Mecamylamine Hydrochloride Tablets
»Mecamylamine Hydrochloride Tablets contain not less than 90.0percent and not more than 110.0percent of the labeled amount of mecamylamine hydrochloride (C11H21N·HCl).
Packaging and storage— Preserve in well-closed containers.
Identification—
A: To a quantity of powdered Tablets,equivalent to about 75mg of mecamylamine hydrochloride,add 50mLof chloroform,and triturate the mixture for 5minutes.Filter,and evaporate the filtrate on a steam bath with the aid of a current of air to dryness:the IRabsorption spectrum of a potassium bromide dispersion of a portion of the residue so obtained exhibits maxima only at the same wavelengths as that of a similar preparation of USP Mecamylamine Hydrochloride RS.
B: Aportion of the residue obtained in Identificationtest Aresponds to the tests for Chloride á191ñ.
Dissolution á711ñ—
Medium: water;750mL.
Apparatus 2: 50rpm.
Time: 30minutes.
Determine the amount of C11H21N·HCl dissolved using the following procedure.
Diluent— Prepare a solution of triethylamine in alcohol (1:100).
Internal standard solution— Prepare a solution of biphenyl in Diluenthaving a concentration of 82.5µg per mL.
Standard solution— Prepare a solution of USP Mecamylamine Hydrochloride RSand biphenyl in Diluenthaving concentrations of 8.25µg per mLof each.
Test solution— [NOTE—Condition the solid-phase extraction column specified in this procedure in the following manner.Wash the column with 5mLof water,then with 5mLof Diluent,and finally with two 5-mLportions of water.]Transfer by pipetting 25.0mLof the solution under test through a freshly conditioned solid-phase extraction column containing L1packing with a sorbent-mass to column volume ratio of 360mg per 5mL,or equivalent.Wash the pipet and the solid-phase extraction column with two 5-mLportions of water.Discard the filtrate.Elute the solid-phase extraction column with two 4-mLportions of Diluent,and collect the eluate in a 10-mLvolumetric flask containing 1.0mLof Internal standard solution.Dilute with Diluentto volume,and mix.
Chromatographic system (see Chromatography á621ñ)—The gas chromatograph is equipped with a flame-ionization detector,a splitless injection system,and a 0.53-mm ×30-m analytical column coated with a 1-5-µm layer of phase G27.The carrier gas is helium at a flow rate of 5.2mLper minute.The detector and column temperatures are maintained at 250and 150,respectively.Chromatograph replicate injections of the Standard solution,and record the peak responses as directed for Procedure:the column efficiency is not less than 4000theoretical plates,the tailing factor is not more than 2,and the relative standard deviation is not more than 2.0%.
Procedure— Separately inject equal volumes (about 2µL)of the Standard solutionand the Test solutioninto the chromatograph,record the chromatograms,and measure the responses for the major peaks.Calculate the amount in mg,of C11H21N·HCl dissolved by the formula:
0.3C(RU/RS),
in which Cis the concentration,in µg per mL,of USP Mecamylamine Hydrochloride RSin the Standard solution;and RUand RSare the peak response ratios of the mecamylamine hydrochloride peak to the internal standard peak obtained from the Test solutionand Standard solution,respectively.
Tolerances— Not less than 75%(Q)of the labeled amount of C11H21N·HCl is dissolved in 30minutes.
Uniformity of dosage units á905ñ: meet the requirements.
Procedure for content uniformity— Place 1Tablet in the digestion flask,and proceed as directed under Nitrogen Determination,Method IIá461ñ.Each mLof 0.01Nsulfuric acid is equivalent to 2.038mg of mecamylamine hydrochloride.
Assay— Weigh and finely powder not fewer than 30Tablets.Transfer an accurately weighed portion of the powder,equivalent to about 50mg of mecamylamine hydrochloride,to a glass-stoppered,125-mLconical flask.Add about 25mLof water,insert the stopper in the flask,and shake by mechanical means for 20minutes.Transfer the contents of the flask to a 250-mLseparator with the aid of small portions of water.Add 1mLof 1Nsodium hydroxide and 5g of sodium chloride,and extract the mixture successively with two 50-mLand three 25-mLportions of ether.Wash the combined ether extracts with three 10-mLportions of water,and wash,in turn,the combined water washes with a 10-mLportion of ether,adding it to the washed combined ether extracts.Transfer the ether phase to a 250-mLconical flask containing 25.0mLof 0.02Nsulfuric acid VS,and evaporate the ether on a steam bath.Cool the solution,add methyl red TS,and titrate the excess acid with 0.02Nsodium hydroxide VS.Each mLof 0.02Nsulfuric acid is equivalent to 4.075mg of mecamylamine hydrochloride (C11H21N·HCl).
Auxiliary Information— Staff Liaison:Andrzej Wilk,Ph.D.,Senior Scientific Associate
Expert Committee:(PA5)Pharmaceutical Analysis 5
USP28–NF23Page 1192
Pharmacopeial Forum:Volume No.28(2)Page 322
Phone Number:1-301-816-8305