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NMR method for differentiating complex mixtures

a complex mixture and nmr technology, applied in chemical methods analysis, nuclear magnetic resonance analysis, instruments, etc., can solve the problems of severe overlap of many complex mixtures, compromise of quantitative measurement ability,

Inactive Publication Date: 2007-03-08
PURDUE RES FOUND INC
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Benefits of technology

[0008] The present teachings are directed to a method for differentiating complex mixtures each having one or more chemical species. The method comprises producing a sample NMR spectrum by subjecting a mixture to a selective spectroscopy process, wherein the NMR spectrum has individual spectral peaks representative of the one or more chemical species within the mixture. The one or more chemical species within the mixture are identified by analyzing the individual spectral peaks, and the individual spectral peaks are then subjected to a multivariate statistical analysis.

Problems solved by technology

However, when measuring the components of complex mixtures, overlapping resonances often result, which thus compromises the ability to measure concentrations quantitatively.
Even small molecules often give rise to 20 or more spectral lines in the 1H NMR spectrum, leading to severe overlap for many complex mixtures.

Method used

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[0032] NMR Samples: L-Amino Acids and TSP (sodium 3-trimethylsilyl (2,2,3,3 2H4) i-propionate) were purchased from Sigma-Aldrich (St. Louis, Mo.) and used without further purification. For NMR analysis, amino acid solutions were prepared in 50 mM phosphate buffer at pH 7. Human urine was collected from the volunteers. A sample of urine collected from a male adult Sprague-Dawley rat was the generous donation of Dr. Peter Kissenger and Dr. Chester Duda of Bioanalytical Systems, Inc. (West Lafayette. Ind.). For NMR analysis, urine samples were prepared by the addition of 60 μl of 1 M phosphate buffer, pH 7, to 540 μl of neat urine. For the PCA study, urine samples were collected at three time points during the day, and these samples were split into thirds, forming 9 samples, 6 of which were spiked with varying concentrations of isoleucine. All NMR samples were run in 5 mm tubes with 10% added D2O (Cambridge Isotopes Laboratory, Inc.) and 50 μl TSP.

[0033] NMR Spectroscopy: NMR spectra ...

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Abstract

A method for differentiating complex mixtures each having one or more chemical species is provided. The method comprises producing a sample NMR spectrum by subjecting a mixture to a selective spectroscopy process, wherein the NMR spectrum has individual spectral peaks representative of the one or more chemical species within the mixture. The one or more chemical species within the mixture are identified by analyzing the individual spectral peaks, and the individual spectral peaks are then subjected to a multivariate statistical analysis.

Description

RELATED APPLICATIONS [0001] This application claims priority to U.S. Provisional Patent Application Ser. No. 60 / 712,786 filed Aug. 31, 2005, the disclosure of which is expressly incorporated herein by reference.[0002] This invention was made with government support under grant reference number NIH / NIDDK 3R21 DK070290-01 awarded by the NIH Roadmap Initiative on Metabolomics Technology. The Government has or may have certain rights in the invention.TECHNICAL FIELD [0003] The present invention is directed toward high-resolution NMR analysis of chemical structures, and more particularly to the use of selective total correlation spectroscopy (“TOCSY”) to quantify and analyze a predetermined set of chemical species. BACKGROUND OF THE INVENTION [0004] It is well known that nuclear magnetic resonance (NMR) spectroscopy provides extremely highly detailed information on molecular structure. NMR is also quantitative because the detected signal is linearly proportional to the absolute number of...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): G06F19/00
CPCG01N24/08G01R33/465G01R33/4625
Inventor RAFTERY, DANIELSANDUSKY, PETER
Owner PURDUE RES FOUND INC
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