Detection method of qualitative analysis of case drugs by utilizing micro-nuclear magnetic resonance spectrometer

A technology of nuclear magnetic resonance spectroscopy and detection method, which is applied in analysis by nuclear magnetic resonance, material analysis by resonance, preparation of samples for testing, etc. Low cost and small footprint

Active Publication Date: 2017-05-24
GUANGXI UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a detection method for the qualitative analysis of case drugs by a miniature nuclear magnetic resonance spectrometer, so as to overcome the shortcom...

Method used

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  • Detection method of qualitative analysis of case drugs by utilizing micro-nuclear magnetic resonance spectrometer
  • Detection method of qualitative analysis of case drugs by utilizing micro-nuclear magnetic resonance spectrometer
  • Detection method of qualitative analysis of case drugs by utilizing micro-nuclear magnetic resonance spectrometer

Examples

Experimental program
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Effect test

Embodiment 1

[0030] 600MHz nuclear magnetic resonance spectrometer to detect two drug standard samples

[0031] Weigh 10mg codeine and N,N-dimethylamphetamine standard samples respectively, put them in 2ml glass bottles, add 0.5mL deuterated water (containing 0.05% TMSP), transfer the standard samples to 5mm NMR tubes after complete dissolution . Put the 5mm nuclear magnetic tube containing the standard sample solution into the autosampler of the bruker 600MHz nuclear magnetic resonance spectrometer to carry out the hydrogen spectrum experiment, and the 600MHz hydrogen spectrum of the two drugs was obtained after the experiment. With reference to the chemical shift (0ppm) of internal standard TMSP, mark the 600MHz hydrogen spectrum chemical shift of these two kinds of drugs, obtain the 600MHz nuclear magnetic resonance spectrometer standard hydrogen spectrum of codeine and N,N-dimethylamphetamine, as figure 2 shown.

[0032] Depend on figure 2 It can be seen that the characteristic pe...

Embodiment 2

[0034] 80MHz miniature nuclear magnetic resonance spectrometer to detect three drug standard samples

[0035] Weigh 50mg of morphine, 80mg of codeine and 50mg of N,N-dimethylamphetamine into three different 2ml glass bottles, add 1ml of deionized water, and dissolve them by ultrasonic. Use a 1ml syringe to draw the drug solution through a 0.45μm filter membrane and place it in a new 2ml glass bottle, then use a 1ml syringe to draw the filtrate and inject it into a picospin 80 miniature nuclear magnetic resonance spectrometer with an experimental temperature of 35°C, and select the onepulse mode for one-dimensional Hydrogen spectrum experiment, get 80MHz hydrogen spectrum of morphine, codeine and N,N-dimethylamphetamine, adjust the water peak chemical shift (4.79ppm) of morphine, codeine and N,N- The chemical shifts of the 80MHz hydrogen spectrum of dimethylamphetamine, while adjusting the baseline and characteristic peaks of the 80MHz hydrogen spectrum of morphine, codeine and...

Embodiment 3

[0041] With reference to the chemical shift (0ppm) of the internal standard TMSP in deuterated water, the 600MHz nuclear magnetic resonance spectrometer standard proton spectrum database of common drugs is established, as follows:

[0042] Weigh 10 mg of morphine (MP), O 3 - Monoacetylmorphine (O3M), O 6 - Monoacetylmorphine (O6M), codeine (CD), acetylcodeine (ACD), heroin (HR), papaverine (PA), cocaine (CA), amphetamine (AM), methamphetamine (MAM) , N,N-dimethylamphetamine (DAM), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA) and ketamine, chemical structures such as figure 1 As shown, put in a 2ml glass bottle, add 0.5ml deuterated water (containing 0.05% TMSP), and transfer the drug standard sample to a 5mm glass NMR tube after completely dissolving, put the 5mm NMR tube containing the drug standard sample into the bruker One-dimensional and two-dimensional spectrogram experiments were performed in the autosampler of the 600MHz NMR spectrome...

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Abstract

The invention relates to a detection method of qualitative analysis of case drugs by utilizing a micro-nuclear magnetic resonance spectrometer. The detection method comprises the following steps of: establishing a standard hydrogen spectrum database of a 600MHz nuclear magnetic resonance spectrometer of common drugs; detecting case drugs by utilizing a 80MHz micro-nuclear magnetic resonance spectrometer to obtain a 80MHz experimental hydrogen spectrum; adjusting the chemical shift, the baseline and the characteristic peak of the 80MHz experimental hydrogen spectrum to an appropriate ratio to obtain a 80MHz treatment hydrogen spectrum of the case drugs; and referring to the chemical shift of a standard drug hydrogen spectrum of the 600MHz nuclear magnetic resonance spectrometer to analyze the 80MHz treatment hydrogen spectrum to obtain components of the case drugs and other detection results. The common drugs can be identified in the hydrogen spectrum by the characteristic peaks of a benzene ring and a methyl group, and the experimental results of drug component detection are consistent with those of the conventional method. The method provided by the invention has the advantages of simple operation, low cost, small occupied space and the like, and meanwhile, the matter structure can be analyzed and the novel drugs can be detected according to the hydrogen spectrum.

Description

technical field [0001] The invention relates to a detection method for qualitatively analyzing case drugs with a miniature nuclear magnetic resonance spectrometer. In particular, it relates to a qualitative analysis method for drugs using a miniature nuclear magnetic resonance spectrometer. Background technique [0002] Drugs are dangerous substances that are harmful to the human body. With the improvement of material conditions, drug crimes have become one of the most serious crimes in today's society. At present, the commonly used methods for drug detection mainly include: gas chromatography, gas chromatography-mass spectrometry, liquid chromatography, liquid chromatography-mass spectrometry, and enzyme-linked immunoassay. These methods are characterized by high sensitivity and quantitative accuracy. However, these methods mainly detect drugs through standard substances or known databases in instruments, and cannot detect newly synthesized unknown drugs. At the same tim...

Claims

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Application Information

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IPC IPC(8): G01N24/08G01N1/28G01N1/34G01N1/14
CPCG01N1/14G01N1/28G01N1/34G01N24/084G01N2001/1463
Inventor 罗轩钟永红黄克建刘晓锋杨宁罗秋莲林翠梧
Owner GUANGXI UNIV
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