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Quantitative method of one-dimensional nuclear magnetic resonance mixture jointly utilizing different nucleuses

A nuclear magnetic resonance and mixture technology, applied in the field of analytical chemistry, can solve problems affecting the accurate quantification of a single compound, and achieve the effect of simple sample preparation

Inactive Publication Date: 2014-12-10
KUNMING INST OF BOTANY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to adopt a quick and easy one-dimensional nuclear magnetic resonance experiment scheme to accurately determine the content of multiple monomer compounds in the mixture, so as to solve the problem of affecting the accurate quantification of individual compounds due to signal overlap in conventional proton spectra

Method used

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  • Quantitative method of one-dimensional nuclear magnetic resonance mixture jointly utilizing different nucleuses
  • Quantitative method of one-dimensional nuclear magnetic resonance mixture jointly utilizing different nucleuses
  • Quantitative method of one-dimensional nuclear magnetic resonance mixture jointly utilizing different nucleuses

Examples

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Effect test

Embodiment 1

[0042] Concentration determination and consistency comparison of tert-butyl phosphate in a model mixture of trimethylphosphine oxide and tert-butyl phosphate:

[0043] In order to verify the feasibility of using one-dimensional proton nuclear magnetic resonance spectrum and phosphorus spectrum as a quantitative analysis method, the present invention uses a series of trimethylphosphine oxide ((CH 3 ) 3 P(O), TMPO) and tert-butyl phosphate ((CH 3 ) 3 CP(O)(OH) 2 The model mixture of TBPA) was used as the research object, and the consistency of the quantitative results obtained by using one-dimensional H-NMR spectrum and phosphorus spectrum were first verified.

[0044] Reagents used and sample preparation: Trimethylphosphine oxide and tert-butyl phosphoric acid with a purity of 98% were purchased from Adamas-beta (Basel, Switzerland) and Across (New Jersey, USA), respectively. 99.9% heavy water (D 2 O) was purchased from CIL (Cambridge Isotope Laboratories; Massachusetts, U...

Embodiment 2

[0050] Determination of the absolute concentration of each component compound in the model mixture of choline, phosphorylcholine and glycerophosphorylcholine:

[0051] In order to further verify the feasibility of using nuclear magnetic resonance one-dimensional hydrogen spectrum and phosphorus spectrum for quantitative analysis, the present invention selects the mixture of choline, phosphorylcholine and glycerophosphorylcholine as a research example, and uses trimethylphosphine oxide as the hydrogen spectrum It is a universal quantitative internal standard for phosphate spectra, and accurately determines the absolute concentration and relative concentration ratio of each component compound.

[0052] Reagents used and sample preparation: choline chloride with a purity of 99%, phosphorylcholine chloride calcium salt tetrahydrate with a purity of 98% and phosphorylcholine glycerol were purchased from Adamas-beta (Basel, Switzerland). Weigh 74.9 mg of choline chloride, 54.8 mg of...

Embodiment 3

[0071] Determination of the relative concentration ratios of the individual component compounds in a model mixture and the extension of the NMR quantification method using different nuclei in combination:

[0072] In some cases, the relative concentration ratio of several compounds in the mixture has certain biological or physiological or pathological medical significance. For example, choline, phosphorylcholine, and glycerophosphorylcholine are considered to be the most important metabolites in human tumor tissues and cells. In vitro studies of tissue extracts have shown that these phosphoric acid derivatives can indicate the condition of certain diseases. Studies have shown that the relative ratio and concentration of these metabolites are related to the development of cancer, such as breast cancer. However, in the one-dimensional hydrogen spectrum, their NMR signals overlap with each other, so it is difficult to accurately determine the concentration or relative proportion ...

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Abstract

The invention provides a method for measuring contents of multiple mono compounds containing different elements in a complex mixture through a one-dimensional nuclear magnetic resonance mixture jointly utilizing different nucleuses, and the application of the method. Even if characteristic signal peaks of various compounds in a mixture in a one-dimensional nuclear magnetic resonance graph of a certain specific nucleus are overlapped, the method can also rapidly and accurately measure absolute concentrations of multiple mono compounds in the mixture. One key factor of the method is taking a compound comprising one or more elements to serve as a universal quantitative internal stand of a nuclear magnetic graph of different nucleuses, and the internal standard plays a role of quantitative bridge in a one-dimensional nuclear magnetic resonance graph of different nucleuses. If the relative concentration ratio of certain compounds is only concerned, the result of the relative concentration ratio measured by the method is not related to the concentration of the internal standard, and is not influenced by weighing error.

Description

technical field [0001] The invention belongs to the field of analytical chemistry methods, in particular to a method for determining the content of various compounds in a mixture using nuclear magnetic resonance technology, more specifically, to a one-dimensional nuclear magnetic resonance method using different nuclei to determine the content of different elements in a mixture method for the content of multiple compounds. Background technique [0002] Nuclear Magnetic Resonance (NMR) has become an essential tool in chemical structure studies because it can provide the most detailed, true and reliable information on chemical structures. In addition to qualitative analysis, NMR is also commonly used in quantitative analysis, because it has many unique advantages: such as no need to destroy the structure of the compound, simple experiment, and the integrated area of ​​the signal is directly proportional to the number of spin nuclei, etc. [0003] Previously, there have been r...

Claims

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Application Information

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IPC IPC(8): G01N24/08
Inventor 胡凯锋徐莉施孝活
Owner KUNMING INST OF BOTANY - CHINESE ACAD OF SCI
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