A: Finely powder a number of Tablets,equivalent to about 90mg of propantheline bromide,and triturate the powder with 10mLof chloroform.Filter,and wash the filter with 10mLof chloroform,collecting the filtrate and washing in a separator.Add 10mLof water,shake,and discard the chloroform layer.Wash the aqueous layer with two 10-mLportions of ether,and discard the ether washings.Filter the aqueous solution,and evaporate on a steam bath with the aid of a current of dry air to dryness.Dissolve the residue in 5mLof chloroform,mix,and proceed as directed in Identificationtest Aunder Propantheline Bromide,beginning with “In a well-ventilated hood”:the specified result is observed.

B: The chromatogram of the Assay preparationobtained as directed in the Assayexhibits a major peak for propantheline bromide,the retention time of which corresponds to that exhibited in the chromatogram of the Standard preparation.

Medium: pH4.5(±0.05)Acetate buffer prepared by mixing 1.64g of anhydrous sodium acetate and 1.25mLof glacial acetic acid with 500mLof water,and diluting with water to obtain 1000mLof solution having a pHof 4.50±0.05;500mL.

Apparatus 2: 50rpm.

Time: 45minutes.

pH3.5buffer solution,Mobile phase,and Chromatographic system— Prepare as directed under Assay.

Procedure— Inject a volume (about 50µL)of a filtered portion of the solution under test into the chromatograph,record the chromatogram,and measure the response for the major peak.Calculate the quantity of C23H30BrNO3dissolved in comparison with a Standard solution having a known concentration of USP Propantheline Bromide RSin the same medium and similarly chromatographed.

Tolerances— Not less than 75%(Q)of the labeled amount of C23H30BrNO3is dissolved in 45minutes.

pH3.5buffer solution andMobile phase— Prepare as directed for Related compoundsunder Propantheline Bromide.

Standard solution— Dissolve accurately weighed quantities of USP Propantheline Bromide Related Compound A RS,USP Xanthanoic Acid RS,and USP Xanthone RSin Mobile phase,and dilute quantitatively and stepwise if necessary,with Mobile phaseto obtain a solution having known concentrations of about 12.0µg of propantheline bromide related compound Aper mL,and about 3.0µg each of xanthanoic acid and xanthone per mL.

Test solution— Use the Assay preparationprepared as directed under Assay.

Chromatographic system (see Chromatography á621ñ)— The liquid chromatograph is equipped with a 254-nm detector and a 4.6-mm ×25-cm column that contains packing L7.The flow rate is about 2.0mLper minute.Chromatograph the Standard solution,and record the peak responses as directed for Procedure:the resolution,R,between the least resolved peaks is not less than 1.2;and the relative standard deviation for replicate injections of the Standard solutionis not more than 6.0%for each component or,if the Assayis performed concomitantly,the relative standard deviation for the propantheline bromide peak in the replicate injections of the Standard solutionis not more than 2.0%.

Procedure— Separately inject equal volumes (about 50µL)of the Standard solutionand the Test solutioninto the chromatograph,record the chromatograms,and measure the responses for the major peaks.Calculate the percentage of xanthanoic acid,xanthone,and propantheline bromide related compound Agreater than or equal to 0.1%in the portion of Tablets taken by the formula: in which Cis the concentration,in µg,of xanthanoic acid,xanthone,or propantheline bromide related compound Aper mLof the Standard solution;CXis the theoretical concentration,in µg per mL,of Propantheline Bromide in the Test solution;and rUand rSare the related compound peak responses obtained from the Test solutionand the Standard solution,respectively:not more than 4.0%of propantheline bromide related compound Aand 1.0%each of xanthone and xanthanoic acid are found.

pH3.5buffer solution andMobile phase— Prepare as directed for Related compoundsunder Propantheline Bromide.

Standard preparation— Dissolve an accurately weighed quantity of USP Propantheline Bromide RSin Mobile phaseto obtain a solution having a known concentration of about 0.3mg per mL.

Assay preparation— Weigh and finely powder not less than 20Tablets.Transfer an accurately weighed portion of the powder,equivalent to 15mg of propantheline bromide,to a 50-mLvolumetric flask,dissolve in Mobile phase,dilute with Mobile phaseto volume,mix.and filter.

Chromatographic system(see Chromatography á621ñ)— The liquid chromatograph is equipped with a 254-nm detector and a 4.6-mm ×25-cm column that contains packing L7.The flow rate is about 2.0mLper minute.Chromatograph the Standard preparation,and record peak responses as directed for Procedure:the relative standard deviation for replicate injections is not more than 2.0%.

Procedure— Separately inject equal volumes (about 50µL)of the Standard preparationand the Assay preparationinto the chromatograph,record the chromatograms,and measure the peak responses.Calculate the quantity,in mg,of C23H30BrNO3in the portion of Tablets taken by the formula: in which Cis the concentration,in mg per mL,of USP Propantheline Bromide RSin the Standard preparation;and rUand rSare the peak responses due to Propantheline Bromide obtained from the Assay preparationand the Standard preparation,respectively.