Methsuximide
2,5-Pyrrolidinedione, 1,3-dimethyl-3-phenyl-, (±)-. (±)-N,2-Dimethyl-2-phenylsuccinimide [77-41-8]. » Methsuximide contains not less than 97.0 percent and not more than 103.0 percent of C12H13NO2, calculated on the dried basis.
Packaging and storage
Preserve in tight containers.
Identification
Melting range 741:
between 50 and 56, determined by a Class I procedure, except that the test specimen is inserted into the bath at about room temperature.
Loss on drying 731
Dry it over phosphorus pentoxide for 16 hours: it loses not more than 0.5% of its weight.
Residue on ignition 281:
not more than 0.2%.
Limit of cyanide
Dissolve 1.0 g in 10 mL of alcohol, and add 3 drops of ferrous sulfate TS, 1 mL of 1 N sodium hydroxide, and a few drops of ferric chloride TS. Warm gently, and finally acidify with 2 N sulfuric acid: no blue precipitate or blue color develops within 15 minutes.
Chromatographic purity
Mobile phase
and Chromatographic systemProceed as directed in the Assay. To evaluate the system suitability requirements, use the Standard preparation as prepared in the Assay.
Standard solution
Dissolve an accurately weighed quantity of USP Methsuximide RS in Mobile phase, and dilute quantitatively, and stepwise if necessary, with Mobile phase to obtain a solution having a known concentration of about 6.0 µg per mL.
Test solution
Transfer about 300 mg of Methsuximide, accurately weighed, to a 50-mL volumetric flask, dissolve in and dilute with Mobile phase to volume, and mix.
Procedure
Separately inject equal volumes (about 20 µL) of the Standard solution and the Test solution into the chromatograph, record the chromatograms, and measure all of the peak responses. Calculate the percentage of each impurity in the portion of Methsuximide taken by the formula:
0.1(CS / CU)(ri / rS)
in which CS is the concentration, in µg per mL, of USP Methsuximide RS in the Standard solution; CU is the concentration, in mg per mL, of Methsuximide in the Test solution; ri is the peak response for each impurity obtained from the Test solution; and rS is the peak response for methsuximide obtained from the Standard solution: not more than 0.1% of any individual impurity is found; and not more than 2.0% of total impurities is found.
Assay
Mobile phase
Prepare a filtered and degassed mixture of water and acetonitrile (11:9). Make adjustments if necessary (see System Suitability under Chromatography 621).
Standard preparation
Dissolve an accurately weighed quantity of USP Methsuximide RS in Mobile phase, and dilute quantitatively, and stepwise if necessary, with Mobile phase to obtain a solution having a known concentration of about 0.6 mg per mL.
Assay preparation
Transfer about 120 mg of Methsuximide, accurately weighed, to a 200-mL volumetric flask, dissolve in and dilute with Mobile phase to volume, and mix.
Chromatographic system
The liquid chromatograph is equipped with a 254-nm detector and a 3.9-mm × 30-cm column that contains packing L1. The flow rate is about 1 mL per minute. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the column efficiency is not less than 5800 theoretical plates; the tailing factor is not more than 1.3; and the relative standard deviation for replicate injections is not more than 0.6%.
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 C12H13NO2 in the portion of Methsuximide taken by the formula:
200CS(rU / rS)
in which CS is the concentration, in mg per mL, of USP Methsuximide 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
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Chromatographic Column
USP32NF27 Page 2935
Chromatographic columns text is not derived from, and not part of, USP 32 or NF 27.
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