Etodolac Extended-Release Tablets
» Etodolac Extended-Release Tablets contain not less than 90.0 percent and not more than 110.0 percent of the labeled amount of etodolac (C17H21NO3).
Packaging and storage
Preserve in well-closed containers. Store at controlled room temperature, protected 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
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.
Dissolution 711
test 1
Medium:
0.05 M phosphate buffer, pH 7.4; 1000 mL.
Apparatus 2:
75 rpm, with USP sinker.
Times:
3, 6, 10, and 16 hours.
Procedure
Determine the amount of C17H21NO3 dissolved by employing UV absorption at the wavelength of maximum absorbance at about 279 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 Etodolac RS in the same Medium. Use Medium as the blank.
Tolerances
The percentages of the labeled amount of C17H21NO3 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:
0.05 M phosphate buffer, pH 7.5; 1000 mL.
Apparatus 2:
100 rpm.
Times:
2, 4, 8, and 14 hours.
Procedure
Determine the amount of C17H21NO3 dissolved by comparing the difference between the absorbances of the filtered portions of the solution under test determined at 278 nm and 245 nm with the difference between the absorbances of a Standard solution having a known concentration of USP Etodolac RS in the same Medium determined at the same wavelengths. Use Medium as the blank, and use a 0.05-cm silica cell.
Tolerances
The percentages of the labeled amount of C17H21NO3 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:
0.05 M phosphate buffer, pH 6.8; 1000 mL.
Apparatus 2:
75 rpm.
Times:
2, 4, 8, and 14 hours.
Procedure
Determine the amount of C17H21NO3 dissolved by employing UV absorption at the wavelength of maximum absorbance at about 278 nm on portions of the solution under test passed through a 10-µm polyethylene filter, suitably diluted with Medium, if necessary, in comparison with a Standard solution having a known concentration of USP Etodolac RS in the same Medium. Use Medium as the blank, and use a 0.05-cm silica cell.
Tolerances
The percentages of the labeled amount of C17H21NO3 dissolved at the times specified conform to Acceptance Table 2.
Uniformity of dosage units 905:
meet the requirements.
Chromatographic purity
Diluent, Mobile phase, and System suitability solution
Proceed as directed in the Assay.
Test solution
Use the Assay preparation.
Chromatographic system
Prepare as directed in the Assay. Chromatograph the System suitability solution, and record the peak responses as directed for Procedure: the relative retention times are about 0.8 for etodolac related compound A and 1.0 for etodolac; the resolution, R, between etodolac related compound A and etodolac is not less than 2.5; and the relative standard deviation for replicate injections is not more than 2.0%.
Procedure
Inject a volume (about 10 µL) of the Test solution into the chromatograph, record the chromatogram, and measure all of the peak areas. Calculate the percentage of each impurity in the portion of Tablets taken by the formula:
100(ri / rs)
in which ri is the peak area for each impurity, and rS is the sum of the areas of all the peaks: not more than 0.2% of any individual impurity is found; and not more than 0.75% of total impurities is found.
Assay
Diluent
Use acetonitrile.
Mobile phase
Prepare a filtered and degassed mixture of acetonitrile, water, and phosphoric acid (500:500:0.25). Make adjustments if necessary (see System Suitability under Chromatography 621).
System suitability solution
Dissolve accurately weighed quantities of USP Etodolac RS and USP Etodolac Related Compound A RS in Diluent, and quantitatively dilute with Diluent to obtain a solution having known concentrations of about 0.48 mg per mL and 0.05 mg per mL, respectively.
Standard preparation
Dissolve an accurately weighed quantity of USP Etodolac RS in Diluent, and quantitatively dilute with Diluent to obtain a solution having a known concentration of about 0.6 mg per mL.
Assay preparation
[noteDo not finely powder Tablets.] Weigh and powder not fewer than 20 Tablets, and transfer an accurately weighed portion of the powder, equivalent to about 600 mg of etodolac, to a 200-mL volumetric flask. Add about 100 mL of Diluent, mix, and shake for 40 minutes by mechanical means. Dilute with Diluent to volume, and mix. Pass through a filter having a 0.45-µm porosity, discarding the first 3 mL of the filtrate. Transfer 2.0 mL of the filtrate to a 10-mL volumetric flask, dilute with Diluent to volume, and mix.
Chromatographic system (see Chromatography 621)
The liquid chromatograph is equipped with a 274-nm detector, a 4.0-mm × 4.0-cm guard column that contains 5-µm packing L1, and a 4.0-mm × 25-cm column that contains 5-µm packing L1. The flow rate is about 1 mL per minute. Chromatograph the System suitability solution, and record the peak responses as directed for Procedure: the relative retention times are about 0.8 for etodolac related compound A and 1.0 for etodolac; the resolution, R, between etodolac related compound A and etodolac is not less than 2.5; and the tailing factor is not more than 2.0. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: 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. Calculate the quantity, in mg, of etodolac (C17H21NO3) in the portion of Tablets taken by the formula:
1000C(rU / rS)
in which C is the concentration, in mg per mL, of USP Etodolac RS in the Standard preparation; and rU and rS are the 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 2336
Pharmacopeial Forum: Volume No. 31(4) Page 1068
Chromatographic columns text is not derived from, and not part of, USP 32 or NF 27.
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