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Glycopyrrolate
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C19H28BrNO3 398.33

Pyrrolidinium, 3-[(cyclopentylhydroxyphenylacetyl)oxy]-1,1-dimethyl-, bromide.
3-Hydroxy-1,1-dimethylpyrrolidinium bromide -cyclopentylmandelate [596-51-0].
» Glycopyrrolate, dried at 105 for 3 hours, contains not less than 98.0 percent and not more than 100.5 percent of C19H28BrNO3.
Packaging and storage— Preserve in tight containers.
Identification—
Solution: 500 µg per mL.
Medium: water.
Absorptivities at 258 nm, calculated on the dried basis, do not differ by more than 3.0%.
C: A solution (1 in 40) responds to the tests for Bromide 191.
Melting range, Class I 741: between 193 and 198, but the range between beginning and end of melting does not exceed 2.
Loss on drying 731— Dry it at 105 for 3 hours: it loses not more than 0.5% of its weight.
Residue on ignition 281: not more than 0.3%.
Ordinary impurities 466—
Test solution: 50 mg per mL in alcohol.
Standard solutions: 0.05 mg per mL, 0.25 mg per mL, 0.5 mg per mL, and 1.0 mg per mL in alcohol.
Eluant: a mixture of ethyl acetate, water, and anhydrous formic acid (74:16:10).
Application volume: 5 µL.
Adsorbent: chromatographic silica gel.
Visualization— Dry the plate at 105 for 15 minutes, followed by Visualization Technique 3; then air-dry the developed plate at room temperature for 2 hours.
Limits— The intensity of any secondary spot obtained from the Test solution corresponds to not more than 0.5%, and the sum of the intensities of all secondary spots obtained from the Test solution corresponds to not more than 2.0%.
Residual solvents 467: meets the requirements.
(Official January 1, 2007)
Assay— Dissolve about 800 mg of Glycopyrrolate, previously dried and accurately weighed, in 50 mL of glacial acetic acid, add 10 mL of mercuric acetate TS and 1 drop of crystal violet TS, and titrate with 0.1 N perchloric acid VS. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 39.83 mg of C19H28BrNO3.
Auxiliary Information— Staff Liaison : Elena Gonikberg, Ph.D., Scientist
Expert Committee : (MDGRE05) Monograph Development-Gastrointestinal Renal and Endocrine
USP29–NF24 Page 1014
Pharmacopeial Forum : Volume No. 29(5) Page 1503
Phone Number : 1-301-816-8251