Examples Showing the Utility of Doping Experiments in 1H NMR Analysis of Mixtures

被引:2
作者
Kaicharla, Trinadh [1 ]
Chinta, Bhavani Shankar [1 ]
Hoye, Thomas R. [1 ]
机构
[1] Univ Minnesota, Dept Chem, Minneapolis, MN 55455 USA
基金
美国国家科学基金会;
关键词
NUCLEAR-MAGNETIC-RESONANCE; NMR; IDENTIFICATION; SPECTROSCOPY; REAGENT;
D O I
10.1021/acs.joc.1c03127
中图分类号
O62 [有机化学];
学科分类号
070303 ; 081704 ;
摘要
Here we provide examples that demonstrate the value of using properly designed and easily performed doping experiments to give insights about the nature of the analyte(s) present in a H-1 NMR sample. Two mixtures, the first quite complex and the second far less so, have been chosen: (i) the crude pyrolysate from reaction of butyric acid in (supercritical) water at 600 degrees C and (ii) a mixture of two basic amines. In the former, 13 distinct carbonyl-containing compounds, ranging in relative concentration of nearly 2 orders of magnitude, were positively identified. The latter highlights the advantage of using a doping experiment as opposed to merely comparing the spectra from two separate samples containing the same analyte.
引用
收藏
页码:5660 / 5667
页数:8
相关论文
共 27 条
  • [1] PYROLYSIS OF UNSATURATED-COMPOUNDS .2. PYROLYSIS OF KETONES
    BAILEY, WJ
    CESARE, F
    [J]. JOURNAL OF ORGANIC CHEMISTRY, 1978, 43 (07) : 1421 - 1423
  • [2] Catalytic advancements in carboxylic acid ketonization and its perspectives on biomass valorisation
    Boekaerts, Bert
    Sels, Bert F.
    [J]. APPLIED CATALYSIS B-ENVIRONMENTAL, 2021, 283 (283)
  • [3] The peroxidation of chloroform
    Chapman, AT
    [J]. JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1935, 57 (01) : 419 - 422
  • [4] PROTON TRANSFERS OF SUBSTITUTED AMMONIUM-SALTS .13. N-INVERSION OF PIPERIDINES IN AQUEOUS ACIDIC SOLUTIONS
    DELPUECH, JJ
    DESCHAMPS, MN
    [J]. TETRAHEDRON, 1978, 34 (19) : 3017 - 3021
  • [5] A guide to the identification of metabolites in NMR-based metabonomics/metabolomics experiments
    Dona, Anthony C.
    Kyriakides, Michael
    Scott, Flora
    Shephard, Elizabeth A.
    Varshavi, Dorsa
    Veselkov, Kirill
    Everett, Jeremy R.
    [J]. COMPUTATIONAL AND STRUCTURAL BIOTECHNOLOGY JOURNAL, 2016, 14 : 135 - 153
  • [6] NMR Spectroscopy for Metabolomics Research
    Emwas, Abdul-Hamid
    Roy, Raja
    McKay, Ryan T.
    Tenori, Leonardo
    Saccenti, Edoardo
    Gowda, G. A. Nagana
    Raftery, Daniel
    Alahmari, Fatimah
    Jaremko, Lukasz
    Jaremko, Mariusz
    Wishart, David S.
    [J]. METABOLITES, 2019, 9 (07)
  • [7] Hydrothermal catalysis of waste greases into green gasoline, jet, and diesel biofuels in continuous flow supercritical water
    Fedie, Ronald L.
    McNeff, Clayton, V
    McNeff, Charles, V
    McNeff, Larry C.
    Greuel, Peter G.
    Yan, Bingwen
    Jenkins, Julie A.
    Brethorst, Jason T.
    Frost, Grant B.
    Hoye, Thomas R.
    [J]. BIOFUELS BIOPRODUCTS & BIOREFINING-BIOFPR, 2022, 16 (02): : 349 - 369
  • [8] TMS is Superior to Residual CHCl3 for Use as the Internal Reference for Routine 1H NMR Spectra Recorded in CDCl3
    Guzman, Alexander L.
    Hoye, Thomas R.
    [J]. JOURNAL OF ORGANIC CHEMISTRY, 2022, 87 (02) : 905 - 909
  • [9] No-D NMR (No-Deuterium proton NMR) spectroscopy: A simple yet powerful method for analyzing reaction and reagent solutions
    Hoye, TR
    Eklov, BM
    Ryba, TD
    Voloshin, M
    Yao, LJ
    [J]. ORGANIC LETTERS, 2004, 6 (06) : 953 - 956
  • [10] Precise NMR Method for Titering Organometal Reagents
    Jakhar, Vineet K.
    Johnson, Eric C.
    Kavuturu, Aditya
    Heller, Jessica K.
    Veige, Adam S.
    Ghiviriga, Ion
    [J]. ORGANIC LETTERS, 2021, 23 (13) : 4945 - 4948