Hyoscyamine Hydrobromide
C17H23NO3·HBr 370.28

Benzeneacetic acid,a-(hydroxymethyl)-,8-methyl-8-azabicyclo[3.2.1]oct-3-yl ester,hydrobromide [3(S)-endo]-.

1aH,5aH-Tropan-3a-ol (-)-tropate (ester)hydrobromide [306-03-6].
»Hyoscyamine Hydrobromide contains not less than 98.5percent and not more than 100.5percent of C17H23NO3·HBr,calculated on the dried basis.[Caution—Handle Hyoscyamine Hydrobromide with exceptional care,since it is highly potent. ]
Packaging and storage— Preserve in tight,light-resistant containers.
Identification—
A: Transfer 30mg of Hyoscyamine Hydrobromide and 36mg of USP Hyoscyamine Sulfate RSto individual 60-mLseparators with the aid of 5-mLportions of water.To each separator add 1.5mLof 1Nsodium hydroxide and 10mLof chloroform.Shake for 1minute,allow the layers to separate,and filter the chloroform extracts through separate filters of about 2g of anhydrous granular sodium sulfate supported on pledgets of glass wool.Extract each aqueous layer with two additional 10-mLportions of chloroform,filtering and combining with the respective main extracts.Evaporate the chloroform solutions under reduced pressure to dryness,and dissolve each residue in 10mLof carbon disulfide:the IRabsorption spectrum,determined in a 1-mm cell,of the solution obtained from the test specimen exhibits maxima only at the same wavelengths as that of the solution obtained from the Reference Standard.
B: To about 1mLof a solution (1in 20)add gold chloride TS,dropwise with shaking,until a definite precipitate separates.Add a small amount of 3Nhydrochloric acid,dissolve the precipitate with the aid of heat,and allow the solution to cool:lustrous reddish brown scales that may be accompanied by reddish brown needles are formed (distinction from atropine and scopolamine).
C: To an aqueous solution (1in 20)add silver nitrate TS:a yellowish-white precipitate is formed,and it is insoluble in nitric acid.
Melting temperature á741ñ: not less than 149.
Specific rotation á781Sñ: not less than -24.
Test solution: 50mg per mL,in water.
Loss on drying á731ñ— Dry it at 105for 2hours:it loses not more than 1.0%of its weight.
Residue on ignition á281ñ: not more than 0.2%.
Other alkaloids— Dissolve 250mg in 1mLof 0.1Nhydrochloric acid,and dilute with water to 15mL.To 5mLof the solution add a few drops of platinic chloride TS:no precipitate is formed immediately.To another 5-mLportion add 2mLof 6Nammonium hydroxide:the mixture may develop a slight opalescence,but no turbidity or precipitate is formed immediately.
Assay— Dissolve about 700mg of Hyoscyamine Hydrobromide,accurately weighed,in a mixture of 50mLof glacial acetic acid and 10mLof mercuric acetate TS.Add 1drop of crystal violet TS,and titrate with 0.1Nperchloric acid VSto a blue-green endpoint.Perform a blank determination,and make any necessary correction.Each mLof 0.1Nperchloric acid is equivalent to 37.03mg of C17H23NO3·HBr.
Auxiliary Information— Staff Liaison:Elena Gonikberg,Ph.D.,Scientist
Expert Committee:(PA4)Pharmaceutical Analysis 4
USP28–NF23Page 986
Phone Number:1-301-816-8251