10,11-Dihydro-N-methyl-5H-dibenzo[a,d]cycloheptene-D5,g-propylamine hydrochloride [894-71-3].
»Nortriptyline Hydrochloride contains not less than 97.0percent and not more than 101.5percent of C19H21N·HCl,calculated on the dried basis.
Packaging and storage Preserve in tight,light-resistant containers.
A: Infrared Absorption á197Sñ
Solution: 50mg per mL.
B: Ultraviolet Absorption á197Uñ
Solution: 10µg per mL.
Absorptivities at 239nm,calculated on the dried basis,do not differ by more than 3.0%.
C: It responds to the tests for Chloride á191ñwhen tested as specified for alkaloidal hydrochlorides.
Melting range,Class Iá741ñ: between 215and 220,but the range between beginning and end of melting does not exceed 3.
Loss on drying á731ñ Dry it at 105for 3hours:it loses not more than 0.5%of its weight.
Residue on ignition á281ñ: not more than 0.1%.
Heavy metals,Method IIá231ñ: 0.001%.
Adsorbent: chromatographic silica gel mixture.
Test solution Transfer about 250mg of Nortriptyline Hydrochloride,accurately weighed,to a 10-mLvolumetric flask.Dissolve in and dilute with methanol to volume,and mix.
Standard solutions Dissolve an accurately weighed quantity of USP Nortriptyline Hydrochloride RSin methanol,and dilute quantitatively,and stepwise if necessary,with methanol to obtain a solution having a known concentration of about 25.0mg per mL(Standard solution A).Dilute appropriate portions of this solution with methanol to obtain Standard solutions B,C,D,E,and Fhaving known concentrations of 125,75,50,25,and 12.5µg per mL,respectively.The final concentrations of Standard solutions B,C,D,E,and Frepresent 0.5%,0.3%,0.2%,0.1%,and 0.05%of Standard solution Aconcentration,respectively.
Application volume: 5µL.
Developing solvent system: a mixture of acetonitrile,methanol,and ammonium hydroxide (10:1:1).
Procedure Apply equal volumes of the Test solutionand Standard solutions A,B,C,D,E,and Fas directed in Ordinary Impurities á466ñ.Examine the plate under short-wavelength UVlight,then spray the plate with Dragendorff's TS,dry the plate with a stream of nitrogen,and then spray with hydrogen peroxide TS:any secondary spot at an RFvalue of 0.78relative to the nortriptyline spot in the Test solutionis not greater than the principal spot for Standard solution D;any other secondary spot in the Test solutionis not more than 0.1%;and the sum of all secondary spots is not more than 0.5%.
Organic volatile impurities,Method Iá467ñ: meets the requirements.
Assay Dissolve about 600mg of Nortriptyline Hydrochloride,accurately weighed,in 50mLof glacial acetic acid,add 10mLof mercuric acetate TS,and titrate with 0.1Nperchloric acid VS,determining the endpoint potentiometrically.Perform a blank determination,and make any necessary correction.Each mLof 0.1Nperchloric acid is equivalent to 29.98mg of C19H21N·HCl.
Auxiliary Information Staff Liaison:Salvador C.Salado,M.S.,Scientist and Latin American Liaison
Expert Committee:(PA3)Pharmaceutical Analysis 3