11/3/2020 USP-NF Ketoprofen Capsules

Printed on: Tue Nov 03 2020, 09:33:12 am

Printed by: Shruti Kharidia
O cial Status: Currently O cial on 03-Nov-2020
O cial Date: O cial as of 1-May-2020
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© 2020 USPC

Ketoprofen Capsules
DEFINITION
Ketoprofen Capsules contain NLT 90.0% and NMT 110.0% of the labeled amount of ketoprofen (C16H14O3).

IDENTIFICATION
Change to read:
• A. ▲SPECTROSCOPIC IDENTIFICATION TESTS 〈197〉, Infrared Spectroscopy: 197K▲ (CN 1-MAY-2020)
Sample solution: Shake a quantity of the contents of the Capsules containing 50 mg of ketoprofen with 5 mL of chloroform for 5 min,
lter, 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 L
Standard solution: 0.024 mg/mL of USP Ketoprofen RS in Mobile phase from Standard stock solution
IA
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 ask. 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 ask. Dilute with Mobile phase to volume.
IC

Chromatographic system
(See Chromatography 〈621〉, System Suitability.)
Mode: LC
Detector: UV 250 nm
Column: 4.6-mm × 25-cm; 5-µm packing L1
FF

Flow rate: 1.2 mL/min

Injection volume: 20 µL
System suitability
Samples: System suitability solution and Standard solution
Suitability requirements
O

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〉

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11/3/2020 USP-NF Ketoprofen Capsules

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 lter. Dilute with Medium, if necessary, to a concentration
similar to that of the Standard solution.
Instrumental conditions
(See Ultraviolet-Visible Spectroscopy 〈857〉.)
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

L
Tolerances: NLT 80% (Q) of the labeled amount of ketoprofen (C16H14O3) is dissolved.
IA
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.
IC

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
FF

Ketoprofen Related Compound D RS in Diluent

Sample solution: Nominally 1 mg/mL of ketoprofen in Mobile phase
Chromatographic system
(See Chromatography 〈621〉, System Suitability.)
Mode: LC
Detector: UV 233 nm
O

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

= concentration of the corresponding USP Ketoprofen Related Compound RS in the Standard solution (mg/mL); use the
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11/3/2020 USP-NF Ketoprofen Capsules
CS concentration of the USP Ketoprofen RS for unknown impurities

CU = nominal concentration of ketoprofen in the Sample solution (mg/mL)

Acceptance criteria: See Table 1.

Table 1

Relative Retention Acceptance Criteria,

Name Time NMT (%)

Ketoprofen related compound Ca 0.3 0.2

Ketoprofen 1.0 —

Ketoprofen related compound Db 1.5 0.3

Individual unspeci ed impurity — 0.2

Total impurities — 0.5

a
  2-(3-Carboxyphenyl) propionic acid.
b  3-Acetylbenzophenone.

ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in tight containers, and store at controlled room temperature.
• USP REFERENCE STANDARDS 〈11〉
USP Ketoprofen RS
(±)-m-Benzoylhydratropic acid.
C16H14O3 254.28 L
IA
USP Ketoprofen Related Compound A RS
α-Methyl-3-(4-methylbenzoyl) benzeneacetic acid.
C17H16O3 268.31
USP Ketoprofen Related Compound C RS
2-(3-Carboxyphenyl) propionic acid.
C10H10O4 194.18
IC

USP Ketoprofen Related Compound D RS

3-Acetylbenzophenone.
C15H12O2 224.25
FF

Auxiliary Information- Please check for your question in the FAQs before contacting USP.

Topic/Question Contact Expert Committee

KETOPROFEN CAPSULES Wei Yang SM22020 Small Molecules 2

O

Scienti c Liaison

Chromatographic Database Information: Chromatographic Database

Most Recently Appeared In:

Pharmacopeial Forum: Volume No. 39(3)

Page Information:

USP43-NF38 - 2510
USP42-NF37 - 2458
USP41-NF36 - 2312

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