Additive for nuclear magnetic resonance spectrum and method for analyzing mixture by virtue of additive

A nuclear magnetic resonance spectrum and analysis method technology, applied in the field of NMR mixture analysis, can solve the problems of small number of compounds, increased solution viscosity, interference component signals, etc., and achieve good practical use value and good scientific research value.

Inactive Publication Date: 2014-12-24
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, foreign literature has reported the application of DOSY technology with polyvinylpyrrolidone and polyethylene glycol as additives. Their disadvantages are that the number of separated compounds is small, their own signals will interfere with component signals, and the solution viscosity increases.

Method used

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  • Additive for nuclear magnetic resonance spectrum and method for analyzing mixture by virtue of additive
  • Additive for nuclear magnetic resonance spectrum and method for analyzing mixture by virtue of additive
  • Additive for nuclear magnetic resonance spectrum and method for analyzing mixture by virtue of additive

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1.1 Reagents and instruments

[0026] Polydimethylsiloxane (viscosity: 100mPa.s, neat(25℃)) (PDMS), benzene, naphthalene and anthracene were purchased from China National Pharmaceutical Group Chemical Reagent Co., Ltd., the grade is analytical pure; deuterated chloroform (containing 0.003% TMS, v / v) was purchased from Cambridge Isotope Laboratories, USA, and the grade is NMR pure; nuclear magnet tube (WG-5mm-Economy-7) was purchased from Wilmad, USA; the spectrometer was Bruker AVANCE III 600M NMR spectrum The instrument has a resonance frequency of 600.13 Hz; the probe is a 5mm ultra-low temperature triple resonance trans-detection probe with a gradient of 53G / cm.

[0027] 1.2 NMR experiment

[0028] Add 8 mg of benzene, 8 mg of naphthalene, 8 mg of anthracene, and 0.6 ml of deuterated chloroform to the two nuclear magnetic tubes respectively, and then add 50 mg of PDMS to one of the nuclear magnetic tubes and shake them sufficiently to prepare two NMR samples for use.

[002...

Embodiment 2

[0033] 2.1 Reagents and instruments

[0034] PDMS (viscosity: 200mPa.s, neat(25℃)), 1,5-dibromopentane, 1-bromopentane and n-pentane were all purchased from China National Pharmaceutical Group Chemical Reagent Co., Ltd. The grade is analytical pure; deuterated Chloroform (containing 0.003% TMS, v / v) was purchased from Cambridge Isotope Laboratories, USA, and the grade is NMR pure; NMR tube (WG-5mm-Economy-7) was purchased from Wilmad, USA; Spectrometer was Bruker AVANCE III 600, Switzerland Mega NMR spectrometer, its resonance frequency is 600.13 Hz; the probe is a 5mm ultra-low temperature triple resonance trans-detection probe, and its gradient is 53G / cm.

[0035] 2.2 NMR experiment

[0036] Add 5 mg of 1,5-dibromopentane, 5 mg of 1-bromopentane, 5 mg of n-pentane and 0.6 ml of deuterated chloroform to the two NMR tubes, and then add 80 mg of PDMS to one of the NMR tubes , Fully shake, prepare two NMR samples for use.

[0037] Put the prepared NMR sample tube into the cavity of th...

Embodiment 3

[0041] 3.1 Reagents and instruments

[0042] Hydrogen-terminated polysiloxane (viscosity: 100mPa.s, neat (25℃)), acetic acid, ethanol and acetonitrile were purchased from China National Pharmaceutical Group Chemical Reagent Co., Ltd., the grade is analytically pure; deuterated chloroform (containing 0.003% TMS ,v / v) was purchased from Cambridge Isotope Laboratories, USA, and the grade is NMR pure; nuclear magnet tube (WG-5mm-Economy-7) was purchased from Wilmad, USA; the spectrometer was the Swiss Bruker AVANCE III 600M NMR spectrometer. The resonance frequency is 600.13 Hz; the probe is a 5mm ultra-low temperature triple resonance trans-detection probe with a gradient of 53G / cm.

[0043] 3.2 NMR experiment

[0044] Add 6 mg of acetic acid, 6 mg of ethanol, 6 mg of acetonitrile and 0.6 ml of deuterated chloroform to the two NMR tubes, and then add 60 mg of hydrogen-terminated polysiloxane to one of the NMR tubes, and shake them sufficiently to prepare two One NMR sample for use.

[...

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Abstract

The invention provides a polysiloxane-based nuclear magnetic resonance spectrum mixture analysis method, which comprises the following steps: employing polysiloxane as an additive, performing separation analysis on components in a liquid mixture in a liquid nuclear magnetic resonance spectroscope by utilizing two-dimensional diffusion-ordered spectroscopy technology, and performing baseline separation on a nuclear magnetic resonance signal of each component on a diffusion dimension to obtain the molecular structure information of each component according to different diffusion coefficients of the components. According to the method, the molecular structure of each component in the mixture can be conveniently, rapidly and qualitatively analyzed, a nuclear magnetic resonance experiment is environment-friendly and pollution-free, and the method has a high scientific research value and a high practical application value.

Description

Technical field [0001] The invention relates to an NMR mixture analysis method. Specifically, it is an additive used in nuclear magnetic resonance spectroscopy and a method for analyzing the mixture using it. Background technique [0002] NMR technology is one of the most powerful tools to characterize the structure of compounds. However, when faced with the analysis of mixtures, NMR technology often appears to be inadequate. The emergence of two-dimensional diffusion ordering spectroscopy (DOSY), which is called chromatographic technology in NMR, allows NMR to analyze mixtures with large differences in structure (a) Johnson, CS, Prog. Nucl. Magn. Reson. Spectrosc. 1999, 34, 203 .; b) Caldarelli, S., Magn. Reson. Chem. 2007, 45, S48.; c) Novoa-Carballal, R., Fernandez-Megia, E., Jimenez, C., Riguera, R., Nat. Prod.Rep.2011,28,78.]. The principle of DOSY technology is to separate the NMR signal of each component in the diffusion dimension according to the diffusion coefficient...

Claims

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Application Information

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IPC IPC(8): G01N24/08
Inventor 黄少华高峻李素英豆孝伟杨盈
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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