British Pharmacopoeia Volume III

Formulated Preparations: Specific Monographs

Ibuprofen Tablets
General Notices

Action and use

Cyclo-oxygenase inhibitor; analgesic; anti-inflammatory.
Definition
Ibuprofen Tablets contain Ibuprofen. They are coated.
With the exception of the requirements for shape, the tablets comply with the requirements
stated under Tablets and with the following requirements.e
Content of ibuprofen, C13H18O2
95.0 to 105.0% of the stated amount.
Identification
A. Extract a quantity of the powdered tablets containing 0.5 g of Ibuprofen with 20 ml of
acetone, filter and evaporate the filtrate to dryness in a current of air without heating. The
infrared absorption spectrum of the residue, Appendix II A, is concordant with the reference
spectrum of ibuprofen (RS 186).
B. Melting point of the residue obtained in test A, after recrystallisation from petroleum
spirit (boiling range, 40 to 60), about 75, Appendix V A.
Test
Related substances
Carry out the method for liquid chromatography, Appendix III D, using 20 l of each of the
following solutions. For solution (1) add 30 ml of methanol to a quantity of the powdered
tablets containing 0.2 g of Ibuprofen, shake for 30 minutes, add 30 ml of methanol and
sufficient water to produce 100 ml, mix and filter through a glass microfibre filter paper
(Whatman GF/C is suitable). For solution (2) dilute 1 volume of solution (1) to 100 volumes
with the mobile phase. For solution (3) dissolve 50 mg of ibuprofen BPCRS in 2.5 ml of a
0.006% w/v solution of 2-(4-butylphenyl)propionic acid EPCRS in methanol (prepared by
diluting 1 volume of 2-(4-butylphenyl)propionic acid EPCRS to 10 volumes with methanol)
and add sufficient methanol to produce 25 ml.

The chromatographic procedure may be carried out using (a) a stainless steel column (15 cm
4.6 mm) packed with end-capped octadecylsilyl silica gel for chromatography (5 m)
(Spherisorb ODS 2 is suitable), (b) as the mobile phase with a flow rate of 2 ml per minute a
mixture of 0.5 volume of orthophosphoric acid, 340 volumes of acetonitrile and
600 volumes of water diluted to 1000 volumes with water after equilibration and (c) a
detection wavelength of 214 nm. Adjust the sensitivity so that the height of the principal
peak in the chromatogram obtained with solution (2) is 70 to 90% of full-scale deflection on
the chart paper. Record the chromatogram for 1.5 times the retention time of the principal
peak.
Equilibrate the column with the mobile phase for about 45 minutes before starting the
chromatography.
When the chromatograms are recorded under the conditions described above, the retention
time of ibuprofen is about 20 minutes. In the chromatogram obtained with solution (3)
measure the height (a) of the peak due to 2-(4-butylphenyl)-propionic acid and the height (b)
of the lowest point of the curve separating this peak from that due to ibuprofen. The test is
not valid unless a is greater than 1.5b. If necessary, adjust the concentration of acetonitrile in
the mobile phase to obtain the required resolution.
In the chromatogram obtained with solution (1) the area of any peak corresponding to 2-(4butylphenyl)propionic acid is not greater than that of the peak due to 2-(4butylphenyl)propionic acid in the chromatogram obtained with solution (3) (0.3%), the area
of any other secondary peak is not greater than 0.3 times the area of the principal peak in the
chromatogram obtained with solution (2) (0.3%) and the sum of the areas of any such peaks
is not greater than 0.7 times the area of the principal peak in the chromatogram obtained with
solution (2) (0.7%). Disregard any peak the area of which is less than 0.1 times the area of
the principal peak in the chromatogram obtained with solution (2) (0.1%).
Assay
Weigh and powder 20 tablets. Carry out the method for liquid chromatography, Appendix III
D, using the following solutions. For solution (1) shake a quantity of the powdered tablets
containing 0.2 g of Ibuprofen with 30 ml of the mobile phase for 30 minutes, add sufficient
of the mobile phase to produce 100 ml and mix thoroughly. Centrifuge 25 ml of the solution
at 2500 g for 5 minutes and use the supernatant liquid. Solution (2) contains 0.2% w/v of
ibuprofen BPCRS in the mobile phase.
The chromatographic procedure may be carried out using (a) a stainless steel column (25 cm
4.6 mm) packed with end-capped octadecylsilyl silica gel for chromatography (10 m)
(Nucleosil C18 is suitable), (b) a mixture of 3 volumes of orthophosphoric acid,
247 volumes of water and 750 volumes of methanol as the mobile phase with a flow rate of
1.5 ml per minute and (c) a detection wavelength of 264 nm.
Calculate the content of C13H18O2 using the declared content of C13H18O2 in ibuprofen BPCRS.