Packaging and storage—
Preserve in tight, light-resistant containers.
Identification—
A:
Transfer 30 mg of Hyoscyamine Hydrobromide and 36 mg of
USP Hyoscyamine Sulfate RS to individual 60-mL separators with the aid of 5-mL portions of water. To each separator add 1.5 mL of 1 N sodium hydroxide and 10 mL of chloroform. Shake for 1 minute, allow the layers to separate, and filter the chloroform extracts through separate filters of about 2 g of anhydrous granular sodium sulfate supported on pledgets of glass wool. Extract each aqueous layer with two additional 10-mL portions of chloroform, filtering and combining with the respective main extracts. Evaporate the chloroform solutions under reduced pressure to dryness, and dissolve each residue in 10 mL of carbon disulfide: the IR absorption 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 1 mL of a solution (1 in 20) add gold chloride TS, dropwise with shaking, until a definite precipitate separates. Add a small amount of 3 N hydrochloric 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 (1 in 20) add silver nitrate TS: a yellowish-white precipitate is formed, and it is insoluble in nitric acid.
Specific rotation 
781S
:
not less than
24
.
Test solution:
50 mg per mL, in water.
Other alkaloids—
Dissolve 250 mg in 1 mL of 0.1 N hydrochloric acid, and dilute with water to 15 mL. To 5 mL of the solution add a few drops of
platinic chloride TS: no precipitate is formed immediately. To another 5-mL portion add 2 mL of 6 N ammonium hydroxide: the mixture may develop a slight opalescence, but no turbidity or precipitate is formed immediately.
Assay—
Dissolve about 700 mg of Hyoscyamine Hydrobromide, accurately weighed, in a mixture of 50 mL of glacial acetic acid and 10 mL of
mercuric acetate TS. Add 1 drop of
crystal violet TS, and titrate with 0.1 N perchloric acid VS to a blue-green endpoint. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 37.03 mg of C
17H
23NO
3·HBr.
-(hydroxymethyl)-, 8-methyl-8-azabicyclo[3.2.1]oct-3-yl ester, hydrobromide [3(S)-endo]-.