» Hydrocortisone Tablets contain not less than 90.0 percent and not more than 110.0 percent of the labeled amount of hydrocortisone (C21H30O5).
Packaging and storage Preserve in well-closed containers.
USP Reference standards 11
Identification Powder a number of Tablets, equivalent to about 50 mg of hydrocortisone, and digest with 15 mL of solvent hexane for 15 minutes. Decant the solvent hexane as completely as possible, and extract the residue first with 10 mL of solvent hexane, then with 10 mL of peroxide-free ether in the same manner as before, and discard the extracts. Digest the final residue with 25 mL of dehydrated alcohol for 15 minutes with frequent agitation, filter, and evaporate the alcohol extract on a steam bath to dryness: the residue so obtained responds to Identification test A under Hydrocortisone.
Medium: water; 900 mL.
Apparatus 2: 50 rpm.
Time: 30 minutes.
Procedure Determine the amount of C21H30O5 dissolved from UV absorbances at the wavelength of maximum absorbance at about 248 nm on filtered portions of the solution under test, suitably diluted with Medium, if necessary, in comparison with a Standard solution having a known concentration of USP Hydrocortisone RS in the same Medium.
Tolerances Not less than 70% (Q) of the labeled amount of C21H30O5 is dissolved in 30 minutes.
Uniformity of dosage units 905: meet the requirements.
procedure for content uniformity
Mobile phase, Internal standard solution, and Standard preparation Prepare as directed in the Assay.
Test preparation Transfer 1 Tablet to a suitable container and add about 0.3 mL of water directly on the Tablet. Allow the Tablet to stand for about 5 minutes. Shake the container to break up the Tablet and sonicate briefly to ensure complete disintegration. Add a few small glass beads and 50.0 mL of Internal standard solution to the container. Shake the container for about 30 minutes. Dilute an accurately measured volume of the clear supernatant with a known, accurately measured volume of Internal standard solution to obtain a final concentration of 0.1 mg per mL. Shake the contents of the container to mix, and analyze the clear solution as directed for Procedure.
Chromatographic system and Procedure Proceed as directed in the Assay. Calculate the quantity, in mg, of C21H30O5 in the Tablet taken by the formula:
50(F2 / F1)C(RU / RS)in which F1 is the volume, in mL, of the supernatant aliquot of the solution from the Tablet taken for dilution; F2 is the final volume, in mL, of the Test preparation; and the other terms are as defined for Procedure in the Assay.
Mobile phase Prepare a solution containing a mixture of butyl chloride, water-saturated butyl chloride, tetrahydrofuran, methanol, and glacial acetic acid (95:95:14:7:6).
Internal standard solution Prepare a solution of USP Prednisone RS in water-saturated chloroform containing 0.06 mg per mL.
Standard preparation Dissolve an accurately weighed quantity of USP Hydrocortisone RS in Internal standard solution to obtain a solution having a known concentration of about 0.1 mg per mL.
Assay preparation Weigh and finely powder not fewer than 10 Tablets. Weigh a portion of the powder, equivalent to about 5 mg of hydrocortisone, and transfer to a suitable container. Add 50.0 mL of Internal standard solution. Shake vigorously for 30 minutes, and centrifuge a portion of this mixture. Use the clear supernatant.
Chromatographic system (see Chromatography 621) The liquid chromatograph is equipped with a 254-nm detector and a 3.9-mm × 30-cm column that contains packing L3. The flow rate is 0.9 mL per minute. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the resolution, R, between hydrocortisone and prednisone is not less than 3.0; and the relative standard deviation for four replicate injections is not more than 2.0%.
Procedure Separately inject equal volumes (about 10 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the responses for the major peaks. Calculate the quantity, in mg, of hydrocortisone (C21H30O5) in the portion of Tablets taken by the formula:
50C(RU / RS)in which C is the concentration, in mg per mL, of USP Hydrocortisone RS in the Standard preparation; and RU and RS are the peak response ratios of the hydrocortisone peak to the internal standard peak obtained from the Assay preparation and the Standard preparation, respectively.
Auxiliary Information Please check for your question in the FAQs before contacting USP.
USP35NF30 Page 3433Pharmacopeial Forum: Volume No. 33(1) Page 72