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Method for separating and detecting rifampicin and related impurities in rifampicin for injection

A technology for rifampicin and injection, which is applied in the field of analytical chemistry, can solve the problems that cannot be separated at the same time, and cannot be used for the separation and detection of 14 kinds of impurities and rifampicin at the same time, so as to achieve precise quality control, improve efficiency and accurate detection results. Effect

Active Publication Date: 2022-01-14
CHONGQING HUAPONT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no related substance detection item for rifampicin for injection in USP42, and the chromatographic conditions for related substances under rifampicin raw materials in USP / EP / JP are basically the same, using octylsilane bonded silica gel column, the main fluid components are acetonitrile and phosphoric acid Potassium dihydrogen buffer, citric acid and perchloric acid cannot separate the above 14 impurities and rifampicin at the same time
It shows that none of the methods disclosed in the prior art can be applied to the separation and detection of the above-mentioned 14 kinds of impurities and rifampicin at the same time

Method used

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  • Method for separating and detecting rifampicin and related impurities in rifampicin for injection
  • Method for separating and detecting rifampicin and related impurities in rifampicin for injection
  • Method for separating and detecting rifampicin and related impurities in rifampicin for injection

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] Chromatographic conditions:

[0069] Use octylsilane bonded silica gel as filler (Agilent ZORBAX Eclipse XDB-C8 4.6mm×250mm, 5μm), and buffer saline solution (take 8.67g of potassium dihydrogen phosphate and 30g of citric acid monohydrate, add water to dissolve and dilute to 1000ml)-methanol-acetonitrile (46:29:25) as mobile phase A, using glacial acetic acid methanol solution (take 5ml of glacial acetic acid, add methanol 1000ml, shake well) as mobile phase B, and perform linear gradient elution in the following table. The detection wavelength is 254nm, the flow rate is 1.4ml per minute, and the column temperature is 30°C.

[0070] Gradient elution program:

[0071]

Embodiment 2

[0073] Reagent preparation:

[0074] Blank solution: acetonitrile-water (1:1)

[0075] System Suitability Solution 1: Take an appropriate amount of impurity D, impurity I and rifampin reference substance, add a small amount of acetonitrile to dissolve, then quantitatively dilute with acetonitrile-water (1:1) to make a mixed solution containing about 40 μg per 1ml , as System Suitability Solution 1.

[0076] System Suitability Solution 2: Take an appropriate amount of impurity B, impurity C, impurity D, impurity E, impurity F, impurity G, impurity H, impurity I, impurity J, impurity K, impurity L and rifampicin, add a small amount of acetonitrile to dissolve , and then quantitatively diluted with acetonitrile-water (1:1) to prepare a mixed solution containing rifampicin 1mg / ml, as system suitability solution 2.

[0077] Sensitivity solution: Accurately weigh an appropriate amount of rifampicin reference substance, add a small amount of acetonitrile (about 10mg plus 1ml aceton...

Embodiment 3

[0081] Detection:

[0082] Take 10 μl of the blank solution and inject it into the liquid chromatograph, and record the chromatogram (see attached figure 1 ).

[0083] Take 10 μl each of system suitability solutions 1 and 2, inject them into the liquid chromatograph, and record the chromatograms. The separation degree of impurity D and impurity A (the impurity produced by impurity D and impurity I in this solution) meets the requirements (see attached figure 2 , 3 ).

[0084] Get 10 μ l of the sensitivity solution and inject it into the liquid chromatograph, record the chromatogram, the signal-to-noise ratio of the main component chromatographic peak height should be greater than 10 (see attached Figure 4 ).

[0085] Accurately measure 10 μl each of the test solution and the reference solution, inject them into the liquid chromatograph respectively, and record the chromatogram. If there are impurity peaks in the chromatogram of the test solution, except for the solvent p...

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Abstract

The invention belongs to the field of analytical chemistry, and particularly relates to a method for separating and detecting rifampicin and related impurities in rifampicin for injection. A chromatographic column adopted by the method takes octyl silane bonded silica gel as a filler, a buffer salt solution, acetonitrile, methanol and an acidic organic solution are adopted as mobile phases for gradient elution, and rifampicin and related impurities are separated and then detected. The detection wavelength is 255+ / -5nm, the flow velocity is 1.0-1.5ml per minute, and the column temperature is 30+ / -3DEG C. The invention provides a method for separating and determining rifampicin and related substances in rifampicin for injection by high performance liquid chromatography, the method is applicable to both the related substances and the rifampicin, one or more related substances in the rifampicin can be separated and detected at the same time, and compared with the prior art, the method has the advantage that the separation and detection efficiency is improved.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for separating and detecting rifampicin for injection and its related impurities by HPLC. Background technique [0002] Rifampicin is a broad-spectrum antibiotic, which has inhibitory effects on Mycobacterium tuberculosis, Gram-positive bacteria, Gram-negative bacteria, Leprae bacillus and trachoma virus. Clinically, it is often used in combination with other anti-tuberculosis drugs as the first-line drug for the treatment of various tuberculosis, and is also used to treat infections caused by bacteria resistant to other antibiotics. Clinically, there are oral administration and injection administration, among which rifampicin for injection has a remarkable effect and quick clinical effect. Rifampicin, the chemical name is 3-[[(4-methyl-1-piperazinyl)imino]methyl]rifamycin. Molecular formula is C 43 h 58 N 4 o 12 , the chemical structural formula is:...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/8675G01N2030/047G01N2030/065Y02A50/30
Inventor 谭辉兰昌云刘阔颜波张崇洋杨逸
Owner CHONGQING HUAPONT PHARMA
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