Mephobarbital Tablets
»Mephobarbital Tablets contain not less than 95.0percent and not more than 110.0percent of the labeled amount of mephobarbital (C13H14N2O3).
Packaging and storage— Preserve in well-closed containers.
Identification— The mephobarbital obtained in the Assaymelts between 174and 181(see Melting Range or Temperature á741ñ)and meets the requirements for Identificationtest Aunder Mephobarbital.
Add the following:
Dissolution á711ñ
Medium: a 1%solution of 3-(dodecyldimethylammonio)propanesulfonate in pH8.0phosphate buffer (prepared by dissolving 10.0g of 3-(dodecyldimethylammonio)propanesulfonate in 400mLof warm water,and adding 250mLof 0.2Mmonobasic potassium phosphate and about 220mLof 0.2Msodium hydroxide;the solution is then cooled to room temperature,and adjusted with 0.2Msodium hydroxide to a pHof 8.0,followed by diluting with water to 1000mL,mixing,and degassing);900mL.
Apparatus 2: 75rpm.
Time: 75minutes.
Procedure— Determine the amount of C13H14N2O3dissolved by employing UVabsorption at the wavelength of maximum absorbance at about 244nm on portions of the solution under test passed through 0.45-µm nylon filters,suitably diluted with Dissolution Medium,if necessary,in comparison with a Standard solution having a known concentration of USP Mephobarbital RSin the same Medium.
Tolerances— Not less than 70%(Q)of the labeled amount of C13H14N2O3is dissolved in 75minutes.USP28
Uniformity of dosage units á905ñ: meet the requirements.
PROCEDURE FOR CONTENT UNIFORMITY—
Alkaline borate solution— Dissolve 6.2g of boric acid and 7.45g of potassium chloride in 500mLof water,add 210mLof sodium hydroxide solution (1in 25),and mix.Add water to make 2000mLof solution,and mix.
Standard solution— [NOTE—Prepare the Standard solution and the Test solution concomitantly.]Dissolve an accurately weighed quantity of USP Mephobarbital RSin Alkaline borate solutionto obtain a solution having a concentration of about 10mg per mL,and quantitatively dilute with water to obtain a solution having a known concentration of about 1.5mg per mL.
Test solution— Transfer 1Tablet to a glass-stoppered centrifuge tube,crush the tablet,and add 25.0mLof Alkaline borate solution.Insert the stopper,shake for 10minutes,and centrifuge until clear,filtering the supernatant,if necessary.Dilute a portion of the subsequent liquid quantitatively,and stepwise if necessary,with water to obtain a solution having a concentration of about 1.5mg of mephobarbital per mL.
Procedure— Transfer 3.0mLeach of the Standard solutionand the Test solutionto separate 200-mLvolumetric flasks,dilute each with a 1in 3solution of Alkaline borate solutionin water to volume,and mix.Concomitantly determine the absorbances of the solutions in 1-cm cells at the wavelength of maximum absorbance at about 245nm,with a suitable spectrophotometer,using a 1in 3solution of Alkaline borate solutionin water as the blank.Calculate the quantity,in mg,of C13H14N2O3in the Tablet taken by the formula:
(TC/D)(AU/AS),
in which Tis the labeled quantity,in mg,of mephobarbital in the Tablet;Cis the concentration,in mg per mL,of USP Mephobarbital RSin the Standard solution;Dis the concentration,in mg per mL,of mephobarbital in the Test solution,based upon the labeled quantity per Tablet and the extent of dilution;and AUand ASare the absorbances of the solutions from the Test solutionand the Standard solution,respectively.
Assay— Weigh and finely powder not fewer than 20Tablets.Transfer an accurately weighed portion of the powder,equivalent to about 300mg of mephobarbital,to an extraction thimble.Extract with 15mLof solvent hexane,allow the thimble to drain,transfer to a continuous-extraction apparatus provided with a tared flask,and extract the mephobarbital with chloroform for 2hours.Evaporate the chloroform on a steam bath with the aid of a current of air,cool,dissolve the residue in about 10mLof alcohol,evaporate,dry the residue at 105for 1hour,cool,and weigh.The weight of the residue represents the weight of mephobarbital (C13H14N2O3)in the portion of Tablets taken.
Auxiliary Information— Staff Liaison:Ravi Ravichandran,Ph.D.,Senior Scientist
Expert Committee:(PA3)Pharmaceutical Analysis 3
USP28–NF23Page 1211
Pharmacopeial Forum:Volume No.30(2)Page 514
Phone Number:1-301-816-8330