Glyburide Tablets
» Glyburide Tablets contain not less than 90.0 percent and not more than 110.0 percent of the labeled amount of glyburide (C23H28ClN3O5S).
Packaging and storage
Preserve in well-closed containers. Store at controlled room temperature.
Labeling
When more than one Dissolution test is given, the labeling states the Dissolution test used only if Test 1 is not used.
Identification, Infrared Absorption 197K
Prepare the test specimen as follows. Grind to a fine powder a number of Tablets, equivalent to about 15 mg of glyburide, add 30 mL of acetonitrile, and shake. Filter the mixture, evaporate the filtrate to dryness, and dry the residue in vacuum at 60 for 3 hours.
Dissolution 711
test 1
Medium:
0.05 M phosphate buffer, pH 9.5; 500 mL.
Apparatus 2:
75 rpm.
Time:
45 minutes.
Determine the percentage of the labeled amount of C23H28ClN3O5S dissolved using the following method. [noteUse low-actinic volumetric flasks.]
Mobile phase
Prepare a filtered and degassed mixture of water and acetonitrile (1:1), and add 4.0 mL of phosphoric acid per L of solution. Make adjustments if necessary (see System Suitability under Chromatography 621).
Standard stock solution
Transfer about 15 mg of USP Glyburide RS, accurately weighed, to a 100-mL volumetric flask, dissolve in Medium with sonication until dissolved, about 25 minutes, and dilute with Medium to volume.
Standard solutions
Dilute the Standard stock solution quantitatively, and stepwise if necessary, with Medium to obtain solutions having known concentrations of 0.003 mg per mL (for Tablets labeled to contain 1.5 mg), 0.006 mg per mL (for Tablets labeled to contain 3.0 mg), 0.009 mg per mL (for Tablets labeled to contain 4.5 mg), and 0.012 mg per mL (for Tablets labeled to contain 6.0 mg).
Test solution
Pass a portion of the solution under test through a suitable 0.45-µm filter.
Chromatographic system (see Chromatography 621)
The liquid chromatograph is equipped with a 215-nm detector and a 4.6-mm × 30-cm column that contains 10-µm packing L1. The flow rate is about 2.0 mL per minute. Chromatograph the Standard solution, and record the peak responses as directed for Procedure: the column efficiency is not less than 4000 theoretical plates; the tailing factor is not more than 2.0; and the relative standard deviation for replicate injections is not more than 3.0%.
Procedure
Separately inject equal volumes (about 50 µL) of the Standard solution and the Test solution into the chromatograph, record the chromatograms, and measure the responses for the major peaks. Determine the amount, in percentage, of C23H28ClN3O5S dissolved by the formula:
in which rU and rS are the peak responses obtained from the Test solution and the Standard solution, respectively; CS is the concentration, in mg per mL, of the Standard solution; 500 is the volume, in mL, of Medium; 100 is the conversion factor to percentage; and LC is the Tablet label claim, in mg.
Tolerances
Not less than 70% (Q) of the labeled amount of C23H28ClN3O5S is dissolved in 45 minutes.
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 8.5; 900 mL.
Apparatus 2:
50 rpm.
Time:
60 minutes.
Determine the percentage of the labeled amount of C23H28ClN3O5S dissolved using the following method.
Mobile phase
Prepare a filtered and degassed mixture of 520 mL of water containing 2.6 g of monobasic ammonium phosphate and 480 mL of acetonitrile. Make adjustments if necessary (see System Suitability under Chromatography 621).
Standard stock solution
Transfer about 67 mg of USP Glyburide RS, accurately weighed, to a 500-mL volumetric flask, dissolve in 40 mL of methanol with sonication for 5 minutes, and dilute with Medium to volume.
Standard solutions
Dilute the Standard stock solution quantitatively, and stepwise if necessary, with Medium to obtain solutions having known concentrations of 0.0017 mg per mL (for Tablets labeled to contain 1.5 mg), 0.0034 mg per mL (for Tablets labeled to contain 3 mg), 0.0047 mg per mL (for Tablets labeled to contain 4.5 mg), and 0.0067 mg per mL (for Tablets labeled to contain 6 mg).
Test solution
Pass a portion of the solution under test through a suitable 0.5-µm filter.
Chromatographic system
The liquid chromatograph is equipped with a 215-nm detector and a 4.0-mm × 25-cm column that contains 10-µm packing L7. The flow rate is about 1.5 mL per minute. Chromatograph the Standard solution, and record the peak responses as directed for Procedure: the tailing factor is not more than 2.0; and the relative standard deviation for replicate injections is not more than 2.0%.
Procedure
Separately inject equal volumes (about 50 µL) of the Standard solution and the Test solution into the chromatograph, record the chromatograms, and measure the responses for the major peaks. Determine the amount, in percentage, of C23H28ClN3O5S dissolved by the formula:
in which rU and rS are the peak responses obtained from the Test solution and the Standard solution, respectively; CS is the concentration, in mg per mL, of the Standard solution; 900 is the volume, in mL, of Medium; 100 is the conversion factor to percentage; and LC is the Tablet label claim, in mg.
Tolerances
Not less than 60% (Q) of the labeled amount of C23H28ClN3O5S is dissolved in 60 minutes.
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 7.5; 900 mL.
Apparatus 2:
50 rpm.
Time:
45 minutes.
Determine the percentage of the labeled amount of C23H28ClN3O5S dissolved using the following method.
Mobile phase
Proceed as directed for the Assay.
Diluent
Prepare a mixture of acetonitrile and water (5:1).
Standard solution
Transfer about 66.6 mg of USP Glyburide RS, accurately weighed, to a 100-mL volumetric flask, and dissolve in and dilute with Diluent to volume. Transfer 10.0 mL of this solution to a 100-mL volumetric flask, and dilute with Medium to volume. Transfer 10.0 mL of this solution to a 100-mL volumetric flask, and dilute with Medium to volume.
Test solution
Pass a portion of the solution under test through a suitable 0.45-µm filter.
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 2 mL per minute. Chromatograph the Standard solution, 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 75 µL) of the Standard solution and the Test solution into the chromatograph, record the chromatograms, and measure the responses for the major peaks. Determine the amount, in percentage, of C23H28ClN3O5S dissolved by the formula:
in which rU and rS are the peak responses obtained from the Test solution and the Standard solution, respectively; CS is the concentration, in mg per mL, of the Standard solution; 900 is the volume, in mL, of Medium; 100 is the conversion factor to percentage; and LC is the Tablet label claim, in mg.
Tolerances
Not less than 70% (Q) of the labeled amount of C23H28ClN3O5S is dissolved in 45 minutes.
Assay
System suitability preparation
Prepare a solution of progesterone in acetonitrile having a known concentration of about 0.2 mg per mL (Solution A). Transfer about 10 mg of USP Glyburide RS, accurately weighed, to a suitable container, add 20.0 mL of Solution A, and shake vigorously to dissolve. Add 4.0 mL of water, and mix.
Standard preparation
To about 10 mg of USP Glyburide RS, accurately weighed, add 20.0 mL of acetonitrile, and shake vigorously to dissolve. Add 4.0 mL of water, and mix.
Assay preparation
Transfer not fewer than 20 Tablets to a suitable container, add water equivalent to 0.4 mL of water per mg of glyburide, and swirl to disperse and wet Tablet material. Then add acetonitrile equivalent to 2.0 mL of acetonitrile per mg of glyburide, and shake for 30 minutes. Centrifuge a portion of the suspension so obtained, and use the clear supernatant.
Chromatographic system
Proceed as directed in the Assay for Glyburide, except to use the System suitability preparation in place of the Standard preparation.
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 height of the major peaks. Calculate the quantity, in mg, of glyburide (C23 H28ClN3O5S) in the portion of Tablets taken by the formula:
WS (rU / rS)
in which WS is the weight, in mg, of USP Glyburide RS taken to prepare the Standard preparation; and rU and rS are the glyburide peak heights 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 2510
Pharmacopeial Forum: Volume No. 33(4) Page 651
Chromatographic columns text is not derived from, and not part of, USP 32 or NF 27.
|