Quantitative super(1)H NMR with External Standards: Use in Preparation of Calibration Solutions for Algal Toxins and Other Natural Products

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DOIResolve DOI: http://doi.org/10.1021/ac048385h
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TypeArticle
Journal titleAnalytical Chemistry
Volume77
Issue10
Pages31233131; # of pages: 9
Subjecthazardous materials; metabolites; N.M.R.; probes; solvents; toxicants; toxins; natural products
AbstractWe examine the use of external standards for quantitative measurement by 1H NMR of solution concentrations of natural products and other low molecular weight, hydrogen-containing compounds and show that precision and accuracy ca. 1% is obtainable with a commercial 11.7 T spectrometer when standards and analytes are contained in separate but identical sealed precision glass NMR tubes. Numerous factors contributing to the intensity of the NMR signals are evaluated. Precise measurements of 360 pulse lengths for each sample provide direct corrections for variations in probe Q-factor that enable samples in different solvents to be compared, provided single-coil excitation and detection is used throughout. Samples need not be prepared in deuterated solvents if the 1H spectra of the solvents are simple enough for peak suppression by presaturation. The approach is particularly suitable for hazardous materials kept in sealed tubes and for the preparation of certified calibration solution reference materials for use with LC-MS and other techniques where deuterated solvents should be avoided.
Publication date
PublisherACS Publications
Copyright noticeCopyright © 2007 American Chemical Society
LanguageEnglish
AffiliationNRC Institute for Marine Biosciences; National Research Council Canada; Aquatic and Crop Resource Development; Measurement Science and Standards
Peer reviewedYes
NRC number1324
NPARC number3538057
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Record identifierb509bae8-2762-458c-8e0b-ac4d55d15b6a
Record created2009-03-01
Record modified2016-05-09
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