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Celecoxib
Impurities Method with Improved Peak Shape
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printable Application Sheet
Notes:
Celecoxib is a selective COX-2 inhibitor used for treatment of acute pain and inflammation due to conditions such as arthritis. It is
marketed by Pfizer under the trade name Celebrex®, which is under patent protection until 2014.
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Method Conditions
| Column |
Cogent Phenyl Hydride™, 4µm, 100A |
| Catalog No. |
69020-7.5P |
| Dimensions |
4.6 x 75 mm |
| Mobile Phase |
A: DI H2O/ 0.1% formic acid
B: 97% MeCN/ 3% DI H2O/ 0.1% formic acid |
| Gradient |
| time (min.) |
%B |
| 0 |
30 |
| 5 |
60 |
| 6 |
30 |
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| Post Time |
4 min. |
| Temperature |
35° C |
| Flow rate |
1.0 mL/min |
| Injection Volume |
5 µL |
| Sample |
A 200 mg strength Celebrex® capsule was ground
and added to a 100 mL volumetric flask. 50 mL
MeOH was added and the solution was sonicated.
The flask was diluted to mark with solvent A
and a portion was filtered with a 0.45 micron
nylon syringe filter (MicroSolv Tech Corp). |
| Peaks |
1. Impurity
2. Celecoxib |
| Detection |
UV 254 nm |
| t0 |
0.9 min |
Discussion
Celecoxib is separated from an impurity in this simple gradient method. The peak shape obtained for the API is excellent and shows good peak
symmetry. In addition, the method shows good repeatability from run to run. The API retention time %RSD from five runs was 0.025%. The five run
overlay chromatogram is shown in Figure A. Figure B shows a zoom-in view so that the impurity peak can be seen clearly. Another benefit of the
method is that the mobile phase is MS-compatible.
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