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Method for quantitatively analyzing content of daminozide through nuclear magnetic resonance hydrogen spectrum

It is a technology of hydrogen nuclear magnetic resonance spectroscopy and quantitative analysis, which is applied in the analysis by nuclear magnetic resonance, material analysis by resonance, and material analysis. The effect of saving test efficiency

Inactive Publication Date: 2022-06-28
HUAIYIN TEACHERS COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods all have the problems of cumbersome operation steps and low analysis efficiency.

Method used

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  • Method for quantitatively analyzing content of daminozide through nuclear magnetic resonance hydrogen spectrum
  • Method for quantitatively analyzing content of daminozide through nuclear magnetic resonance hydrogen spectrum
  • Method for quantitatively analyzing content of daminozide through nuclear magnetic resonance hydrogen spectrum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Butyryzide residues in peanuts were analyzed by 1H NMR spectroscopy. The specific steps are as follows:

[0040] Accurately weigh about 1.0 g (accurate to 0.0001 g) of the crushed and mixed sample into a 10 ml centrifuge tube, add 6 ml of heavy water, shake for 30 minutes and then centrifuge for 15 minutes (3000 r / min). Pipette 0.6ml of the supernatant into a 0.5mm nuclear magnetic tube for on-machine testing, and test and calculate the content of butyryl hydrazide according to the steps in the technical solution

[0041] Table 1 Test of butyryzide residues in peanuts

[0042]

Embodiment 2

[0044] The purity of the butyryzide raw material was analyzed by hydrogen nuclear magnetic resonance spectroscopy, and the specific steps were as follows:

[0045]Weigh 50mg of butyryzide API, transfer it into a 2mL disposable PE centrifuge tube, add 1.5mL of standard solution, ultrasonicate for 5min, the solution is clear and transparent, add 0.6mL to the NMR tube, and test on the machine. Calculate the actual content of butyric hydrazide according to the following formula, and calculate the purity of the raw material according to the actual content of butyric hydrazide.

[0046]

[0047] Table 2 butyryzide raw material drug purity analysis

[0048]

[0049]

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Abstract

The method comprises the following steps: obtaining a sample to be detected with a target component of butyrohydrazide to be detected, adopting maleic acid as an internal standard, dissolving the maleic acid and the sample to be detected in deuterated water D2O to obtain a solution to be detected, optimizing test parameters of a wavelength dispersive spectrometer for nuclear magnetic resonance analysis, and determining the content of the butyrohydrazide in the wavelength dispersive spectrometer according to the content of the butyrohydrazide in the wavelength dispersive spectrometer. The method comprises the following steps: measuring the nuclear magnetic resonance hydrogen spectrum of a to-be-measured solution to obtain the quantitative peaks of maleic acid and butyrohydrazide, respectively integrating the quantitative peaks of maleic acid and butyrohydrazide to obtain integral areas S maleic acid and S butyrohydrazide, and calculating the content of butyrohydrazide in the to-be-measured sample according to a formula. According to the method, a derivatization step is not needed, and complicated purification processes such as extraction and filtration are not needed, so that the test process can be greatly simplified, a new thought can be provided for determining the compounds by a quantitative nuclear magnetic resonance technology, and the application range of the quantitative nuclear magnetic resonance technology is expanded.

Description

technical field [0001] The invention relates to the technical field of food safety detection, and more particularly to a method for quantitatively analyzing the content of butyryl hydrazide by hydrogen nuclear magnetic resonance spectroscopy. Background technique [0002] Butyrazide is a succinic plant growth regulator that preserves chlorophyll in plants and prolongs the life of some perishable vegetables. However, studies have shown that butyrate hydrazide has a clear carcinogenic effect, so postharvest use has been restricted in the United States. It is a pity that Chinese consumers have not been able to identify which fruits use butyrhydrazide for freshness. Therefore, it is of great practical significance to develop a method for quantitative analysis of butyryl hydrazide. [0003] At present, the detection methods of butyrate hydrazide reported abroad mainly include thin-layer chromatography, gas chromatography, colorimetry, and chromatography-mass spectrometry, while...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N24/08
CPCG01N24/082
Inventor 胡正松卢明祝安礼涛阚玉和
Owner HUAIYIN TEACHERS COLLEGE
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