Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

An RT-HPLC detecting method for valdecoxib/parecoxib related substances

An RT-HPLC, detection method technology, applied in the field of drug analysis, can solve the problem of inability to separate valdecoxib valdecoxib characteristic peaks, inability to distinguish between parecoxib characteristic peaks and parecoxib isomers. Separation of characteristic peaks of meta-parecoxib

Active Publication Date: 2016-06-08
TAIZHOU FUDAN-ZHANGJIANG PHARM CO LTD +2
View PDF3 Cites 13 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The technical problem to be solved by this invention is to provide a detection method to solve the problem that the prior art cannot separate the characteristic peaks of valdecoxib from the isomers of valdecoxib and the characteristic peaks of meta-valdecoxib. The problem of not being able to separate the characteristic peaks of parecoxib from the characteristic peaks of parecoxib isomers and meta-parecoxib

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • An RT-HPLC detecting method for valdecoxib/parecoxib related substances
  • An RT-HPLC detecting method for valdecoxib/parecoxib related substances
  • An RT-HPLC detecting method for valdecoxib/parecoxib related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Instrument and chromatographic conditions

[0037] High performance liquid chromatography: Agilent1260 high performance liquid chromatography system and workstation;

[0038] Chromatographic column: phenyl column (SUPELCOSILLC-DP250*4.6mm, 5μm);

[0039] Prepare a 0.01mol / L disodium hydrogen phosphate solution, adjust the pH value to 3.0 with phosphoric acid as the water phase, the ratio of water phase to methanol in the mobile phase is 52:48, set the flow rate to 1.0ml / min, and the detection wavelength to 215nm. The temperature is 40°C.

[0040] (2) Experimental steps

[0041] Take parecoxib sodium, meta-parecoxib (G), parecoxib isomers (F), valdecoxib, meta-valdecoxib (D), valdecoxib Isomer (C), hydrolysis impurity (A), disubstituted impurity (B), dimer impurity (H), acetylation impurity (E), valdecoxibate ethyl ester (J), starting Appropriate amount of material S, S isomer (I), dissolved and diluted with methanol-water (1:1) to make about 0.2 mg each of valde...

Embodiment 2

[0044] (1) Instrument and chromatographic conditions

[0045] High performance liquid chromatography: Agilent1260 high performance liquid chromatography system and workstation;

[0046] Chromatographic column: phenyl column (SUPELCOSILLC-DP250*4.6mm, 5μm);

[0047] Prepare 0.01mol / L disodium hydrogen phosphate solution, adjust the pH value to 3.0 with phosphoric acid as the water phase, the ratio of water phase to methanol in the mobile phase is 55:45, set the flow rate to 1.0ml / min, and the detection wavelength to 215nm. The temperature is 40°C.

[0048] (2) Experimental steps

[0049] Take parecoxib sodium, meta-parecoxib (G), parecoxib isomers (F), valdecoxib, meta-valdecoxib (D), valdecoxib Isomer (C), hydrolysis impurity (A), disubstituted impurity (B), dimer impurity (H), acetylation impurity (E), valdecoxibate ethyl ester (J), starting Appropriate amount of material S, S isomer (I), dissolved and diluted with methanol-water (1:1) to make about 0.2 mg each of valdeco...

Embodiment 3

[0052] (1) Instrument and chromatographic conditions

[0053] High performance liquid chromatography: Agilent1260 high performance liquid chromatography system and workstation;

[0054] Chromatographic column: phenyl column (SUPELCOSILLC-DP250*4.6mm, 5μm);

[0055] Prepare a 0.01mol / L disodium hydrogen phosphate solution, adjust the pH value to 3.0 with phosphoric acid as the water phase, and carry out gradient elution with the water phase-methanol ratio in the mobile phase as shown in Table 2, set the flow rate to 1.0ml / min, and detect the wavelength at 215 nm, the column temperature is 40°C.

[0056] Table 2

[0057]

water box%

The organic phase%

0min

52

48

25min

52

48

40min

40

60

40.1min

52

48

50min

52

48

[0058] (2) Experimental steps

[0059] Take parecoxib sodium, meta-parecoxib (G), parecoxib isomers (F), valdecoxib, meta-valdecoxib (D), valdecoxib Isomer (C), h...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
lengthaaaaaaaaaa
particle diameteraaaaaaaaaa
Login to View More

Abstract

The invention relates to the technical field of medicine analysis, and particularly relates to a reversed-phase high-performance liquid chromatography (RT-HPLC) detecting method for valdecoxib / parecoxib related substances. The RT-HPLC detecting method includes preparing an analysis solution, determining chromatography conditions and detecting in an instrument. The method can effectively detect existence of the related substances in valdecoxib and parecoxib solutions, particularly separates the characteristic peak of the valdecoxib, the characteristic peak of a valdecoxib isomeride and the characteristic peak of meta valdecoxib in a spectrum, and particularly separates the characteristic peak of the parecoxib, the characteristic peak of a parecoxib isomeride and the characteristic peak of meta parecoxib in a spectrum, thus ensuring quality controllability of products.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a reversed-phase high-performance liquid chromatography detection method for related substances of valdecoxib / parecoxib. Background technique [0002] The so-called "related substances" in drug analysis refer to the starting materials, reagents, intermediates, by-products and isomers brought in during the production of raw materials Special impurities such as degradation products, polymers or crystal transformations generated during storage and transportation. The type of related substances is closely related to the synthesis route and preparation process of the drug. Any change in any factor in the process of drug synthesis and preparation may lead to different types of related substances. Therefore, the detection and control process of related substances is relatively complicated. The detection of related substances is an important indicator for controlling the quality o...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/89
Inventor 周静霍立茹张若明田建宣尹明福董成成甘益民邱雪飞杨斌
Owner TAIZHOU FUDAN-ZHANGJIANG PHARM CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com