Ketoprofen Capsules
DEFINITION
Ketoprofen Capsules contain NLT 90.0% and NMT 110.0% of the labeled amount of ketoprofen (C16H14O3).
IDENTIFICATION
• A. Infrared Absorption 
197K
197K
Sample solution:
Shake a quantity of the contents of the Capsules containing 50 mg of ketoprofen with 5 mL of chloroform for 5 min, filter, and evaporate to dryness using a rotary evaporator.
Acceptance criteria:
Meet the requirements
• B.
The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.
ASSAY
• Procedure
The Standard solution and Sample solution must be protected from light.
Mobile phase:
Acetonitrile, glacial acetic acid, and water (90:1:110)
System suitability stock solution:
0.25 mg/mL of USP Ketoprofen RS and 0.5 mg/mL of USP Ketoprofen Related Compound A RS in Mobile phase
System suitability solution:
0.02 mg/mL of USP Ketoprofen RS and 0.04 mg/mL of USP Ketoprofen Related Compound A RS in Mobile phase from System suitability stock solution
Standard stock solution:
0.24 mg/mL of USP Ketoprofen RS in Mobile phase
Standard solution:
0.024 mg/mL of USP Ketoprofen RS in Mobile phase from Standard stock solution
Sample solution:
Nominally 0.024 mg/mL of ketoprofen in Mobile phase prepared as follows. Remove completely the contents of NLT 20 Capsules, and transfer a quantity of the contents, equivalent to 200 mg of ketoprofen, to a 250-mL volumetric flask. Add 150 mL of Mobile phase, stir for 2 h, then dilute with Mobile phase to volume. Centrifuge a portion of the preparation. Pipet 3.0 mL of clear supernatant into a 100-mL volumetric flask. Dilute with Mobile phase to volume.
Chromatographic system
Mode:
LC
Detector:
UV 250 nm
Column:
4.6-mm × 25-cm; 5-µm packing L1
Flow rate:
1.2 mL/min
Injection volume:
20 µL
System suitability
Samples:
System suitability solution and Standard solution
Suitability requirements
Resolution:
NLT 3.0 between ketoprofen and ketoprofen related compound A, System suitability solution
Tailing factor:
NMT 1.5 for the ketoprofen peak, System suitability solution
Relative standard deviation:
NMT 2.0%, Standard solution
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of the labeled amount of ketoprofen (C16H14O3) in the portion of Capsules taken:
Result = (rU/rS) × (CS/CU) × 100
| rU | = | = peak response from the Sample solution |
| rS | = | = peak response from the Standard solution |
| CS | = | = concentration of USP Ketoprofen RS in the Standard solution (mg/mL) |
| CU | = | = nominal concentration of ketoprofen in the Sample solution (mg/mL) |
Acceptance criteria:
90.0%–110.0%
PERFORMANCE TESTS
• Dissolution 711
711
The Standard solution and Sample solution must be protected from light.
Medium:
0.05 M phosphate buffer, pH 7.4; 1000 mL
Apparatus 2:
50 rpm
Time:
30 min
Standard solution:
USP Ketoprofen RS in Medium
Sample solution:
Pass a portion of the solution under test through a suitable filter. Dilute with Medium, if necessary, to a concentration similar to that of the Standard solution.
Instrumental conditions
Mode:
UV
Analytical wavelength:
260 nm
Cell path length:
1 cm
Blank:
Medium
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of the labeled amount of ketoprofen (C16H14O3) dissolved:
Result = (AU/AS) × (CS/L) × D × V × 100
| AU | = | = absorbance from the Sample solution |
| AS | = | = absorbance from the Standard solution |
| CS | = | = concentration of the Standard solution (mg/mL) |
| L | = | = label claim (mg/Capsule) |
| D | = | = dilution factor of the Sample solution |
| V | = | = volume of Medium, 1000 mL |
Tolerances:
NLT 80% (Q) of the labeled amount of ketoprofen (C16H14O3) is dissolved.
IMPURITIES
• Organic Impurities
The System suitability solution, Standard solution, and Sample solution must be protected from light.
Buffer:
68.0 g/L of monobasic potassium phosphate in water. Adjust with phosphoric acid to a pH of 3.5 ± 0.05.
Mobile phase:
Acetonitrile, water, and Buffer (43:55:2)
Diluent:
Acetonitrile and water (2:3)
System suitability solution:
5 µg/mL of USP Ketoprofen RS and 1.5 µg/mL of USP Ketoprofen Related Compound D RS in Diluent
Standard solution:
2 µg/mL of USP Ketoprofen RS, 2 µg/mL of USP Ketoprofen Related Compound C RS, and 3 µg/mL of USP Ketoprofen Related Compound D RS in Diluent
Sample solution:
Nominally 1 mg/mL of ketoprofen in Mobile phase
Chromatographic system
Mode:
LC
Detector:
UV 233 nm
Column:
4.6-mm × 15-cm; 5-µm packing L1
Flow rate:
1 mL/min
Injection volume:
20 µL
Run time:
7 times the retention time of ketoprofen
System suitability
Sample:
System suitability solution
Suitability requirements
Resolution:
NLT 7.0 between ketoprofen related compound D and ketoprofen
Relative standard deviation:
NMT 10% for the ketoprofen peak
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of each impurity in the portion of Capsules taken:
Result = (rU/rS) × (CS/CU) × 100
| rU | = | = peak response of each impurity from the Sample solution |
| rS | = | = peak response of the corresponding related compound from the Standard solution |
| CS | = | = concentration of the corresponding USP Ketoprofen Related Compound RS in the Standard solution (mg/mL); use the concentration of the USP Ketoprofen RS for unknown impurities |
| CU | = | = nominal concentration of ketoprofen in the Sample solution (mg/mL) |
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in tight containers, and store at controlled room temperature.
• USP Reference Standards 11
11
USP Ketoprofen RS 
(±)-m-Benzoylhydratropic acid.
C16H14O3 254.28
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(±)-m-Benzoylhydratropic acid.
C16H14O3 254.28
USP Ketoprofen Related Compound A RS
-Methyl-3-(4-methylbenzoyl) benzeneacetic acid.
C17H16O3 268.31
-Methyl-3-(4-methylbenzoyl) benzeneacetic acid.
C17H16O3 268.31
USP Ketoprofen Related Compound C RS
2-(3-Carboxyphenyl) propionic acid.
C10H10O4 194.18
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2-(3-Carboxyphenyl) propionic acid.
C10H10O4 194.18
USP Ketoprofen Related Compound D RS
3-Acetylbenzophenone.
C15H12O2 224.25
3-Acetylbenzophenone.
C15H12O2 224.25
Auxiliary Information—
Please check for your question in the FAQs before contacting USP.
| Topic/Question | Contact | Expert Committee |
|---|---|---|
| Monograph | Hillary Z Cai
Scientific Liaison, Small Molecules (301) 230-3379 |
(SM22010) Monographs - Small Molecules 2 |
| 711 |
Margareth R.C. Marques, Ph.D.
Senior Scientific Liaison (301) 816-8106 |
(GCDF2010) General Chapters - Dosage Forms |
| Reference Standards | RS Technical Services 1-301-816-8129 rstech@usp.org |
USP38–NF33 Page 4007
Pharmacopeial Forum: Volume No. 39(3)