(Ph Eur monograph 1489)
99.0 per cent to 101.0 per cent (dried substance).
White or yellowish crystalline powder.
Sparingly soluble in water, soluble in methanol, practically
insoluble in methylene chloride.
A, C, D.
20.0 mg in 0.05M sulphuric acid and dilute
to 100.0 ml with the same acid. Dilute 2.0 ml of the solution to 10.0 ml with 0.05M sulphuric acid. Examined between 200 nm
and 350 nm (2.2.25), the solution shows two absorption maxima at 245 nm and 310 nm. The
ratio of the absorbance measured at 245 nm to that measured at 310 nm is 3.2 to 3.4.
absorption spectrophotometry (2.2.24).
Comparison: ambroxol hydrochloride
by thin-layer chromatography (2.2.27).
Dissolve 50 mg of the substance to be examined in methanol R and dilute to 5 ml with the same solvent.
Dissolve 50 mg of ambroxol hydrochloride CRS in methanol R and dilute to 5 ml with the same solvent.
TLC silica gel F254 plate R.
Concentrated ammonia R, 1-propanol R, ethyl acetate R, hexane R
Over 2/3 of the plate.
Examine in ultraviolet light at 254 nm.
The principal spot in the chromatogram obtained with the test
solution is similar in position and size to the principal spot in the chromatogram
obtained with the reference solution.
25 mg in 2.5 ml of water R, mix with
1.0 ml of dilute ammonia R1 and allow to stand for 5 min. Filter and acidify the
filtrate with dilute nitric acid R. The filtrate gives reaction (a) of chlorides
Dissolve 0.75 g in methanol
R and dilute to 15 ml with the same solvent.
Appearance of solution
Solution S is clear (2.2.1) and not more intensely coloured than reference solution Y6
(2.2.2, Method II).
4.5 to 6.0.
Dissolve 0.2 g in carbon dioxide-free water R and dilute to 20 ml with the same solvent.
Liquid chromatography (2.2.29).
Prepare the solutions immediately before use.
Dissolve 50.0 mg of the substance to be examined in water R and dilute to 50.0 ml with the same solvent.
Reference solution (a)
Dilute 5.0 ml of the test solution to 250.0 ml with water R. Dilute 1.0 ml of this solution to 20.0 ml
with the mobile phase.
Reference solution (b)
Dissolve 5 mg of the substance to be examined in 0.2 ml of methanol R and add 0.04 ml of a mixture of 1 volume of formaldehyde
solution R and 99 volumes of water R.
Heat at 60C for 5 min. Evaporate to dryness under a current of nitrogen. Dissolve the
residue in 5 ml of water R and dilute
to 20 ml with the mobile phase.
size: l = 0.25 m, Ø = 4.0
stationary phase: octadecylsilyl silica gel for
chromatography R (5 mm).
A mixture of equal volumes of acetonitrile R and a
solution prepared as follows: dissolve 1.32 g of ammonium phosphate R in 900 ml of water R, adjust to pH 7.0 with phosphoric acid R
and dilute to 1000 ml with water R.
Spectrophotometer at 248 nm.
Reference solution (a).
3 times the retention time of the principal peak in the
chromatogram obtained with the test solution.
resolution: minimum of 4.0 between
the peaks due to impurity B and ambroxol in the chromatogram obtained with reference
any impurity: not more than the area of
the principal peak in the chromatogram obtained with reference solution (a) (0.1 per
total: not more than 3 times the
area of the principal peak in the chromatogram obtained with reference solution (a) (0.3
disregard limit: 0.1 times the area of the
principal peak in the chromatogram obtained with reference solution (a).
Heavy metals (2.4.8)
Maximum 20 ppm.
1.0 g complies with limit test C. Prepare the standard using 2
ml of lead standard solution (10 ppm Pb) R.
Loss on drying (2.2.32)
Maximum 0.5 per cent, determined on 1.000 g by drying in an
oven at 100-105C.
Sulphated ash (2.4.14)
Maximum 0.1 per cent, determined on 1.0 g.
Dissolve 0.300 g in 70 ml of alcohol R and add 5 ml of 0.01M hydrochloric
acid. Carry out a potentiometric titration (2.2.20),
using 0.1M sodium hydroxide. Read the volume added between the two points of inflexion.
1 ml of 0.1M sodium
hydroxide is equivalent to 41.46 mg of C13H19Br2ClN2O.
Store protected from light.
Action and use