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Method for separating and determining pasiniazide and related impurities thereof by HPLC method

A technology for pasoniazid and related substances, applied in the field of analytical chemistry, can solve problems such as control, and achieve the effects of ensuring quality controllable, precise quality controllability, and improving efficiency

Active Publication Date: 2018-03-20
CHONGQING HUAPONT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The national drug standard [WS-10001-(HD-0322)-2002] contains the quality standard of this product, but there is no control on related substances

Method used

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  • Method for separating and determining pasiniazide and related impurities thereof by HPLC method
  • Method for separating and determining pasiniazide and related impurities thereof by HPLC method
  • Method for separating and determining pasiniazide and related impurities thereof by HPLC method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Chromatographic conditions:

[0068] Chromatographic column: Shimadzu VP ODS 250×4.6mm, 5.0μm

[0069] Column flow rate: 1.0ml / min

[0070] Detection wavelength: UV 280nm

[0071] Column temperature: 30°C

[0072] Injection volume: 20μl

[0073] Solvent: buffer salt (disodium hydrogen phosphate 8.7g, sodium dihydrogen phosphate 3.4g, add water to dissolve and dilute to 1000ml)-methanol=90:10

[0074] Mobile phase: A: Phosphate buffer (8.7g disodium hydrogen phosphate, 3.4g sodium dihydrogen phosphate, 2.0g tetrabutylammonium hydrogen sulfate, add water to dissolve, and dilute to 1000ml)

[0075] B: Methanol

[0076] Gradient elution:

[0077]

[0078]

[0079] 1. Solution preparation

[0080] System suitability solution: take the appropriate amount of pasniazid reference substance, impurity A, impurity B, impurity C, impurity D, and impurity E, dissolve in methanol and dilute with a solvent to make about 1 mg of pasniazid and impurity per 1 ml 2ug mixed so...

Embodiment 2

[0087] Embodiment 2 comparative example

[0088] The national drug standard [WS-10001-(HD-0322)-2002] contains the quality standard of this product, and the relevant substances are not controlled;

[0089] According to the Chinese Pharmacopoeia 2015 edition persinazid related substance items only m-aminophenol (impurity B) is controlled, using isocratic elution, the mobile phase is: phosphate buffer (disodium hydrogen phosphate 8.7g, sodium dihydrogen phosphate 3.4g, add appropriate amount of water to dissolve, 10% tetrabutylammonium hydroxide solution 23ml, and dilute to 1000ml)-methanol=90:10. As a result, it was found that the main peak of impurity B and isoniazid could not be effectively separated under the conditions of this chromatographic system; the main peak of impurity D (a possible degradation impurity) coincided with the main peak of p-aminosalicylic acid and could not be effectively detected; the peak of impurity E appeared under isocratic elution conditions The ...

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Abstract

The invention belongs to the field of analytical chemistry and particularly relates to a method for separating and determining pasiniazide and related impurities thereof by an HPLC method. According to the method, an adopted chromatographic column takes octadecylsilane chemically bonded silica as filler, a mobile phase A and a mobile phase B are adopted to carry out gradient elution, and detectionis carried out in a detector; related substances comprise isoniazide, p-aminosalicylic acid and related impurities; the related impurities are one or more of A to E; the mobile phase A is a phosphatebuffer solution, and the mobile phase B is methanol. The method provided by the invention can be used for simultaneously separating and determining the isoniazide, the p-aminosalicylic acid and the related impurities A to E in the pasiniazide, and the efficiency of separation detection is increased compared with the prior art; the controllable quality of pasiniazide raw pharmaceutical materials and preparations thereof can be more accurately ensured, and the product can be safe and effective finally.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for separating and measuring pasniazid and its related impurities by HPLC. Background technique [0002] Palsoniazid is a prescription drug, a synthetic anti-tuberculosis drug, used to treat various types of pulmonary tuberculosis, endobronchial tuberculosis and extrapulmonary tuberculosis. It can also be used as a protective drug for tuberculosis-related operations, and can also be used to prevent tuberculosis infection and recurrence in long-term or high-dose corticosteroids and immunosuppressive therapy. [0003] The anti-tuberculosis component of pasniazid is mainly isoniazid, which is loosely combined with aminosalicylic acid and isoniazid. Theoretically, the ratio of aminosalicylic acid and isoniazid should be 1: 0.8957 (ratio of relative molecular mass). The p-aminosalicylic acid in the molecule can prevent the acetylation of isoniazid in the body...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 谭辉兰昌云颜波
Owner CHONGQING HUAPONT PHARMA
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