Tripelennamine Hydrochloride, chemical structure, molecular formula, Reference Standards
»Tripelennamine Hydrochloride contains not less than 98.0percent and not more than 100.5percent of C16H21N3·HCl,calculated on the dried basis.
Packaging and storage
Preserve in well-closed,light-resistant containers.
USP Reference standards á11ñ
USP Tripelennamine Hydrochloride RS.
It meets the requirements under IdentificationOrganic Nitrogenous Bases á181ñ.
It meets the requirements of the tests for Chloride á191ñ.
Melting range á741ñ:
between 188and 192.
Loss on drying á731ñ
Dry it at 105for 3hours:it loses not more than 1.0%of its weight.
Residue on ignition á281ñ:
not more than 0.1%.
Ion-pair solution,Mobile phase,andBenzaldehyde solution
Proceed as directed in the Assay.
Proceed as directed in the Assay.To evaluate system suitability requirements,use the System suitability preparationand the Standard preparation,as prepared in the Assay.
Use the Assay preparation.
Inject a volume (about 10µL)of the Test solutioninto the chromatograph,record the chromatogram,and measure all of the peak responses.Calculate the percentage of each impurity in the portion of Tripelennamine Hydrochloride taken by the formula:
in which riis the peak response for each impurity;and rSis the sum of the responses for all the peaks:not more than 0.1%of any individual impurity is found;and not more than 1.0%of total impurities is found.
Organic volatile impurities,Method Iá467ñ:
meets the requirements.
Prepare a 29mMsodium 1-octanesulfonate solution.
Transfer 530mLof methanol to a suitable container,add 1.0mLof N,N-dimethyloctylamine,and mix thoroughly.Add 430mLof the Ion-pair solution,mix,and adjust with phosphoric acid to a pHof 3.0.Make adjustments if necessary (see System Suitabilityunder Chromatography á621ñ).
Transfer 1.0mLof benzaldehyde to a 100-mLvolumetric flask,dilute with Mobile phaseto volume,and mix.Transfer 5.0mLof the solution so obtained to a 100-mLvolumetric flask,dilute with Mobile phaseto volume,and mix.
System suitability preparation
Transfer about 50mg of 2-benzylaminopyridine,accurately weighed,to a 100-mLvolumetric flask,add 10mLof methanol,sonicate to dissolve,dilute with Mobile phaseto volume,and mix.Transfer 5.0mLof the solution so obtained to a 100-mLvolumetric flask,add 5.0mLof Benzaldehyde solution,dilute with Mobile phaseto volume,and mix.
Dissolve an accurately weighed quantity of USP Tripelennamine Hydrochloride RSin Mobile phase,and dilute quantitatively,and stepwise if necessary,with Mobile phaseto obtain a solution having a known concentration of about 0.5mg per mL.
Transfer about 50mg of Tripelennamine Hydrochloride,accurately weighed,to a 100-mLvolumetric flask,dissolve in and dilute with Mobile phaseto volume,and mix.
(see Chromatography á621ñ)The liquid chromatograph is equipped with a 242-nm detector and a 4.6-mm ×25-cm column that contains packing L7.The flow rate is about 1mLper minute.The column temperature is maintained at 35.[NOTENew columns are conditioned with Mobile phase overnight before the initial use and may be reconditioned,as necessary,thereafter.]Chromatograph the System suitability preparation,and record the peak responses as directed for Procedure:the relative retention times are about 0.75for benzaldehyde and 1.0for 2-benzylaminopyridine;and the resolution,R,between benzaldehyde and 2-benzylaminopyridine is not less than 3.5.Chromatograph the Standard preparation,and record the peak responses as directed for Procedure:the column efficiency is not less than 10,000theoretical plates;and the relative standard deviation for replicate injections is not more than 1.0%.
Separately inject equal volumes (about 10µL)of the Standard preparationand the Assay preparationinto the chromatograph,record the chromatograms,and measure the responses for the major peaks.Calculate the quantity,in mg,of C16H21N3·HCl in the portion of Tripelennamine Hydrochloride taken by the formula:
in which Cis the concentration,in mg per mL,of USP Tripelennamine Hydrochloride RSin the Standard preparation;and rUand rSare the peak responses obtained from the Assay preparationand the Standard preparation,respectively.
Staff Liaison:Karen A Russo,Ph.D.,Scientist
Expert Committee:(PA1)Pharmaceutical Analysis 1
Pharmacopeial Forum:Volume No.30(4)Page 1312
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