Ephedrine hydrochloride, racemic
EUROPEAN PHARMACOPOEIA 7.0
by the general monograph Substances for pharmaceutical use (2034). It is therefore not necessary to identify these impurities for demonstration of compliance. See also 5.10. Control of impurities in substances for pharmaceutical use): B.
H OH
A. (- )-(lÄ)-l-hydroxy-l-phenylpropan-2-one,
H OH
H CH3
B. (lS,2S)-2-(methylamino)-l-phenylpropan-l-ol (pseudoephedrine).
01/2008:0715 corrected 6.0
ephedrine hydrochloride, racemic
Ephedrin! racemici hydrochloridum
H OH
'CH3 andenantiomer , HCl
H CH3
C10H16C1NO [134-71-4]
Mr 201.7
DEFINITION
Racemic ephedrine hydrochloride contains not less than 99.0 per cent and not more than the equivalent of 101.0 per cent of (li?S,2Si?)-2-(methylamino)-l-phenylpropan-l-ol hydrochloride, calculated with reference to the dried substance.
CHARACTERS
A white or almost white, crystalline powder or colourless crystals, freely soluble in water, soluble in ethanol (96 per cent). It melts at about 188 °C.
IDENTIFICATION
First identification: B, E. Second identification: A, C, D, E.
A. Optical rotation (see Tests).
B. Examine by infrared absorption spectrophotometry (2.2.24), comparing with the spectrum obtained with racemic ephedrine hydrochloride CRS. Examine the substances prepared as discs.
C. Examine the chromatograms obtained in the test for related substances. The principal spot in the chromatogram obtained with test solution (b) is similar in position, colour and size to the principal spot in the chromatogram obtained with reference solution (a).
D. To 0.1 mL of solution S (see Tests) add 1 mL of water R, 0.2 mL of copper sulfate solution R and 1 mL of strong sodium hydroxide solution R. A violet colour is produced. Add 2 mL of ether R and shake. The ether layer is purple and the aqueous layer is blue.
E. To 5 mL of solution S add 5 mL of water R. The solution gives reaction (a) of chlorides (2.3.1).
TESTS
Solution S. Dissolve 5.00 g in distilled water R and dilute to 50.0 mL with the same solvent.
Appearance of solution. Solution S is clear (2.2.1) and colourless (2.2.2, Method II).
Acidity or alkalinity. To 10 mL of solution S add 0.1 mL of
methyl red solution R and 0.1 mL of 0.01 M sodium hydroxide; the solution is yellow. Add 0.2 mL of 0.01 M hydrochloric acid; the solution is red.
Optical rotation (2.2.7): + 0.2° to -0.2°, determined on solution S.
Related substances. Examine by thin-layer chromatography (2.2.27), using silica gel G R as the coating substance. Test solution (a). Dissolve 0.20 g of the substance to be examined in methanol R and dilute to 10 mL with the same solvent.
Test solution (b). Dilute 1 mL of test solution (a) to 10 mL with methanol R.
Reference solution (a). Dissolve 20 mg of racemic ephedrine hydrochloride CRS in methanol R and dilute to 10 mL with the same solvent.
Reference solution (b). Dilute 1 mL of test solution (a) to 200 mL with methanol R.
Apply separately to the plate 10 |jL of each solution. Develop over a path of 15 cm using a mixture of 5 volumes of chloroform R, 15 volumes of concentrated ammonia R and 80 volumes of 2-propanol R. Allow the plate to dry in air. Spray with ninhydrin solution R and heat at 110 °C for 5 min. Any spot in the chromatogram obtained with test solution (a), apart from the principal spot, is not more intense than the spot in the chromatogram obtained with reference solution (b) (0.5 per cent). Disregard any spot of lighter colour than the background.
Sulfates (2.4.13). 15 mL of solution S complies with the limit test for sulfates (100 ppm).
Loss on drying (2.2.32). Not more than 0.5 per cent, determined on 1.000 g by drying in an oven at 105 °C.
Sulfated ash (2.4.14). Not more than 0.1 per cent, determined on 1.0 g.
ASSAY
Dissolve 0.170 g in 30 mL of ethanol (96 per cent) R. Add
5.0 mL of 0.01 M hydrochloric acid. Carry out a potentiometric
titration (2.2.20), using 0.1 M sodium hydroxide. Read
the volume added between the two points of inflexion.
1 mL of 0.1 M sodium hydroxide corresponds to 20.17 mg of
C10H16C1NO.
STORAGE
Store protected from light.
01/2010:2411 corrected 7.0
epinastine hydrochloride
Epinastini hydrochloridum
and enantiomer
HCI
C16H16C1N3
M, 285.8
[108929-04-0] DEFINITION
(13bi?5)-9,13b-Dihydro-l/Wibenzo[c,/]imidazo[l,5-a]azepin-3-amine hydrochloride.
Content: 99.0 per cent to 101.0 per cent (dried substance). CHARACTERS
Appearance: white or almost white, hygroscopic, crystalline powder.
1928
See the information section on general monographs (cover pages)