A kind of high performance liquid chromatography analysis method of dihydralazine sulfate related substances

A technology of dihydralazine sulfate and high performance liquid chromatography, which is applied in the field of ultra-high performance liquid chromatography analysis of related substances of dihydralazine sulfate and its tablets, can solve the problem that it is difficult to effectively control dihydralazine sulfate and its tablets. issues such as drug product quality and safety risks

Active Publication Date: 2021-02-02
CHANGZHOU PHARMA FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, a set of comprehensive, effective and stable analytical methods for the analysis of related substances of dihydralazine sulfate and its tablets has not been established. It is difficult to effectively control the product quality of dihydralazine sulfate and its tablets. potential risks

Method used

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  • A kind of high performance liquid chromatography analysis method of dihydralazine sulfate related substances
  • A kind of high performance liquid chromatography analysis method of dihydralazine sulfate related substances
  • A kind of high performance liquid chromatography analysis method of dihydralazine sulfate related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: detection instrument and chromatographic conditions:

[0029] High performance liquid chromatography: Waters UPLC AcQuity H-Class

[0030] Chromatographic column: the reverse phase C18 column is selected from Infinity Lab Poroshell 120 SB-C18, the specification is 4.6*150mm, 2.7Micron.

[0031] Mobile phase A: Take 2.0g of anhydrous potassium dihydrogen phosphate, add 1000ml of water to dissolve, adjust the pH to 1.8 with phosphoric acid;

[0032] Mobile phase B: Methanol;

[0033] Detection wavelength: 228nm;

[0034] Flow rate: 0.35ml / min

[0035] Column temperature: 5°C

[0036] Gradient elution program:

[0037] time (min) Mobile phase A(%) Mobile phase B(%) 0 98 2 17 60 40 23 0 100 25 98 2

[0038] Preparation of the reference solution: Take impurities A, B, C, D, E, F, about 5 mg each, in a 50ml volumetric flask, add diluent to dissolve and dilute to the mark, shake well, as the stock solution of the re...

Embodiment 2

[0048] Embodiment 2: detection instrument and chromatographic conditions:

[0049] Ultra-Performance Liquid Chromatography: Waters UPLC AcQuity H-Class

[0050]Chromatographic column: the reversed-phase C18 column is selected from Infinity Lab Poroshell 120 SB-C18, the specification is 4.6*150mm, 2.7Micron.

[0051] Mobile phase A: Take 2.0g of anhydrous potassium dihydrogen phosphate, add 1000ml of water to dissolve, and adjust the pH to 2.0 with phosphoric acid;

[0052] Mobile phase B: Methanol;

[0053] Detection wavelength: 230nm;

[0054] Flow rate: 0.40ml / min

[0055] Column temperature: 15°C

[0056] The gradient elution procedure is the same as in Example 1.

[0057] For the results, see the attached image 3 .

Embodiment 3

[0058] Embodiment 3: detection instrument and chromatographic conditions:

[0059] Ultra-Performance Liquid Chromatography: Waters UPLC AcQuity H-Class

[0060] Chromatographic column: the reverse phase C18 column is selected from Infinity Lab Poroshell 120 SB-C18, the specification is 4.6*150mm, 2.7Micron.

[0061] Mobile phase A: Take 2.0g of anhydrous potassium dihydrogen phosphate, add 1000ml of water to dissolve, and adjust the pH to 2.2 with phosphoric acid;

[0062] Mobile phase B: Methanol;

[0063] Detection wavelength: 232nm;

[0064] Flow rate: 0.45ml / min

[0065] Column temperature: 25°C

[0066] The gradient elution procedure is the same as in Example 1.

[0067] For the results, see the attached Figure 4 .

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Abstract

The invention discloses an ultra-high performance liquid chromatography analysis method for dihydralazine sulfate and its related substances. Waters UPLC AcQuity H-Class is used, a reversed-phase C18 column is used, and potassium dihydrogen phosphate-phosphate buffer is used as the mobile phase A, Gradient elution with methanol as mobile phase B. The method can effectively control the known impurity content through the principal component self-contrast method with a correction factor, and the separation between the main peak and adjacent impurity peaks and between each impurity peak is greater than 1.5. The method of the application is simple, easy to operate, and has good reproducibility, accurate analysis and positioning of impurities, and can provide a reliable analysis method for controlling the quality of dihydralazine sulfate and its tablets.

Description

technical field [0001] The invention relates to a method for analyzing chemical drugs, in particular to an ultra-high performance liquid chromatography analysis method for dihydralazine sulfate and related substances in its tablets. Background technique [0002] Dihydralazine sulfate (Dihydralazine sulphate), the chemical name is 1,4-dihydrazino-2,3-naphthyridine sulfate bisesquihydrate, and its structural formula is as follows: [0003] [0004] Dihydralazine sulfate is a diuretic, commonly used in clinical adjuvant treatment of mild to moderate hypertension. At present, Journal of the Indian chemical society, 1990, vol, 67, P779-780 discloses the synthesis method of dihydralazine sulfate, which adopts the cyclization reaction of phthalic anhydride and hydrazine hydrate to obtain diketonalazine, and then chlorates it into dichlordalazine, Then nucleophilic substitution with hydrazine hydrate and salt formation to obtain dihydralazine sulfate. [0005] There are only a ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/74
CPCG01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/74G01N2030/324
Inventor 于立国朱怡君邱荣荣杨志明金晓峰孙光祥王兵
Owner CHANGZHOU PHARMA FACTORY
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