(klor proe' pa mide).
» Chlorpropamide contains not less than 97.0 percent and not more than 103.0 percent of C10H13ClN2O3S, calculated on the dried basis.
Packaging and storage Preserve in well-closed containers.
USP Reference standards 11
B: It responds to the Thin-Layer Chromatographic Identification Test 201. Prepare the test solution by dissolving an accurately weighed quantity of Chlorpropamide in acetone to obtain a solution containing 1 mg per mL. Develop the chromatogram in a solvent system consisting of a mixture of methylene chloride, methanol, cyclohexane, and ammonium hydroxide (100:50:30:10).
Melting range 741: between 126 and 129.
Loss on drying 731 Dry it in vacuum at 60 for 2 hours: it loses not more than 1.0% of its weight.
Residue on ignition 281: not more than 0.4%.
Selenium 291: 0.003%.
Heavy metals, Method II 231: 0.003%.
Mobile phase Prepare a filtered and degassed mixture of equal volumes of acetonitrile and dilute glacial acetic acid (1 in 100). [noteDo not exceed 50% of acetonitrile. ] Make adjustments if necessary (see System Suitability under Chromatography 621).
Standard preparation Dissolve an accurately weighed quantity of USP Chlorpropamide RS in Mobile phase, and dilute quantitatively, and stepwise if necessary, with Mobile phase to obtain a solution having a known concentration of about 0.05 mg per mL.
Assay preparation Transfer about 50 mg of Chlorpropamide, accurately weighed, to a 100-mL volumetric flask, add Mobile phase to volume, and mix. Transfer 10 mL of this solution to a second 100-mL volumetric flask, add Mobile phase to volume, and mix.
Chromatographic system (see Chromatography 621)The liquid chromatograph is equipped with a 240-nm detector and a 4.6-mm × 25-cm column that contains packing L1. The flow rate is about 1.5 mL per minute. Chromatograph the Standard preparation, and record the peak responses as directed under Procedure: the tailing factor for the analyte peak is not more than 1.5, and the relative standard deviation 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 responses for the major peaks. Calculate the quantity, in mg, of C10H13ClN2O3S in the portion of Chlorpropamide taken by the formula:
1000C(rU / rS)in which C is the concentration, in mg per mL, of USP Chlorpropamide RS in the Standard preparation, and rU and rS are the peak responses obtained from the Assay preparation and the Standard preparation, respectively.
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USP35NF30 Page 2645