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Method for separating etoricoxib and related substances thereof by using high performance liquid chromatography

A technique for etoricoxib and related substances, applied in the field of liquid chromatography separation and determination of etoricoxib and related substances, can solve the problems of incomplete removal, influence on drug purity and quality, etc., and achieve the effect of ensuring quality controllable

Active Publication Date: 2015-05-13
BEIJING VENTUREPHARM BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the process of synthesizing etoricoxib, some important intermediates may affect the purity and quality of the drug due to incomplete removal

Method used

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  • Method for separating etoricoxib and related substances thereof by using high performance liquid chromatography
  • Method for separating etoricoxib and related substances thereof by using high performance liquid chromatography
  • Method for separating etoricoxib and related substances thereof by using high performance liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Instruments and Conditions

[0040] High performance liquid chromatography: Shimadzu: LC-20AT, CBM-20A, SIL-20AC, SPD-M20A, CTO-10ASvp;

[0041] Chromatographic column: Phenyl (Kromasil, 250mm×4.6mm, 5μm)

[0042] Mobile phase A: 0.02mol / L ammonium formate buffer solution (pH 3.5)

[0043] B: Acetonitrile

[0044] Using gradient elution:

[0045] T (min) 0 3 5 25 35 45 52 60 B（%） 8 8 18 18 35 33 8 8

[0046] Flow rate: 1.0mL / min

[0047] Detection wavelength: 235nm

[0048] Injection volume: 10μL

[0049] Experimental procedure

[0050] Take an appropriate amount of etoricoxib and its related substances, and dissolve the samples with 50% methanol water to prepare a sample solution containing about 0.5 mg / mL of etoricoxib and its related substances; another appropriate amount of 50% methanol water is used as a blank solvent. Perform HPLC analysis according to the above conditions, and record the chromatograms. see attached result...

Embodiment 2

[0052] Instruments and Conditions

[0053] High performance liquid chromatography: Shimadzu: LC-20AT, CBM-20A, SIL-20AC, SPD-M20A, CTO-10ASvp;

[0054] Chromatographic column: Phenyl (Kromasil, 250mm×4.6mm, 5μm)

[0055] Mobile phase A: 0.02mol / L ammonium formate buffer solution (pH 3.5)

[0056] B: Acetonitrile

[0057] Using gradient elution;

[0058] T (min) 0 10 25 26 50 55 60 B（%） 7 14 18 35 35 7 7

[0059] Flow rate: 1.0mL / min

[0060] Detection wavelength: 235nm

[0061] Injection volume: 10μL

[0062] Experimental procedure

[0063] Take an appropriate amount of etoricoxib and its related substances, and dissolve the samples with 50% methanol water to prepare a sample solution containing about 0.5 mg / mL of etoricoxib and its related substances; another appropriate amount of 50% methanol water is used as a blank solvent. Perform HPLC analysis according to the above conditions, and record the chromatograms. see attached results Fig...

Embodiment 3

[0065] The model of high performance liquid chromatograph, without special requirement, the chromatograph that the present invention adopts is Shimadzu: LC-20AT, CBM-20A, SIL-20AC, SPD-M20A, CTO-10ASvp

[0066] Chromatographic column: Phenyl (Kromasil, 250mm×4.6mm, 5μm)

[0067] Mobile phase A: 0.02mol / L ammonium formate buffer solution (pH 3.5)

[0068] B: Acetonitrile

[0069] Using gradient elution;

[0070] T (min) 0 15 25 28 55 56 60 B（%） 7 15 20 32 32 7 7

[0071] Flow rate: 1.0mL / min

[0072] Detection wavelength: 235nm

[0073] Injection volume: 10μL

[0074] Experimental procedure

[0075] Take an appropriate amount of etoricoxib and its related substances, and dissolve the samples with 50% methanol water to prepare a sample solution containing about 0.5 mg / mL of etoricoxib and its related substances; another appropriate amount of 50% methanol water is used as a blank solvent. Perform HPLC analysis according to the above condition...

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Abstract

The invention belongs to the field of analytical chemistry and discloses a method for separating and determining etoricoxib and related substances thereof by using liquid chromatography. The method can be used for quantitatively determining the contents of etoricoxib and related substances thereof by using phenyl silane bonded silica gel as a chromatographic column of fillers and using a certain proportion of buffer salt solutions-organic phases as mobile phases, thus effectively controlling the quality of etoricoxib. The method has strong specificity and high precision and is simple and convenient to operate.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a liquid chromatography separation and determination method for etoricoxib and its related substances. Background technique [0002] Etoricoxib is a highly selective cyclooxygenase-2 (COX-2) inhibitor drug, the English name is Etoricoxib, the chemical name is [5-chloro-2-(6-methylpyridin-3 base)-3 -(4-Methylsulfonylphenyl)pyridine](5-Chloro-3-(4-methanesulfonyl-phenyl)-6'-methyl-[2,3']bipyridinyl), molecular formula C 18 h 15 ClN 2 o 2 S, the structural formula is: [0003] [0004] Etoricoxib is used in the treatment of osteoarthritis (OA), rheumatoid arthritis and acute gouty arthritis. Etoricoxib is an analgesic drug with improved performance compared with traditional non-steroidal anti-inflammatory drugs (NSAIDs), and it is the only coxib drug that has been proven effective in the treatment of acute gouty arthritis. Other indications currently approved...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 赵路路王宇杰马苏峰
Owner BEIJING VENTUREPHARM BIOTECH
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