Diclofenac Sodium Extended-Release Tablets
» Diclofenac Sodium Extended-Release Tablets contain not less than 90.0 percent and not more than 110.0 percent of the labeled amount of diclofenac sodium (C14H10Cl2NNaO2).
Packaging and storage
Preserve in well-closed containers. Store at controlled room temperature, and protect from light.
Labeling
When more than one Dissolution Test is given, the labeling states the Dissolution Test used only if Test 1 is not used.
Identification
A:
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.
B: Thin-Layer Chromatographic Identification Test 201
Solvent system:
methanol, toluene, glacial acetic acid (40:60:0.5).
Test solution
Finely powder not fewer than 10 Tablets. Accurately weigh a portion of the powder, equivalent to about 50 mg of diclofenac sodium, and transfer to a 25-mL volumetric flask. Add about 15 mL of methanol, sonicate for 10 minutes, shake by mechanical means for 10 minutes, dilute with methanol to volume, and mix. Centrifuge this solution, and use the clear supernatant as the Test solution.
Standard solution
Accurately weigh about 50 mg of USP Diclofenac Sodium RS into a 25-mL volumetric flask. Add 10 mL of methanol, shake by mechanical means for 10 minutes, dilute with methanol to volume, and mix.
Dissolution 711
test 1
Medium:
0.05 M phosphate buffer, pH 7.5; 900 mL.
Apparatus 2:
50 rpm; use wire sinkers.
Times:
1, 5, 10, 16, and 24 hours.
Procedure
Determine the amount of C14H10Cl2NNaO2 dissolved by employing UV absorption at the wavelength of maximum absorbance at about 276 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 Diclofenac Sodium RS in the same Medium.
Tolerances
The percentages of the labeled amount of C14H10Cl2NNaO2 dissolved at the times specified conform to Acceptance Table 2.
test 2
If the product complies with this test, the labeling indicates that it meets USP Dissolution Test 2.
Medium, Apparatus, and Procedure
Proceed as directed for Test 1.
Times:
1, 2, 4, 6, and 10 hours.
Tolerances
The percentages of the labeled amount of C14H10Cl2NNaO2 dissolved at the times specified conform to Acceptance Table 2.
test 3
If the product complies with this test, the labeling indicates that it meets USP Dissolution Test 3.
Medium and Procedure
Proceed as directed for Test 1.
Apparatus 1:
100 rpm.
Times:
2, 4, 8, and 16 hours.
Tolerances
The percentages of the labeled amount of C14H10Cl2NNaO2 dissolved at the times specified conform to Acceptance Table 2.
Uniformity of dosage units 905:
meet the requirements.
Assay
[noteProtect the Assay preparation, Standard preparation, and System suitability solution from light.]
Diluent:
a mixture of acetonitrile and water (43:57).
0.05 M Monobasic potassium phosphate buffer
Dissolve 6.8 g of monobasic potassium phosphate in 950 mL of water, adjust with dilute phosphoric acid or dilute potassium hydroxide solution to a pH of 4.0 ± 0.05, dilute with water to 1 L, and mix.
Mobile phase
Prepare a filtered and degassed mixture of acetonitrile, 0.05 M Monobasic potassium phosphate buffer, and tetrahydrofuran (43:57:2). Make adjustments if necessary (see System Suitability under Chromatography 621).
Diclofenac related compound A solution
Dissolve an accurately weighed quantity of USP Diclofenac Related Compound A RS in Diluent, and quantitatively dilute with Diluent to obtain a solution having a known concentration of about 200 µg per mL.
Standard preparation
Dissolve an accurately weighed quantity of USP Diclofenac Sodium RS in Diluent, and quantitatively dilute with Diluent to obtain a solution having a known concentration of about 200 µg per mL.
System suitability solution
Transfer 10 mL of the Standard preparation and 5 mL of Diclofenac related compound A solution to a 20-mL volumetric flask. Dilute with Diluent to volume, and mix.
Assay preparation
Powder not fewer than 20 Tablets, and transfer an accurately weighed portion of the powder, equivalent to about 100 mg of diclofenac sodium, to a 100-mL volumetric flask, add about 50 mL of Diluent, sonicate for about 15 minutes, then shake by mechanical means for 15 minutes. Add a few drops of methanol to remove the foam, dilute with Diluent to volume, and mix. Transfer 10.0 mL of the supernatant to a 50-mL volumetric flask, dilute with Diluent to volume, and mix.
Chromatographic system (see Chromatography 621)
The liquid chromatograph is equipped with a 254-nm detector and a 4.6-mm × 15-cm column that contains 5-µm packing L1. The flow rate is about 1.5 mL per minute. Inject 40 µL of the System suitability solution into the chromatograph, and record the peak responses as directed for Procedure: the relative retention times are about 0.9 for diclofenac related compound A and 1.0 for diclofenac; and the resolution, R, between the diclofenac peak and the diclofenac related compound A peak is not less than 2.0. Inject 20 µL of the Standard preparation into the chromatograph, and record the peak responses as directed for Procedure: the tailing factor of the diclofenac peak is not more than 2.0; and the relative standard deviation of the diclofenac peak for replicate injections is not more than 2.0%.
Procedure
Separately inject equal volumes (about 20 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the area responses for the major peaks. Calculate the quantity, in mg, of diclofenac sodium (C14H10Cl2NNaO2) in the portion of Tablets taken by the formula:
500C(rU / rS)
in which C is the concentration, in mg per mL, of USP Diclofenac Sodium RS in the Standard preparation; and rU and rS are the diclofenac peak responses obtained from the Assay preparation and the Standard preparation, respectively.
Auxiliary Information
Please check for your question in the FAQs before contacting USP.
Chromatographic Column
USP32NF27 Page 2125
Pharmacopeial Forum: Volume No. 33(2) Page 218
Chromatographic columns text is not derived from, and not part of, USP 32 or NF 27.
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