score":null,"Total":0}
Dissolution Dynamic Nuclear Polarization of the 77Se Nucleus
77Se is a spin
, low sensitivity nucleus with a natural abundance of 7.6 %. Although 77Se NMR is very useful in the characterization of selenium containing molecules including seleno-proteins, the detection of 77Se is challenging in biological samples without enrichment. Therefore, the goal of this work was to establish whether the 77Se signal could be enhanced in the liquid state by dissolution dynamic nuclear polarization (DNP) NMR without the need of enrichment. The dominant spin-lattice relaxation mechanism for 77Se is via chemical shift anisotropy, which is highly dependent on the molecular symmetry. Here we tested three selenium compounds (sodium selenate, sodium selenite and selenocystine) with different molecular symmetries in dissolution DNP experiments and demonstrated that 77Se DNP using commercially available hardware is feasible but the achieved NMR signal enhancements (1368-fold for selenate, 125-fold for selenite and no enhancement for selenocystine at 9.4 T) were strongly dependent on molecular symmetry.