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Bicalutamide Tablets
» Bicalutamide Tablets contain not less than 90.0 percent and not more than 110.0 percent of the labeled amount of bicalutamide (C18H14F4N2O4S).
Packaging and storage— Preserve in tight containers. Store at controlled room temperature.
USP Reference standards 11
USP Bicalutamide RS
.
USP Bicalutamide Related Compound B RS.
Identification— The retention time of the major peak in the chromatogram of the Assay preparation corresponds to that in the chromatogram of the Standard preparation, as obtained in the Assay.
Uniformity of dosage units 905: meet the requirements.
procedure for content uniformity
1% Sodium lauryl sulfate solution— Dissolve 15 g of sodium lauryl sulfate in 1.5 L of water.
Standard solution— Dissolve an accurately weighed quantity of USP Bicalutamide RS in a minimum amount of tetrahydrofuran, and dilute quantitatively with 1% Sodium lauryl sulfate solution to obtain a solution having a known concentration of about 0.05 mg per mL.
Test solution— Transfer 1 Tablet to a 100-mL volumetric flask, add about 10 mL of water, and sonicate for approximately 30 minutes. Add about 80 mL of tetrahydrofuran, and sonicate for 30 minutes to complete dissolution of the bicalutamide. Allow to cool to room temperature, and dilute with tetrahydrofuran to volume. Pass this solution through a 0.45-µm suitable filter unit, transfer 10.0 mL of filtrate to a 100-mL volumetric flask, and dilute with 1% Sodium lauryl sulfate solution to volume.
Procedure— Concomitantly determine the UV absorbances of the Standard solution and the Test solution with a suitable spectrophotometer at 270 nm, using 1% Sodium lauryl sulfate solution as the blank. Calculate the quantity, in mg, of bicalutamide (C18H14F4N2O4S) in the Tablet taken by the formula:
1000C(AU / AS)
in which C is the concentration, in mg per mL, of USP Bicalutamide RS in the Standard solution; and AU and AS are the absorbances obtained from the Test solution and the Standard solution, respectively.
Limit of 4-amino-2-(trifluoromethyl)benzonitrile—
Mobile phase and System suitability solution— Proceed as directed in the Assay.
Standard solution— Dissolve an accurately weighed quantity of USP Bicalutamide RS in tetrahydrofuran to obtain a solution having a known concentration of about 0.2 mg per mL. Transfer 5.0 mL of this solution to a 50–mL volumetric flask, and dilute with Mobile phase to volume.
Test solution— Transfer an accurately weighed quantity of the powdered Tablet prepared in the Assay preparation, equivalent to about 50 mg of bicalutamide, to a 25-mL volumetric flask. Add about 2 mL of tetrahydrofuran, and allow to stand for 5 minutes. Add about 20 mL of Mobile phase, and sonicate for 10 minutes. Allow to cool to room temperature, and dilute with Mobile phase to volume. Pass the sample through a suitable 0.2-µm filter.
Chromatographic system (see Chromatography 621) Proceed as directed in the Assay, except to use a liquid chromatograph equipped with a 220-nm detector.
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 4-amino-2-(trifluoromethyl)benzonitrile in the portion of Tablets taken by the formula:
100(1/1.4)(CS / CU)(rU / rS)
in which 1.4 is the relative response factor for 4-amino-2-(trifluoromethyl)benzonitrile, CS is the concentration, in mg per mL, of USP Bicalutamide RS in the Standard solution; CU is the concentration, in mg per mL, of bicalutamide in the Test solution based on the label claim; rU is the peak area for 4-amino-2-(trifluoromethyl)benzonitrile obtained from the Test solution; and rS is the peak area for bicalutamide obtained from the Standard solution: not more than 0.1% of 4-amino-2-(trifluoromethyl)benzonitrile is found. [note—The relative retention time for 4-amino-2-(trifluoromethyl)benzonitrile is about 0.4.]
Assay—
Mobile phase— Prepare a mixture of water, tetrahydrofuran, and acetonitrile (65:20:15).
Standard preparation— Dissolve an accurately weighed quantity of USP Bicalutamide RS in tetrahydrofuran to obtain a solution having a known concentration of about 0.8 mg per mL. Transfer 5.0 mL of this solution to a 100-mL volumetric flask, and dilute with Mobile phase to volume.
Assay preparation— Grind not fewer than 20 Tablets to a fine powder. Transfer an accurately weighed quantity of powdered Tablets, equivalent to about 50 mg of bicalutamide, to a 100-mL volumetric flask. Add about 50 mL of tetrahydrofuran, and sonicate for at least 10 minutes to complete dissolution. Allow to cool to room temperature, and dilute with tetrahydrofuran to volume. Pass this solution through a suitable 0.45-µm filter. Transfer 4.0 mL of the filtrate to a 50-mL volumetric flask, and dilute with Mobile phase to volume.
System suitability solution— Dissolve suitable quantities of USP Bicalutamide RS and USP Bicalutamide Related Compound B RS in tetrahydrofuran to obtain a solution having known concentrations of about 0.8 mg of USP Bicalutamide RS per mL and 0.4 mg of USP Bicalutamide Related Compound B RS per mL. Transfer 5.0 mL of this solution to a 100-mL volumetric flask, and dilute with Mobile phase to volume.
Chromatographic system (see Chromatography 621) The liquid chromatograph is equipped with a 270-nm detector, and a 5-mm × 12.5-cm column that contains 3-µm packing L1. The flow rate is about 1.5 mL per minute. The column temperature is maintained at 50. Chromatograph the System suitability solution, and record the peak areas as directed for Procedure: the relative retention time for the bicalutamide related compound B peak is about 1.1; the resolution, R, between bicalutamide and bicalutamide related compound B is greater than 1.9; the tailing factor of the bicalutamide peak is less than 1.3; and the relative standard deviation for replicate injections calculated for the bicalutamide peak 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 areas for the bicalutamide peaks. Calculate the quantity, in percentage of the label claim, of bicalutamide (C18H14F4N2O4S) in the portion of Tablets taken by the formula:
100(CS / CU)(rU / rS)
in which CS is the concentration, in mg per mL, of USP Bicalutamide RS in the Standard preparation; CU is the concentration, in mg per mL, of bicalutamide in the Assay preparation based on the label claim; and rU and rS are the peak areas obtained from the Assay preparation and the Standard preparation, respectively.USP32
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Topic/Question Contact Expert Committee
Monograph Feiwen Mao, M.S.
Scientist
1-301-816-8320
(MDOOD05) Monograph Development-Ophthalmics Oncologics and Dermatologicals
Reference Standards Lili Wang, Technical Services Scientist
1-301-816-8129
RSTech@usp.org
USP32–NF27 Page 1674
Pharmacopeial Forum: Volume No. 34(5) Page 1147
Chromatographic Column—
Chromatographic columns text is not derived from, and not part of, USP 32 or NF 27.