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Method for detecting genotoxic impurities of 2-amino-5-nitrothiazole in nitazoxanide

A technology of nitrothiazole and nitazoxanide, applied in the field of analysis and detection, can solve the problems of no relevant reports and the like, and achieve the effects of good durability, strong specificity and high separation efficiency

Pending Publication Date: 2021-06-18
REYOUNG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

According to the relevant ICH guidelines, the genotoxic impurity limit is ≤1.5μg / Day, and there is no relevant report on the genotoxic impurity detection method so far

Method used

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  • Method for detecting genotoxic impurities of 2-amino-5-nitrothiazole in nitazoxanide
  • Method for detecting genotoxic impurities of 2-amino-5-nitrothiazole in nitazoxanide
  • Method for detecting genotoxic impurities of 2-amino-5-nitrothiazole in nitazoxanide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The high-performance liquid chromatography of the present invention is used to detect 2-amino-5-nitrothiazole genotoxic impurities in nitazoxanide, wherein the liquid phase conditions are as follows:

[0028] Chromatographic column: the size is 4.6mm×250mm, the filler is octadecyl bonded silica gel, and the average particle size of the filler particles is 5μm;

[0029] Column temperature: 35°C;

[0030] Mobile phase: a mixed solution of phosphoric acid aqueous solution (pH value 2.5) and acetonitrile in a volume ratio of 55:45;

[0031] Flow rate: 1.0ml / min;

[0032] Detection wavelength: 385nm.

[0033] The detection steps are as follows:

[0034] (1) With 2-amino-5-nitrothiazole as reference substance, acetonitrile is solvent, and preparation concentration is the 2-amino-5-nitrothiazole reference substance solution of 3ng / ml;

[0035] (2) Take 20 μl of blank solvent and 20 μl of 2-amino-5-nitrothiazole reference substance solution to detect by high-performance liq...

Embodiment 2

[0060] Embodiment 2: specificity test

[0061] Take each 10 μl of blank solvent, reference substance solution, and need testing solution and inject into the high-performance liquid chromatograph respectively, and record the chromatogram, such as Figure 4 As shown, the results show that the matrix in the blank solvent and the test product does not interfere with the determination of 2-amino-5-nitrothiazole, indicating that the specificity of the detection method of the present invention is good.

Embodiment 3

[0062] Embodiment 3: quantitative limit and detection limit test

[0063] Take an appropriate amount of 2-amino-5-nitrothiazole, add acetonitrile to dissolve and dilute to prepare a corresponding solution. Take 10 μl and inject into high performance liquid chromatography. The concentration of the solution when S / N ≈ 10 is used as the limit of quantification, the solution for the limit of quantification is diluted 2 to 3 times, and the concentration of the solution with S / N ≈ 3 is used as the limit of detection. At the same time, the precision of the limit of quantification was investigated.

[0064]The results showed that the detection limit concentration of 2-amino-5-nitrothiazole was 0.4ng / ml, and the quantification limit concentration was 1.2ng / ml.

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Abstract

The invention relates to the technical field of analysis and detection, in particular to a method for detecting genotoxic impurities of 2-amino-5-nitrothiazole in nitazoxanide. According to the method for detecting the genotoxic impurities of the 2-amino-5-nitrothiazole in the nitazoxanide, detection is carried out through a high performance liquid chromatography, 2-amino-5-nitrothiazole is used as a reference substance, acetonitrile is used as a diluent, and the content of the 2-amino-5-nitrothiazole in a sample is calculated through an external standard method, wherein a chromatographic column adopts octadecyl bonded silica gel as a filling agent, and a mobile phase adopts a mixed solution of a phosphoric acid aqueous solution and acetonitrile. According to the method for detecting the genotoxic impurities of the 2-amino-5-nitrothiazole in the nitazoxanide, the blank that the genotoxic impurities are analyzed through a high performance liquid chromatography method is filled, and compared with a traditional liquid chromatography method, the method is easy to operate, convenient, efficient, wide in application range and higher in sensitivity which can reach 0.6 ppm, and guarantees the safety of drugs.

Description

technical field [0001] The invention relates to the technical field of analysis and detection, in particular to a method for detecting 2-amino-5-nitrothiazole genotoxic impurities in nitazoxanide. Background technique [0002] Genotoxic impurities are a class of impurities that can react with DNA, cause DNA damage, induce gene mutations at very low levels, and may cause cancer. Because of its strong toxicity, it poses a strong threat to the safety of medication. In recent years, regulatory agencies in various countries such as ICH, FDA, and EMA have made clearer requirements for genotoxic impurities. More and more pharmaceutical companies are In the process of new drug research and development, focus on the control and detection of genotoxic impurities. [0003] The structural formula of 2-amino-5-nitrothiazole is as follows: [0004] [0005] The structure analysis is: 1H NMR (600MHz, DMSO-d6) δ8.80 (s, 2H), 8.26 (s, 1H); 13CNMR (150MHz, DMSO-d6) δ 173.87, 147.86, 135....

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 苗得足胡清文赵征尹诗杨书华刘德杰王向华
Owner REYOUNG PHARMA
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