Methylprednisolone Sodium Succinate for Injection
» Methylprednisolone Sodium Succinate for Injection is a sterile mixture of Methylprednisolone Sodium Succinate with suitable buffers. It may be prepared from Methylprednisolone Sodium Succinate or from Methylprednisolone Hemisuccinate with the aid of Sodium Hydroxide or Sodium Carbonate. It contains the equivalent of not less than 90.0 percent and not more than 110.0 percent of the labeled amount of methylprednisolone (C22H30O5) in the volume of constituted solution designated on the label.
Packaging and storage Preserve in Containers for Sterile Solids as described under Injections 1.
USP Reference standards 11
USP Endotoxin RS
Constituted solution At the time of use, it meets the requirements for Constituted Solutions under Injections 1.
Identification It meets the requirements of Identification test A under Methylprednisolone Sodium Succinate.
Bacterial endotoxins 85 It contains not more than 0.17 USP Endotoxin Unit per mg of methylprednisolone.
pH 791: between 7.0 and 8.0, in a solution containing about 50 mg of methylprednisolone sodium succinate per mL.
Loss on drying 731 Dry it at 105 for 3 hours: it loses not more than 2.0% of its weight.
Particulate matter 788: meets the requirements for small-volume injections.
Free methylprednisolone Using the chromatograms obtained in the Assay, measure the areas of the peaks from the internal standard and free methylprednisolone. Calculate the ratio of the area of the free methylprednisolone peak to that of the internal standard in the chromatogram obtained from the Standard preparation, SS, and the same ratio in the chromatogram obtained from the Assay preparation, SU. Calculate the quantity, in mg, of free methylprednisolone in the Assay preparation taken by the formula:
100C(SU / SS)in which C is the concentration, in mg per mL, of USP Methylprednisolone RS in the Standard preparation; and SU and SS are the ratios as defined above. The amount of free methylprednisolone is not more than 6.6% of the labeled amount of methylprednisolone.
Other requirements It meets the requirements for Sterility Tests 71, Uniformity of Dosage Units 905, and Labeling under Injections 1.
Internal standard solution Prepare a solution of USP Fluorometholone RS in tetrahydrofuran containing about 3 mg per mL.
Mobile phase Prepare a filtered mixture of butyl chloride, water-saturated butyl chloride, tetrahydrofuran, methanol, and glacial acetic acid (95:95:14:7:6). Make adjustments if necessary (see System Suitability under Chromatography 621).
Standard preparation Weigh accurately about 32.5 mg of USP Methylprednisolone Hemisuccinate RS, and transfer it to a 50-mL volumetric flask. Add by pipet 5.0 mL of Internal standard solution and 5.0 mL of a solution of glacial acetic acid in chloroform (3 in 100) containing in each mL an accurately known quantity of about 0.30 mg of USP Methylprednisolone RS. Dilute with glacial acetic acid in chloroform (3 in 100) to volume, and mix.
Assay preparation Mix the constituted solutions prepared from the contents of 10 vials of Methylprednisolone Sodium Succinate for Injection. Transfer an accurately measured volume of the resulting constituted solution, equivalent to about 50 mg of methylprednisolone, to a suitable flask containing 10.0 mL of Internal standard solution, and dilute with glacial acetic acid in chloroform (3 in 100) to 100.0 mL. Shake thoroughly for 5 minutes, then allow the phases to separate, discarding the upper phase.
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 about 1.0 mL per minute. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the order of elution of peaks is the internal standard peak, methylprednisolone hemisuccinate peak, and successive smaller peaks of free methylprednisolone and methylprednisolone 17-hemisuccinate.
Procedure Separately inject equal volumes (about 6 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the peak areas for the internal standard, methylprednisolone hemisuccinate, and methylprednisolone 17-hemisuccinate. Calculate the quantity, in mg, of methylprednisolone (C22H30O5) in the portion of constituted solution taken by the formula:
0.789(100C)(RU / RS)in which 0.789 is the ratio of the molecular weight of methylprednisolone to that of methylprednisolone hemisuccinate; C is the concentration, in mg per mL, of USP Methylprednisolone Hemisuccinate RS in the Standard preparation; and RU and RS are the ratios of the sum of the peak areas for methylprednisolone hemisuccinate and methylprednisolone 17-hemisuccinate to the peak area of the internal standard obtained from the Standard preparation and the Assay preparation, respectively. To this quantity add the amount, in mg, of free methylprednisolone found in the test for Free methylprednisolone.
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USP35NF30 Page 3889