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

Method for separating and measuring sulfonamide-class impurities in celecoxib through HPLC (High Performance Liquid Chromatography) and application

A technology for sulfonamides and celecoxib, which is used in the separation and determination of sulfonamide impurities in celecoxib by HPLC and the application field, can solve the problems such as the simultaneous separation and quantitative determination of sulfonamides cannot be well achieved, and achieves peak type Good results

Active Publication Date: 2019-06-18
HINYE PHARM CO LTD
View PDF7 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0021] It can be seen that the above-mentioned existing analytical methods cannot realize the simultaneous separation and quantitative determination of the three impurities of sulfonamide, 4-SAPH and YF042-14.

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
  • Method for separating and measuring sulfonamide-class impurities in celecoxib through HPLC (High Performance Liquid Chromatography) and application
  • Method for separating and measuring sulfonamide-class impurities in celecoxib through HPLC (High Performance Liquid Chromatography) and application
  • Method for separating and measuring sulfonamide-class impurities in celecoxib through HPLC (High Performance Liquid Chromatography) and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Embodiment 1: Determination of detection wavelength

[0062] Instrument: Waters e2695-2489 high performance liquid chromatography

[0063] Chromatographic column: phenyl bonded silica gel as filler (Supelcosil LC-DP 4.6*250mm, 5um)

[0064] Mobile phase: Acetonitrile was used as mobile phase A, and 0.05% phosphoric acid solution was used as mobile phase B to carry out gradient elution according to the following table 2:

[0065] time (min)

Mobile phase A (%)

Mobile phase B (%)

0

15

85

15

15

85

20

80

20

25

80

20

30

15

85

35

15

85

[0066] At 0 min, the volume ratio of the inorganic acid in the mobile phase to the organic phase was 85%: 15% (i.e. the initial volume ratio); at 20 min, the volume ratio of the inorganic acid in the mobile phase was reduced to 20%, and the volume ratio of the organic phase The volume ratio increased to 80%; 30 minutes later, the volume ratio of the...

Embodiment 2

[0077] Embodiment 2: the HPLC detection of celecoxib crude drug

[0078] The apparatus and reagents are the same as in Example 1.

[0079] Take about 10 mg each of the sulfonamide reference substance, 4-SAPH reference substance and YF042-14 reference substance, weigh them accurately, place them in 100ml measuring bottles, add diluent to dissolve and dilute to the mark, take 1ml of each of the above three solutions and put them in the same 200ml In the measuring bottle, add diluent to dilute to the mark, and use it as the reference substance stock solution (4-SAPH needs to be newly prepared before use). Precisely pipette 1.5ml of the reference substance stock solution, put it in a 20ml volumetric bottle, add diluent to dilute to the mark, shake well, and use it as the reference substance solution (newly prepared for immediate use).

[0080] Take about 100mg of celecoxib, accurately weighed, put in a 10ml measuring bottle, add 2ml of acetonitrile to dissolve, then dilute to the...

Embodiment 3

[0091] Embodiment 3: system suitability test

[0092] The apparatus and reagents are the same as in Example 1. The system applicability of this embodiment also inspected the system applicability of the instrument during continuous sampling. Since 4-SAPH is unstable, only the other two impurities, sulfonamide and YF042-14, were used to investigate the applicability of the instrument system.

[0093] Take about 10 mg each of the sulfonamide reference substance and YF042-14 reference substance, weigh them accurately, place them in 100ml measuring bottles, add diluent to dissolve and dilute to the mark, take 1ml of each of the above two solutions and put them in the same 200ml measuring bottle, add diluent diluted to volume as a system suitability stock solution. Precisely pipette 1.5ml of the reference substance stock solution, put it in a 20ml measuring bottle, add diluent to dilute to the mark, shake well, and use it as a system suitability solution.

[0094] Take the system ...

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
wavelengthaaaaaaaaaa
Login to View More

Abstract

The invention provides a method for separating and measuring sulfonamide-class impurities in celecoxib through HPLC (High Performance Liquid Chromatography) and application. According to the chromatographic column of the high performance liquid chromatography, phenyl bonded silica gel is adopted as a stationary phase, and an inorganic acid-organic phase is adopted as a mobile phase to perform gradient elution; the temperature of the stationary phase ranges from 25 to 35 degrees Celsius, the flow rate of the stationary phase ranges from 0.9 to 1.1 mL / min, and the detection wavelength of the stationary phase ranges from 248 to 250 nm; the temperature of a sample chamber ranges from 4 to 10 degrees Celsius; and the initial volume ratio of the inorganic acid to the organic phase of the mobilephase ranges from (72:28) to (85:15). The method of the invention can simultaneously separate and quantitatively measure three kinds of sulfonamide-class impurities, namely, sulfonamide, 4-SAPH and YF042-14 in celecoxib and chemical medicines containing sulfonamide-class impurities without being interfered, has a good peak pattern, and can completely and effectively control the quality of the celecoxib raw material. The method has the advantages of high specificity, high sensitivity and good accuracy.

Description

technical field [0001] The invention relates to the technical field of chemical drug analysis, in particular to a method and application for separating and measuring sulfonamide impurities in celecoxib by using HPLC, and in particular to a method for simultaneously separating and measuring celecoxib by using high performance liquid chromatography Method and application of sulfonamide genotoxic impurity sulfonamide, 4-SAPH, YF042-14 present in the present invention. technical background [0002] Sulfonamide and 4-SAPH (4-sulfonylphenylhydrazine hydrochloride) are the starting materials for the synthesis of celecoxib API; The by-product generated by the condensation reaction between the starting material 4-SAPH and unreacted ethyl trifluoroacetate during the process of raw material medicine. All three are possible impurities in celecoxib. The chemical structural formulas of the three are as follows: [0003] [0004] Sulfa 4-SAPH YF042-14 [0005] Genotoxic impurities r...

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): G01N30/02G01N30/06
Inventor 肖倩南朱红霖朱丹丹程雪清王衡新高玉贺
Owner HINYE 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