Standarder for råvarer
GLYCOPYRRONII BROMIDUM
Glycopyrronium bromide
Glykopyrroniumbromid
Antatt som nordisk legemiddelstandard.
C19H28BrNO3 Mr 398.3
Definition
Glycopyrronium bromide contains not less than 99.0 per cent and not more than the equivalent of 101.0 per cent of (3RS)-3-[(RS)-(2-cyclopentyl-2-hydroxy-2-phenylacetyl)oxy]-1,1-dimethylpyrrolidinium bromide, calculated with reference to the dried substance.
Characters
A white, crystalline powder, freely soluble in water and in alcohol, very slightly soluble in ether.
Identification
A. Melting point (Ph.Eur. 2.2.14) 193 °C to 198 °C.
B. Examine by infrared absorption spectrophotometry (Ph.Eur. 2.2.24) comparing with the spectrum obtained with glycopyrronium bromide NRP. Examine the substances prepared as discs.
C. It gives reaction (a) of bromides (Ph.Eur. 2.3.1).
Tests
Solution S. Dissolve 0.5 g in water R and dilute to 25 ml with the same solvent.
Appearance of solution. Solution S is clear (Ph.Eur. 2.2.1) and colourless (Ph.Eur., Method II 2.2.2).
Acidity or alkalinity. To 10 ml of solution S add 0.05 ml of phenolphthalein solution R1. The solution is colourless. Not more than 0.2 ml of 0.01 M sodium hydroxide is required to change the colour of the indicator to pink. Add 0.4 ml of 0.01 M hydrochloric acid and 0.05 ml of methyl red solution R. The solution is red or orange.
Related substances. Examine by thin layer chromatography (Ph.Eur. 2.2.27) using silica gel G R as the coating substance.
Test solution. Dissolve 0.25 g of the substance to be examined in alcohol R and dilute to 5 ml with the same solvent.
Reference solution. Dilute 0.5 ml of the test solution to 100 ml with alcohol R.
Apply separately to the plate 5 μl of each solution and develop over a path of 15 cm using the mixture of 10 volumes of anhydrous formic acid R, 16 volumes of water R and 74 volumes of ethyl acetate R. Dry the plate at 100 °C to 105 °C for 15 min. Allow to cool and spray with dilute potassium iodobismuthate solution R until the spots appear. Any spot in the chromatogram obtained with the test solution, apart from the principal spot, is not more intense than the spot in the chromatogram obtained with the reference solution (0.5 per cent).
Loss on drying (Ph.Eur. 2.2.32). Not more than 0.5 per cent, determined on 1.000 g by drying in an oven at 100 °C to 105 °C for 3 hours.
Sulphated ash (Ph.Eur. 2.4.14). Not more than 0.1 per cent, determined on 1.0 g.
Assay
Dissolve 0.300 g in a mixture of 40 ml of acetic anhydride R and 10 ml of anhydrous acetic acid R. Titrate with 0.1 M perchloric acid, determining the end-point potentiometrically (Ph.Eur. 2.2.20).
1 ml of 0.1 M perchloric acid is equivalent to 39.83 mg of C19H28BrNO3.
Storage
Store in a well-closed container.
Sist gjennomgått: 01.07.2010
Første gang publisert: 12.01.2009