- British Pharmacopoeia Volume III
- Formulated Preparations: Specific Monographs
Beclometasone Aqueous Nasal Spray |
Beclometasone Nasal Spray
Glucocorticoid.
Beclometasone Aqueous Nasal Spray is an aqueous suspension of Anhydrous Beclometasone Dipropionate in a suitable container fitted with an appropriate nasal delivery system.
The liquid nasal spray complies with the requirements stated under Nasal Preparations and with the following requirements.
80.0 to 120.0% of the amount stated to be delivered by actuation of the valve.
A. Evaporate a quantity of the nasal spray to dryness. The infrared absorption spectrum of the residue, Appendix II A, is concordant with the reference spectrum of beclometasone dipropionate (RS 379).
B. In the Assay, the principal peak in the chromatogram obtained with solution (1) corresponds to the peak due to beclometasone dipropionate in the chromatogram obtained with solution (2).
Carry out the method for thin-layer chromatography, Appendix III A, using the following solutions in acetone.
(1) Evaporate a quantity of the nasal spray containing 0.5 mg of Anhydrous Beclometasone Dipropionate to dryness and dissolve the residue in 2 mL of acetone. Evaporate the solution to a volume such that the whole solution can be applied to the plate.
(2) 0.1% w/v of beclometasone dipropionate BPCRS.
(3) Dilute 1 volume of solution (2) to 2 volumes.
(4) Dilute 1 volume of solution (2) to 4 volumes.
(a) Use as the coating silica gel G.
(b) Use the mobile phase described below.
(c) Apply separately to the plate the whole of solution (1) and 10 µL of each of solutions (2), (3) and (4).
(d) Develop the plate to 15 cm.
(e) After removal of the plate, allow it to dry in air, spray with alkaline tetrazolium blue solution and heat at 50° for 5 minutes. Cool and spray again with alkaline tetrazolium blue solution.
3 volumes of methanol and 97 volumes of 1,2-dichloroethane.
In the chromatogram obtained with solution (1):
any secondary spot is not more intense than the spot in the chromatogram obtained with solution (2) (2%);
not more than one such spot is more intense than the spot in the chromatogram obtained with solution (3) (1%);
not more than two such spots are more intense than the spot in the chromatogram obtained with solution (4) (0.5%).
Disregard any spot with an Rf value of more than 0.85.
Carry out the method for liquid chromatography, Appendix III D, using the following solutions.
(1) Discharge the container a sufficient number of times to obtain 0.5 mg of Anhydrous Beclometasone Dipropionate, add 30 mL of mobile phase, mix with the aid of ultrasound, dilute to 50 mL with mobile phase and filter. Dilute 3 volumes of this solution to 20 volumes with mobile phase.
(2) 0.00015% w/v of beclometasone dipropionate BPCRS in the mobile phase.
(3) 0.00015% w/v each of testosterone propionate BPCRS and beclometasone dipropionate BPCRS in the mobile phase.
(a) Use a stainless steel column (10 cm × 4.6 mm) packed with octadecylsilyl silica gel for chromatography (5 µm) (Spherisorb ODS 1 is suitable).
(b) Use isocratic elution and the mobile phase described below.
(c) Use a flow rate of 2 mL per minute.
(d) Use a column temperature of 50°.
(e) Use a detection wavelength of 239 nm.
(f) Inject 20 µL of each solution.
30 volumes of water and 70 volumes of methanol, adjusted if necessary so that the resolution factor between the peaks due to beclometasone dipropionate and testosterone propionate is at least 2.0.
The test is not valid unless, in the chromatogram obtained with solution (3), the resolution factor between the two principal peaks is at least 2.0.
Calculate the average content of C28H37ClO7 delivered by a single actuation of the valve using the declared content of C28H37ClO7 in beclometasone dipropionate BPCRS.