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Terahertz spectroscopy detection method for thiobarbituric acid polymorphism

A thiobarbituric acid and spectral detection technology, which is used in measurement devices, phase influence characteristic measurement, preparation of samples for testing, etc. Simple measurement method and non-destructive effect of detection technology

Inactive Publication Date: 2017-08-22
CHINA JILIANG UNIV
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Problems solved by technology

The current detection methods mainly include single crystal X-ray diffraction and solid-state nuclear magnetic resonance spectroscopy. However, the two detection methods have the disadvantages of cumbersome sample preparation, complex analysis, and high photon energy that may lead to crystal transformation. Therefore, it is necessary to explore a fast and nondestructive method The detection method is critical

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  • Terahertz spectroscopy detection method for thiobarbituric acid polymorphism
  • Terahertz spectroscopy detection method for thiobarbituric acid polymorphism
  • Terahertz spectroscopy detection method for thiobarbituric acid polymorphism

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Embodiment 1

[0036] This embodiment provides a terahertz spectroscopic detection method for polymorphs of thiobarbituric acid, comprising the following steps:

[0037] Sample preparation steps:

[0038] Preparation of crystal form II (sample 2): take thiobarbituric acid raw material and dissolve it in absolute ethanol, and naturally evaporate at room temperature to obtain a light yellow solid;

[0039] Specifically, take the thiobarbituric acid raw material and dissolve it in dehydrated ethanol at a temperature of 50°C. During the dissolution process, stir fully for about 20 minutes until it is completely dissolved, then place it at room temperature, and cool it naturally. After 15 days, it crystallized to form light yellow solid crystal form II.

[0040] Preparation of crystal form III (sample 3): Dissolve thiobarbituric acid raw material in absolute ethanol, dry in air, and evaporate naturally to obtain a yellow solid;

[0041] Specifically, take the thiobarbituric acid raw material an...

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Abstract

The invention provides a terahertz spectroscopy detection method for thiobarbituric acid polymorphism and aims at solving the problems of complicated sample preparation and analysis as well as polymorphic transformation caused by high photon energy in an existing detection method. The thiobarbituric acid polymorphism is prepared by using a solvent recrystallization method, and is measured by using a terahertz time-domain spectroscopy to obtain optical parameters of the thiobarbituric acid polymorphism on a terahertz wave. The method for measuring a sample by using terahertz time-domain spectroscopy is simple, fast and lossless.

Description

technical field [0001] The invention belongs to the fields of medicinal chemistry and spectral analysis. In particular, it relates to a terahertz spectroscopic detection method for polymorphic forms of thiobarbituric acid Background technique [0002] Thiobarbituric acid, as a central nervous system depressant, can be used for sedation and hypnosis. Currently, thiobarbituric acid has 6 polymorphic forms and 1 hydrated crystal form. Previous studies have shown that the polymorphs of thiobarbituric acid can be prepared by solvent recrystallization and grinding. However, thiobarbituric acid itself has tautomeric transformation. When the grinding time and frequency change slightly, thiobarbituric acid is prone to crystal transformation. [0003] The premise of rational selection of drug crystal forms in medicine and clinical treatment is the detection and identification of drug active ingredients. The polymorphic form is more likely to change under other external conditions ...

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Application Information

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IPC IPC(8): G01N21/3586G01N21/41G01N1/40
CPCG01N1/4022G01N21/3586G01N21/41G01N2001/4027
Inventor 蔡强杜勇张琪刘建军
Owner CHINA JILIANG UNIV
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