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A high-performance liquid chromatography analysis method for related substances of regano

A high-performance liquid chromatography and analysis method technology, applied in the field of drug analysis, can solve problems such as inability to effectively separate and analyze, inability to accurately quantitatively determine impurities, and drug safety risks.

Active Publication Date: 2018-04-24
NANJING HERON PHARMA SCI & TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

That is to say, the impurities described in the present invention cannot be effectively separated and analyzed under the above conditions, and these potential impurities cannot be accurately quantitatively determined, which brings a great risk to the drug safety of Reganosen

Method used

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  • A high-performance liquid chromatography analysis method for related substances of regano
  • A high-performance liquid chromatography analysis method for related substances of regano
  • A high-performance liquid chromatography analysis method for related substances of regano

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Example 1 High-performance liquid chromatography analysis method for related substances in the raw material drug of Reganoson

[0067] The high-performance liquid chromatographic analysis method for detecting related substances in the raw material drug of Reganosen, specifically includes the following steps:

[0068] (a) Chromatographic conditions setting: Agilent C18 (250×4.6mm, 5μm) reversed-phase C18 column is used, column temperature is 35°C; mobile phase A is a phosphate buffer system of sodium 1-pentanesulfonate, and the 1- The concentration of sodium pentanesulfonate is 15mmol / L, the concentration of phosphoric acid in the buffer system is 0.02mol / L, and the pH is adjusted to 4.2 with sodium hydroxide; the mobile phase B is methanol, and gradient elution is carried out; the flow rate is 1.0ml / min ; The detection wavelength is 247nm; The eluent is composed of mobile phase A and mobile phase B, and the elution procedure is as follows,

[0069] ;

[0070] (b) Pr...

Embodiment 2

[0078] Example 2 High performance liquid chromatography analysis method for related substances in Ruiganuosheng injection

[0079] The high-performance liquid chromatography analysis method for detecting related substances in Reganosheng injection specifically includes the following steps:

[0080] (I) Chromatographic condition setting: Agilent C18 (250×4.6mm, 5 μm) is used as a reversed-phase C18 column, and the column temperature is 35°C; mobile phase A is a phosphate buffer system of sodium 1-pentanesulfonate, and the 1- The concentration of sodium pentanesulfonate is 15mmol / L, the concentration of phosphoric acid in the buffer system is 0.02mol / L, and the pH is adjusted to 4.2 with sodium hydroxide; the mobile phase B is methanol, and gradient elution is carried out; the flow rate is 1.0ml / min ; The detection wavelength is 247nm; The eluent is composed of mobile phase A and mobile phase B, and the elution procedure is as follows,

[0081] ;

[0082] (II) Preparation of...

Embodiment 3

[0090] Example 3 Screening and exploration of mobile phase conditions

[0091] Take the reference substance of Reganosen, and appropriate amounts of impurities A, D, F, G, H, I, and J, and make a solution with a certain concentration, and use it as a system adaptability solution for investigation. Take an appropriate amount of system adaptability solution and inject it into the high-performance liquid chromatograph. The main test results are summarized in the attached Figure 2-3 And attached figure 1 .

[0092]

[0093] Note 1 The procedure is as follows,

[0094] .

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Abstract

The invention discloses a high performance liquid chromatographic analysis method for related substances of regadenoson. According to the method, a reversed phase column and an ultraviolet detector are adopted, and a 1-alkyl sodium sulfonate solution-methanol is adopted as a flowing phase for gradient elution. By the method, all known impurities in regadenoson raw materials and a preparation can be analyzed at the same time, the content of each known impurity can be effectively controlled by a principal component self-contrast method adopting a correction factor, degrees of separation between each impurity peak as well as between a major peak and an adjacent impurity peak are all more than 1.5, and the peak impurity of the major peak and each impurity peak is higher than 1.0. A simple and reliable analysis method is provided for quality control over the regadenoson raw materials and the preparation.

Description

technical field [0001] The invention belongs to the field of drug analysis, and in particular relates to a high-performance liquid chromatography analysis method for related substances of reganosen. Background technique [0002] Regadenoson, chemical name 1-(6-amino-9-((2S,3R,4S,5R)-3,4-dihydroxy-5-(hydroxymethyl)tetrahydrofuran ring-yl)- 9H-purin-2-yl)-N-methyl-1H-pyrazole-4-carboxamide monohydrate, the structural formula is as follows, [0003] . [0004] Regadenoson (trade name Lexiscan) is a selective adenosine receptor agonist developed by CV Therapeutics, which can relax coronary arteries. This drug is used for radionuclide myocardial perfusion imaging in patients who cannot undergo exercise stress testing. Clinicians also use it for CT imaging beyond the applicable disease. [0005] There are many impurities in Reganosan. From the perspective of sources, the impurities in Reganosan mainly come from the reaction raw materials, synthetic intermediates, reaction by...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/34G01N30/60G01N30/89
CPCG01N30/02G01N30/34G01N30/60G01N30/89G01N2030/027
Inventor 徐丽闵涛曹卫王继芳刘婷婷
Owner NANJING HERON PHARMA SCI & TECH CO LTD
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