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A method for detecting a target substance by nuclear magnetic resonance

A target substance, nuclear magnetic resonance technology, which can be used in magnetic resonance measurement, measurement using nuclear magnetic resonance spectrum, and analysis using nuclear magnetic resonance, etc., and can solve problems such as impossible and quantitative difficulties.

Inactive Publication Date: 2010-06-09
F HOFFMANN LA ROCHE & CO AG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] A problem in many analytical applications of NMR spectroscopy is that the NMR signal of a substance of interest may overlap with that of other substances, making quantitation difficult or even impossible
Thus, the known signal shifting methods have the disadvantage that the intended shifting signal may be very close to at least one other signal from which it should be distinguished

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  • A method for detecting a target substance by nuclear magnetic resonance
  • A method for detecting a target substance by nuclear magnetic resonance
  • A method for detecting a target substance by nuclear magnetic resonance

Examples

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Embodiment 1

[0044] An overview of the different spin system topologies that can be used to identify and quantify known target species in dense NMR spectra is shown in figure 1 and figure 2 middle. In these examples, the detected spins (integer or half-integer, such as spin 1 / 2) are shown in bold in the following structural formulas 1 H or spin 1 2 H) leads to an NMR singlet in the case of the target substance. By changing the sample conditions (pH, salt, T), the signal of interest can be shifted to non-overlapping spectral regions. However, it is not always straightforward to identify shifted lines. In an isotopically labeled target substance, the same spin interacts with the isotopic nucleus substituted therein. This interaction can be used to identify the signal of interest and quantify the amount of the unlabeled counterpart molecule of the same type.

[0045] Particularly, figure 1 The case where the isotopes are labeled as spin 1 / 2 nuclei is shown. Starting with an unlabeled...

Embodiment 2

[0066] The assay described above was used to detect glycine in cerebrospinal fluid (CSF) collected from the cisterna magna of adult Wistar male rats (under anesthesia with 3-5% gaseous isoflurane). Immediately after collection, CSF was stored at -80°C. Mix an appropriate aliquot of CSF with 6 μL of 8.5N NaOD, 10 μL of 1 mM 13 C-glycine (both carbon atoms are used 13 C mark) and 20% D 2 A solution of O in 80% water was mixed to give a total volume of 200 μL. After vortexing for 30 seconds, the solution was centrifuged at 13000 rpm for 1 minute and the supernatant was transferred to a 3 mm NMR tube. Samples were freshly prepared prior to measurement.

[0067] Equipped with a 5mm cryoprobe (CryoProbe) and used XWINNMR 3.5 (Bruker BioSpin, The measurement of CSF on the Bruker Avance-II 600MHz instrument controlled by Switzerland) 1 H NMR spectrum. Each sample was manually tuned and matched, and shimmed with the manufacturer's gradient shimming program. 32k data points wer...

Embodiment 3

[0074] Figure 4 A schematic diagram of the quantification strategy applied to two-dimensional NMR spectroscopy is shown in . Depending on the sample conditions, the target compound to be quantified has a signal with a chemical shift of 3.7-3.8 ppm. One-dimensional obtained on biological matrices 1 H NMR spectrum ( image 3 , left panel) exhibit severe signal overlap. Applying two-dimensional TOCSY spectroscopy (cf. A. Bax and D. G. Davis (1985), J. Magn. Reson. 65, 355), the situation is improved by isolating off-diagonal signals of known spin system topology , but the two triplet signals marked by small boxes are still unclear ( image 3 , middle panel). only in 13 After the peak formation of the C-labeled substance ( image 3 , right panel), the triplet of interest was clearly identified as the lower one, which is now clearly a doublet as a triplet. by right image 3 Integrating the NMR triplet signal in the extracted line shown in the small box on the right, the r...

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Abstract

A method for detecting a known target substance in a sample by means of nuclear magnetic resonance (NMR) of a preselected nuclear species contained in the target substance is described. The method comprises the steps of: a) providing a starting sample known or suspected to contain the target substance; b) adding to the starting sample an amount of isotope-labeled target substance, thus obtaining a composite sample, the isotope-labeled target substance being obtainable from the target substance by replacing at least one nucleus thereof by another isotope thereof, wherein said replacing induces a change in the position or multiplicity of at least one NMR signal of the target substance; c) acquiring NMR signals of the preselected nuclear species from the composite sample; d) determining actual positions of an auxiliary set of NMR signals of the isotope-labeled target substance; e) calculating actual positions of a principal set of NMR signals of the target substance from the actual positions of the auxiliary set of signals and from a predetermined relationship between relative positions of the signals of the isotope-labeled target substance and of the signals of the target substance; f) detecting at least one signal of the target substance located at an actual position calculated by step e).

Description

[0001] invention technical field [0002] The invention relates to a method for detecting a target substance in a sample by nuclear magnetic resonance. Background technique [0003] NMR spectroscopy is a well-known and widely used technique for the qualitative and quantitative analysis of a wide variety of samples. This technique usually involves performing a test on a preselected nuclear isotope with non-zero spin angular momentum (e.g. 1 H. 13 C or many other isotopes) under selective conditions to record nuclear magnetic resonance spectra, hereinafter referred to as NMR spectra. Typically, NMR spectra obtained from samples containing molecular species contain multiple signal peaks originating from nuclei of preselected isotopes. Each signal peak corresponds to a specific resonance frequency attributable to one or several nuclei experiencing a specific local magnetic field as a result of a specific molecular environment. Thus, it is observed that the resonant frequency o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N24/08G01R33/46G01R33/465
CPCG01N24/08G01R33/465G01R33/4625G01R33/46G01R33/485Y10T436/24
Inventor 格茨·施洛特贝克阿尔弗雷德·罗什汉斯·森
Owner F HOFFMANN LA ROCHE & CO AG
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