Methylprednisolone
(meth'' il pred nis' oh lone).
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374.48Pregna-1,4-diene-3,20-dione, 11,17,21-trihydroxy-6-methyl-, (6
,11
)-.
11
,17,21-Trihydroxy-6-methylpregna-1,4-diene-3,20-dione
[83-43-2].» Methylprednisolone contains not less than 97.0 percent and not more than 103.0 percent of C22H30O5, calculated on the dried basis.
Packaging and storage—
Preserve in tight, light-resistant containers.
USP Reference standards 
11
—
11—
USP Methylprednisolone RS 
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Identification—
B:
Ultraviolet Absorption 197U—
197U—
Solution:
10 µg per mL.
Medium:
alcohol.
Absorptivities at 243 nm, calculated on the dried basis, do not differ by more than 3.0%.
C:
Dissolve about 5 mg in 2 mL of sulfuric acid: a red color is produced.
Loss on drying 731—
Dry it at 105
for 3 hours: it loses not more than 1.0% of its weight.
731—
Dry it at 105 for 3 hours: it loses not more than 1.0% of its weight.
Residue on ignition 281:
not more than 0.2%.
281:
not more than 0.2%.
Chromatographic purity—
Mobile phase—
Prepare a filtered and degassed mixture of water, tetrahydrofuran, dimethyl sulfoxide, and butanol (149:40:10:1). Make adjustments if necessary (see System Suitability in Chromatography 621).
621).
Diluting solution—
Prepare a filtered mixture of water, tetrahydrofuran, and glacial acetic acid (72:25:3).
Standard solution—
Dissolve an accurately weighed quantity of USP Methylprednisolone RS in Diluting solution. Dilute quantitatively, and stepwise if necessary, with Diluting solution to obtain a solution having a known concentration of about 0.01 mg per mL.
Test solution—
Transfer about 25 mg of Methylprednisolone, accurately weighed, to a 25-mL volumetric flask, dissolve in and dilute with Diluting solution to volume, and mix.
Chromatographic system
(see Chromatography 621)—The liquid chromatograph is equipped with a 254-nm detector and a 4.6-mm × 20-cm column that contains packing L1. The flow rate is about 1 mL per minute. Chromatograph the Standard solution, and record the peak responses as directed for Procedure: the column efficiency is not less than 800 theoretical plates; and the relative standard deviation for replicate injections is not more than 5.0%.
621)—The liquid chromatograph is equipped with a 254-nm detector and a 4.6-mm × 20-cm column that contains packing L1. The flow rate is about 1 mL per minute. Chromatograph the Standard solution, and record the peak responses as directed for Procedure: the column efficiency is not less than 800 theoretical plates; and the relative standard deviation for replicate injections is not more than 5.0%.
Procedure—
Separately inject equal volumes (about 10 µL) of the Standard solution and the Test solution into the chromatograph, record the chromatograms, and measure the peak responses. Calculate the percentage of each impurity in the portion of Methylprednisolone taken by the formula:
100(CS / CU)(ri / rS)
in which CS and CU are the concentrations, in mg per mL, of Methylprednisolone in the Standard solution and the Test solution, respectively; ri is the peak response for each impurity obtained from the Test solution; and rS is the peak response for methylprednisolone in the Standard solution: not more than 1.0% of any individual impurity is found, and not more than 2.0% of total impurities is found.
Assay—
Mobile phase—
Prepare a solution containing a mixture of butyl chloride, water-saturated butyl chloride, tetrahydrofuran, methanol, and glacial acetic acid (475:475:70:35:30).
Internal standard solution—
Dissolve prednisone in a 3 in 100 solution of glacial acetic acid in chloroform to obtain a solution having a concentration of about 0.2 mg per mL.
Standard preparation—
Dissolve an accurately weighed quantity of USP Methylprednisolone RS in Internal standard solution to obtain a solution having a known concentration of about 0.2 mg per mL.
Assay preparation—
Using about 10 mg of Methylprednisolone, accurately weighed, proceed as directed for Standard preparation.
Chromatographic system
(see Chromatography )—The liquid chromatograph is equipped with a 254-nm detector and a 4-mm × 25-cm column that contains packing L3. The flow rate is about 1 mL per minute. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the resolution, R, between the methylprednisolone and internal standard peaks is not less than 4.0; and the relative standard deviation for 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: the relative retention times are about 0.7 for prednisone and 1.0 for methylprednisolone. Calculate the quantity, in percent, of C22H30O5 in the portion of Methylprednisolone taken by the formula:
100(CS / CU)(RU / RS)
in which CS is the concentration of methylprednisolone, in mg per mL, in the Standard preparation; CU is the nominal concentration, in mg per mL, of Methylprednisolone in the Assay preparation; and RU and RS are the ratios of the peak responses for the methylprednisolone peak and 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.
| Topic/Question | Contact | Expert Committee |
|---|---|---|
| Monograph | Mary S. Waddell
Scientific Liaison 1-301-816-8124 |
(SM42010) Monographs - Small Molecules 4 |
| Reference Standards | RS Technical Services 1-301-816-8129 rstech@usp.org |
USP35–NF30 Page 3884
Pharmacopeial Forum: Volume No. 33(6) Page 1189