Method for separating and determining 3-amino-4-imino rifamycin S and related impurities

A technology for rifamycin and related impurities, which is applied in the field of analytical chemistry, can solve the problem that the determination method of 3-amino-4-imino-rifamycin has not been queried, and achieves an effective method, simple operation and short analysis time. Effect

Pending Publication Date: 2021-06-11
CHONGQING HUABANGSHENGKAI PHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the United States Pharmacopoeia USP version, European Pharmacopoeia EP, and Chinese Pharmacopoeia have not found a method for the determination of related substances of 3-amino4-iminorifamycin S

Method used

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  • Method for separating and determining 3-amino-4-imino rifamycin S and related impurities
  • Method for separating and determining 3-amino-4-imino rifamycin S and related impurities
  • Method for separating and determining 3-amino-4-imino rifamycin S and related impurities

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] Supplies and methods

[0075] 3-amino-4-iminorifamycin S standard, 3-aminorifamycin S, and rifamycin S standard were all obtained from commercial channels. The sources of 3-amino-4-iminorifamycin S for testing and 3-bromorifamycin S, impurity A, impurity B, impurity C, and impurity D are from Chongqing Hua Bangshengkai Pharmaceutical Co., Ltd.

[0076] The test instruments used are Shimadzu high performance liquid chromatography (UV detector)

[0077] The chromatographic column is ZORBAX Eclipse XDB-C18, 4.6×250mm, 5-Micron; the column temperature is 30°C; the injection volume is 15μl; the flow rate is 1.0ml / min; the sample concentration is 0.4mg / ml.

[0078] Mobile phase A: the volume ratio of acetonitrile and methanol is 900:100;

[0079] Mobile phase B: a mixed solution of ammonium dihydrogen phosphate buffer and acetonitrile, the volume ratio is 800:200, the concentration of ammonium dihydrogen phosphate solution is 0.1mol / L, and the pH value is 6-8.5.

[0080] ...

Embodiment 2

[0092] The buffer salt used is sodium dihydrogen phosphate aqueous solution, pH is 6.0, gradient elution, the results are shown in the appendix figure 1 .

Embodiment 3

[0094] The buffer salt used is potassium dihydrogen phosphate aqueous solution, the pH is 6.0, and the results of gradient elution are shown in the appendix figure 2 .

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Abstract

The invention belongs to the field of analytical chemistry, and particularly relates to a method for separating and determining 3-amino-4-imino rifamycin S and related impurities. A chromatographic column adopted in the method takes octadecylsilane chemically bonded silica as a filler, a mobile phase A and a mobile phase B are adopted for gradient elution, and a detector is entered for detection; the related impurities comprise one or more of 3-amino rifamycin S, 3-bromo rifamycin S, rifamycin S, an impurity A, an impurity B, an impurity C and an impurity D; the mobile phase A is acetonitrile and methanol; and the mobile phase B is a phosphate buffer solution. According to the method disclosed by the invention, the 3-amino rifamycin S, the 3-bromo rifamycin S, the rifamycin S, the impurity A, the impurity B, the impurity C and the impurity D can be simultaneously separated and determined; and the quality of the 3-amino-4-imino rifamycin S bulk drug can be accurately controlled, and the safety and effectiveness of the product are finally ensured.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for separating and measuring raw material drug rifabutin intermediate 3-amino-4-iminorifamycin S and related substances. Background technique [0002] 3-Amino-4-imino rifamycin S has high antibacterial activity and is an important intermediate in the synthesis of many rifamycin derivatives (such as rifabutin). At present, the main synthesis method is to synthesize 3-halogenated rifamycin S or SV through halogenation reaction, nitration reaction, reduction reaction, oxidation reaction and ammoniation reaction. During this series of reactions, various compounds will be produced, and finally some of them will remain in the 3-amino-4-iminorifamycin S as impurities. Therefore, the quality of 3-amino4iminorifamycin S is a key factor for the quality assurance of rifabutin. [0003] In drug analysis, the so-called "related substances" refer to substances that ar...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/74
CPCG01N30/02G01N30/06G01N30/34G01N30/74G01N2030/047
Inventor 李小成谭涛莫彬唐朝君
Owner CHONGQING HUABANGSHENGKAI PHARM
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