Methylprednisolone Tablets

General Notices

Action and use

Glucocorticoid.

Definition

Methylprednisolone Tablets contain Methylprednisolone.

The tablets comply with the requirements stated under Tablets and with the following requirements.

Content of methylprednisolone, C22H30O5

90.0 to 110.0% of the stated amount.

Identification

Extract a quantity of the powdered tablets containing 50 mg with 100 mL of chloroform, filter and evaporate the filtrate to dryness. The residue complies with the following tests.

A. The infrared absorption spectrum, Appendix II A, is concordant with the reference spectrum of methylprednisolone (RS 225).
B. Carry out the method for thin-layer chromatography, Appendix III A, using the following solutions.
(1) Shake a quantity of the powdered tablets containing 10 mg of methylprednisolone in a mixture of 1 volume of methanol and 9 volumes of dichloromethane and dilute to 10 mL with the same solvent; centrifuge and use the supernatant liquid.
(2) Dissolve 20 mg of methylprednisolone BPCRS in a mixture of 1 volume of methanol and 9 volumes of dichloromethane and dilute to 20 mL with the same solvent mixture.
(3) Dissolve 10 mg of hydrocortisone BPCRS in solution (2) and dilute to 10 mL with solution (2).
chromatographic conditions
(a) Use as the coating silica gel F254..
(b) Use the mobile phase as described below.
(c) Apply 5 µL of each solution.
(d) Develop the plate to 15 cm.
(e) After the first development carry out the second development, dry in air and examine under ultraviolet light (254nm). Spray with alcoholic solution of sulfuric acid, heat at 120 °C for 10 minutes or until the spots appear. Allow to cool. Examine in daylight and under ultraviolet light (365 nm).
mobile phase
For the first developmentAdd a mixture of 1.2 volumes of water and 8 volumes of methanol to a mixture of 15 volumes of ether and 77 volumes of dichloromethane.
For the second developmentButanol saturated with a mixture of 5 volumes of water, 15 volumes of toluene and 80 volumes of ether.
system suitability

The test is not valid unless the chromatogram obtained with solution (3) shows two clearly separated spots.

confirmation

The principal spot in the chromatogram obtained with solution (1) is similar in position, colour in daylight, fluorescence in ultraviolet light at 365 nm and size to that in the chromatogram obtained with solution (2).

Tests

Dissolution

Comply with the requirements for Monographs of the British Pharmacopoeia in the dissolution test for tablets and capsules, Appendix XII B1.

test conditions
(a) Use Apparatus 1, rotating the basket at 100 revolutions per minute.
(b) Use 900 mL of water, at a temperature of 37°, as the medium.
procedure

After 45 minutes withdraw a sample of the medium and measure the absorbance of the filtered sample, suitably diluted with the dissolution medium if necessary, at the maximum at 256 nm, Appendix II B using water in the reference cell.

determination of content

Calculate the total content of methylprednisolone, C22H30O5, in the medium taking 400 as the value of A (1%, 1 cm) at the maximum at 256 nm.

Related substances

Carry out the method for thin-layer chromatography, Appendix III A, using the following solutions.

(1) Shake a quantity of the powdered tablets containing 20 mg of Methylprednisolone for 15 minutes with 2 mL of a mixture of 1 volume of methanol and 9 volumes of chloroform, centrifuge and use the supernatant liquid.
(2) Dilute 1 volume of Solution (1) to 50 volumes with a mixture of 1 volume of methanol and 9 volumes of chloroform.
(3) Dilute 1 volume of solution (2) to 4 volumes with a mixture of 1 volume of methanol and 9 volumes of chloroform.
(4) For solution (4) dissolve 1 mg of hydrocortisone in a mixture of 0.1 mL of solution (1) and 0.9 mL of methanol.
chromatographic conditions
(a) Use as the coating silica gel F254 (Merck silica gel F254 plates are suitable).
(b) Use the mobile phase as described below.
(c) Apply 5 µL of each solution.
(d) Develop the plate to 15 cm.
(e) After removal of the plate, dry in air and examine under ultraviolet light (254 nm).
mobile phase

1.2 volumes of water, 8 volumes of methanol, 15 volumes of ether and 77 volumes of dichloromethane.

system suitability

The test is not valid unless the chromatogram obtained with solution (4) shows two principal spots that are close together but separated.

limits

Any secondary spot in the chromatogram obtained with solution (1) is not more intense than the spot in the chromatogram obtained with solution (2) (2%) and not more than one such spot is more intense than the spot in the chromatogram obtained with solution (3) (0.5%).

Assay

Weigh and powder 20 tablets. Suspend a quantity of the powder containing 10 mg of Methylprednisolone in 10 mL of water and extract with successive quantities of 100, 50, 50 and 40 mL of chloroform. Wash each extract with the same 10 mL quantity of water, filter and dilute the combined filtrates to 250 mL with chloroform. Evaporate 25 mL just to dryness, dissolve the residue in sufficient aldehyde-free ethanol (96%) to produce a solution containing between 390 and 410 µg of Methylprednisolone in 10 mL and complete the tetrazolium assay of steroids, Appendix VIII J, beginning at the words ‘Transfer 10 mL…’.

Dissolve a quantity of methylprednisolone BPCRS in sufficient aldehyde-free ethanol (96%) to produce a solution containing between 390 and 410 µg in 10 mL and complete the tetrazolium assay beginning at the words ‘Transfer 10 mL…’. From the absorbances so obtained, and using the declared content of C22H30O5 in methylprednisolone BPCRS, calculate the content of C22H30O5 in the tablets.

Storage

Methylprednisolone Tablets should be stored protected from light.