Glycopyrrolate
;)
Pyrrolidinium,3-[(cyclopentylhydroxyphenylacetyl)oxy]-1,1-dimethyl-,bromide.
3-Hydroxy-1,1-dimethylpyrrolidinium bromide a-cyclopentylmandelate [596-51-0].
»Glycopyrrolate,dried at 105
for 3hours,contains not less than 98.0percent and not more than 100.5percent of C19H28BrNO3.
for 3hours,contains not less than 98.0percent and not more than 100.5percent of C19H28BrNO3.
Packaging and storage—
Preserve in tight containers.
Identification—
A:
Infrared Absorption á197Kñ.
Solution:
500µg per mL.
Medium:
water.
Absorptivities at 258nm,calculated on the dried basis,do not differ by more than 3.0%.
C:
Asolution (1in 40)responds to the tests for Bromide á191ñ.
Melting range,Class Iá741ñ:
between 193and 198,but the range between beginning and end of melting does not exceed 2.
and 198,but the range between beginning and end of melting does not exceed 2.
Loss on drying á731ñ—
Dry it at 105for 3hours:it loses not more than 0.5%of its weight.
for 3hours:it loses not more than 0.5%of its weight.
Residue on ignition á281ñ:
not more than 0.3%.
Ordinary impurities á466ñ—
Test solution:
50mg per mLin alcohol.
Standard solutions:
0.05mg per mL,0.25mg per mL,0.5mg per mL,and 1.0mg per mLin alcohol.
Eluant:
a mixture of ethyl acetate,water,and anhydrous formic acid (74:16:10).
Application volume:
5µL.
Adsorbent:
chromatographic silica gel.
Visualization—
Dry the plate at 105for 15minutes,followed by Visualization Technique 3;then air-dry the developed plate at room temperature for 2hours.
for 15minutes,followed by Visualization Technique 3;then air-dry the developed plate at room temperature for 2hours.
Limits—
The intensity of any secondary spot obtained from the Test solutioncorresponds to not more than 0.5%,and the sum of the intensities of all secondary spots obtained from the Test solutioncorresponds to not more than 2.0%.
Assay—
Dissolve about 800mg of Glycopyrrolate,previously dried and accurately weighed,in 50mLof glacial acetic acid,add 10mLof mercuric acetate TSand 1drop of crystal violet TS,and titrate with 0.1Nperchloric acid VS.Perform a blank determination,and make any necessary correction.Each mLof 0.1Nperchloric acid is equivalent to 39.83mg of C19H28BrNO3.
Auxiliary Information—
Staff Liaison:Elena Gonikberg,Ph.D.,Scientist
Expert Committee:(PA4)Pharmaceutical Analysis 4
USP28–NF23Page 913
Pharmacopeial Forum:Volume No.29(5)Page 1503
Phone Number:1-301-816-8251