(eye'' soe floo' pre done as' e tate).
» Isoflupredone Acetate contains not less than 97.0 percent and not more than 103.0 percent of C23H29FO6, calculated on the dried basis.
Packaging and storage Preserve in well-closed, light-resistant containers.
Labeling Label it to indicate that it is intended for veterinary use only. Where it is intended for use in preparing injectable dosage forms, the label states that it is sterile or must be subjected to further processing during the preparation of injectable dosage forms.
USP Reference standards 11
USP Prednisolone Acetate RS
Test preparation: 25 mg in 2000 mL of alcohol.
Procedure Proceed as directed under Spectrophotometry and Light-Scattering 851, and measure the absorbance at 240 nm: the absorptivity is between 35.0 and 38.0.
Specific rotation 781S: between +110 and +120.
Test solution: 10 mg per mL, in dioxane.
Bacterial endotoxins 85 Where the label states that Isoflupredone Acetate is sterile or that it must be subjected to further processing during the preparation of injectable dosage forms, it contains not more than 125 USP Endotoxin Units per mg of isoflupredone acetate.
Loss on drying 731 Dry it at 105 for 4 hours: it loses not more than 1.0% of its weight.
Residue on ignition 281: not more than 0.5%.
Solution A Prepare a mixture of water, methanol, acetonitrile, and glacial acetic acid (500:350:150:3), and degas.
Solution B Prepare a mixture of acetonitrile, methanol, and water (550:500:3), and degas.
Mobile phase Use variable mixtures of Solution A and Solution B as directed for Chromatographic system. Make adjustments if necessary (see System Suitability under Chromatography 621).
System suitability solution Dissolve accurately weighed quantities of USP Isoflupredone Acetate RS and USP Prednisolone Acetate RS in Solution A to obtain a solution having known concentrations of about 0.03 mg of each per mL. Sonicate, if necessary, to dissolve.
Test solution Dissolve an accurately weighed quantity of Isoflupredone Acetate in Solution A to obtain a solution having a concentration of about 0.3 mg per mL. Sonicate, if necessary, to dissolve. Use this solution within 16 hours.
Chromatographic system (see Chromatography 621) The liquid chromatograph is equipped with a 254-nm detector and a 4.6-mm × 25-cm column that contains packing L7. The flow rate is about 1 mL per minute. Protect the column from temperature fluctuations. The chromatograph is programmed as follows.
Procedure Inject a volume (about 50 µL) of the Test solution into the chromatograph, record the chromatogram, and measure the areas for the major peaks. Calculate the percentage of each impurity in the portion of Isoflupredone Acetate taken by the formula:
100(ri / rs)in which ri is the peak response for each impurity; and rs is the sum of the responses of all the peaks: not more than 1.0% of any individual impurity is found; and not more than 2.0% of total impurities is found, excluding those that are present in amounts less than 0.05%.
Other requirements Where the label states that it is sterile, it meets the requirements for Sterility Tests 71 when tested as directed for Direct Transfer Method under Test Procedures.
Mobile phase Prepare a mixture of n-butyl chloride, water-saturated n-butyl chloride, tetrahydrofuran, methanol, and glacial acetic acid (475:475:70:35:30). Make adjustments if necessary (see System Suitability under Chromatography 621).
Diluent Use water-saturated chloroform.
Internal standard solution Dissolve an accurately weighed quantity of fluoxymesterone in Diluent to obtain a solution having a known concentration of about 0.9 mg per mL.
Standard preparation Dissolve about 4 mg of USP Isoflupredone Acetate RS, accurately weighed, in 8.0 mL of Internal standard solution and 32.0 mL of Diluent.
Assay preparation Transfer about 4 mg of Isoflupredone Acetate, accurately weighed, to a suitable container. Dissolve in 8.0 mL of Internal standard solution and 32.0 mL of Diluent, centrifuge, and use the clear chloroform portion.
Chromatographic system (see Chromatography 621) The liquid chromatograph is equipped with a 254-nm detector and a 4-mm × 30-cm column that contains packing L3. The flow rate is about 0.7 mL per minute. Chromatograph the Standard preparation, and record the peak areas as directed for Procedure: the relative retention times are about 1.0 for isoflupredone acetate and 1.2 for fluoxymesterone; the resolution, R, between isoflupredone acetate and fluoxymesterone is not less than 2.0; and the relative standard deviation for replicate injections is not more than 2.0%.
Procedure Separately inject equal volumes (about 12 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the areas for the major peaks. Calculate the quantity, in mg, of C23H29FO6 in the portion of Isoflupredone Acetate taken by the formula:
WS(RU / RS)in which WS is the weight, in mg, of USP Isoflupredone Acetate RS taken to prepare the Standard preparation; and RU and RS are the peak area ratios of isoflupredone acetate to fluoxymesterone obtained from the Assay preparation and the Standard preparation, respectively.
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USP35NF30 Page 3568Pharmacopeial Forum: Volume No. 27(4) Page 2749