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High performance liquid chromatography analysis method for dihydralazine sulfate related substances

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

Active Publication Date: 2020-09-01
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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  • High performance liquid chromatography analysis method for dihydralazine sulfate related substances
  • High performance liquid chromatography analysis method for dihydralazine sulfate related substances
  • High performance liquid chromatography analysis method for 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 related substances thereof. Waters UPLC AcQuity H-Class is used, a reversed-phaseC18 column is adopted, a monopotassium phosphate-phosphoric acid buffer solution is used as a mobile phase A, and methanol is used as a mobile phase B, and then gradient elute treatment is performed.According to the method, the known impurity content can be effectively controlled through a main component self-contrast method with correction factors, and the separation degree between a main peak and adjacent impurity peaks and the separation degree between the main peak and each impurity peak are both larger than 1.5. The method is simple, convenient to operate, good in reproducibility and accurate in impurity analysis and positioning, and a reliable analysis method can be provided for controlling the quality of dihydralazine sulfate and tablets thereof.

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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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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