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Method for heteronuclear quantitative determination using nmr-spectroscopy, reference substances therefor, and method for determining the degree of deuteration of a deuterated compound

A technology for quantitative determination of compounds, applied in the direction of measurement using nuclear magnetic resonance spectrum, magnetic resonance measurement, and measurement using magnetic variables, which can solve the problems of large measurement uncertainty, inability to obtain, failure, etc.

Active Publication Date: 2020-11-20
BRUKER BIOSPIN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this job fails due to the volume change
Even with the PULCON (Pulse Length Based Concentration Determination) method, no more precise results can be obtained than the standard deviation of the mean volume of the NMR tubes in question allows
The second problem is that each NMR tube must be individually tuned for sensitivity, so called "tuned and matched"
Volume changes and matching cause large measurement uncertainties

Method used

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  • Method for heteronuclear quantitative determination using nmr-spectroscopy, reference substances therefor, and method for determining the degree of deuteration of a deuterated compound
  • Method for heteronuclear quantitative determination using nmr-spectroscopy, reference substances therefor, and method for determining the degree of deuteration of a deuterated compound
  • Method for heteronuclear quantitative determination using nmr-spectroscopy, reference substances therefor, and method for determining the degree of deuteration of a deuterated compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0133] The determination of sodium in embodiment 1-heparin sodium

[0134] In the following, the determination of sodium in heparin sodium is provided as an example of the method of the present invention, heterokaryon quantitation.

[0135] For this purpose, the sodium content of 16 different sodium-heparin solution samples (S1-S16) was determined by the method according to the present invention (NMR) and compared with the method commonly used for this purpose by atomic absorption spectroscopy (AAS). The obtained values ​​are compared.

[0136] To prepare samples, weigh a defined amount of Na-heparin and dissolve in a defined volume of D 2 O middle. Alternatively, a defined amount of the appropriate deuterated solvent can also be weighed. As deuterated solvent, DMSO-d 6 can be used as D 2 Alternatives to O.

[0137] In particular, the determination of sodium by NMR according to the present invention is required in the European and US Pharmacopoeias 1 Additional experime...

Embodiment 2

[0147] The mensuration of embodiment 2-NMR solvent deuteration degree

[0148] Suitable solvents for NMR experiments must contain very high levels of deuterium 2 H, instead of the naturally more abundant hydrogen atoms 1 H. For conventional NMR experiments, a specification of "very high" is sufficient, i.e. >99%D. The remaining 1% is 1 H.

[0149] Knowing this degree of deuteration is important for the heteronuclear quantitative NMR method according to the present invention. In the case of solvents with a very high degree of deuteration, e.g. >99.95% deuterated D 2 O, 0.05% 1 The ratio of H is unimportant and only contributes to the uncertainty of the assay. To accurately determine the degree of deuteration, NMR spectroscopy is a natural fit, as it can be used to measure 2 H(D) and 1 Hboth. The integral ratio D / H is directly proportional to the degree of deuteration. The necessary calibration is done by adding the same non-deuterated solvent and making the appropria...

Embodiment 3

[0159] Example 3 - Determination of deuterated NMR solvents with other deuterated solvents whose deuterated degree is known

[0160] In this example 3, deuterated CDCl was measured 3 degree of deuteration. For this, deuterated CDCl was prepared in a mixing ratio of about 1:1 3 and DMSO-d for Example 2 6 (Deuterated degree 99.57%) mixture. Since the mixing ratio does not need to be known exactly, it can be weight-related or volume-related. Other mixing ratios can also be used as long as meaningful NMR spectra can be obtained. Measure the resulting mixture of 2 H and 1 H NMR (one single pulse each).

[0161] Figure 7 The prepared CDCl is shown on the left 3 and DMSO-d 6 mixture 1 H NMR spectra and the corresponding 2 H NMR Spectrum.

[0162] Will come from DMSO-d 6 The integral ratio D / H of the spectrum is the same as that from CDCl 3 Integral ratio D / H comparison of the spectra, taking into account the known degree of protonation (DMSO-d 6 {H} DMSO ), calcul...

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Abstract

Disclosed is a method for the quantitative determination of an analyte in a test sample using an NMR spectrometer, the deuterated solvent that is used to dissolve the analyte being used as an internalstandard. Also disclosed are specific reference substances for use in the method according to the invention. Also described is a method for determining the degree of deuteration of a deuterated compound.

Description

technical field [0001] The present invention relates to a method for the quantitative determination of an analyte in a test product using an NMR spectrometer, wherein a deuterated solvent for dissolving the analyte is used as an internal standard, a reference substance for the method of the present invention, and a A method for determining the degree of deuteration of a deuterated compound. Background technique [0002] Nuclear magnetic resonance spectroscopy, hereinafter also referred to as NMR spectroscopy, is one of the basic methods for structural elucidation of organic compounds. It is based on the fact that the atomic nuclei of bulk elements have a non-zero nuclear spin and that the resulting angular momentum upon application of an external magnetic field allows statements to be made about the chemical environment of said atoms. [0003] Atoms with nuclear spin zero (I=0), such as 12 C or 16 O, not detectable by NMR spectroscopy. In contrast, all atoms with non-zer...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01R33/46
CPCG01N24/082G01N1/28G01N2001/2893G01R33/46G01R33/4625G01R35/005
Inventor 贝恩德·维利·卡罗-汉斯·迪尔
Owner BRUKER BIOSPIN
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