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A kind of rt-hplc detection method of related substances of valdecoxib/parecoxib

A technology of RT-HPLC and parecoxib, which is applied in the field of drug analysis, can solve the problems of separation of characteristic peaks of valdecoxib and isomerism of parecoxib characteristic peaks and parecoxib Problems such as separation of characteristic peaks of body and meta-parecoxib

Active Publication Date: 2019-12-13
TAIZHOU FUDAN-ZHANGJIANG PHARM CO LTD +2
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  • 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

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  • A kind of rt-hplc detection method of related substances of valdecoxib/parecoxib
  • A kind of rt-hplc detection method of related substances of valdecoxib/parecoxib
  • A kind of rt-hplc detection method of related substances of valdecoxib/parecoxib

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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 (SUPELCOSIL LC-DP 250*4.6mm, 5μm);

[0039] 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 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 (SUPELCOSIL LC-DP 250*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 valde...

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 (SUPELCOSIL LC-DP 250*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), hydrolysis impurity (A), disubstituted impurity (B...

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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 substances such as starting materials, reagents, intermediates, by-products and isomers brought in during the production of raw materials, and may also be Special impurities such as degradation products, polymers or crystal transformations produced 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 indi...

Claims

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Application Information

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Patent Type & Authority Patents(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
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