EUROPEAN PHARMACOPOEIA 5.

Mianserinhydrochloride

Apply to the plate 2 pl of each solution. Develop over a path of 15 cm using a mixture 01/2005:0846 of 5 volumes of diethylamine R, 20 volumes of ether R and 75 volumes of cyclohexane R. Examine in ultraviolet light at 254 nm. The MIANSERIN HYDROCHLORIDE 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 reference solution (a). The test is not valid unless the chromatogram obtained with reference solution (b) shows two clearly separated principal spots. D.It gives reaction (a) of chlorides (2.3.1).
Mr 300.8

Mianserini hydrochloridum C18H21ClN2 DEFINITION Mianserin hydrochloride contains not less than 98.5 per cent and not more than the equivalent of 101.0 per cent of (RS)-2-methyl-1,2,3,4,10,14bhexahydrodibenzo[c,/]pyrazino[1,2a]az epine hydrochloride, calculated with reference to the dried substance.

IDENTIFICATION First identification: B, D. Second identification: A, C, D. A. Dissolve 50.0 mg in water R and dilute to 50.0 ml with the same solvent. Dilute 5.0 ml of the solution to 50.0 ml with water R. Examined between 230 nm and 350 nm (2.2.25), the solution shows an absorption maximum at 279 nm. The specific absorption at the maximum is 64 to 72. B. Examine by infrared absorption spectrophotometry (2.2.24), comparing with the spectrum obtained with mianserin hydrochloride CRS. Examine the substances as discs prepared using potassium chloride R. If the spectra obtained show differences, dissolve the substance to be examined and the reference substance separately in methanol R, evaporate to dryness and record new spectra using the residues. C. Examine by thin-layer chromatography (2.2.27), using silica gel GF254 R as the coating substance. Test solution. Dissolve 10 mg of the substance to be examined in methylene chloride R and dilute to 5 ml with the same solvent. Reference solution (a). Dissolve 10 mg of mianserin hydrochloride CRS in methylene chloride R and dilute to 5 ml with the same solvent. Reference solution (b). Dissolve 10 mg of mianserin hydrochloride CRS and 10 mg of cyproheptadine hydrochloride CRS in methylene chloride R and dilute to 5 ml with the same solvent.

ASSAY Dissolve 0.200 g in a mixture of 5.0 ml of 0.01 Mhydrochloric acid and 50 ml of alcohol R. Carry out a potentiometric titration (2.2.20), using 0.1 M sodium hydroxide. Read the volume added between the two points of inflexion. l ml of 0.1 M sodium hydroxide is equivalent to 30.08 mg of C18H21ClN2* STORAGE Store protected from light.
A. [2-[(2^S)-4-methyl-2-phenylpiperazin-1yl]phenyl]metha- nol.

IMPURITIES

Monographs

CHARACTERS White or almost white, crystalline powder or crystals, sparingly soluble in water, soluble in methylene chloride, slightly soluble in alcohol.

TESTS pH (2.2.3). Dissolve 0.10 g in carbon dioxidefree water R and dilute to 10 ml with the same solvent. The pH of the solution is 4.0 to 5.5. Related substances. Examine by thin-layer chromatography (2.2.27), using silica gel G R as the coating substance. Test solution. Dissolve 0.20 g of the substance to be examined in a mixture of 1 volume of ammonia R and 4 volumes of methanol R and dilute to 10 ml with the same mixture of solvents. Reference solution (a). Dilute 1 ml of the test solution to 200 ml with a mixture of 1 volume of ammonia R and 4 volumes of methanol R. Reference solution (b). Dilute 5 ml of reference solution (a) to 25 ml with a mixture of 1 volume of ammonia R and 4 volumes of methanol R. Apply to the plate 5 pl of each solution. Develop over a path of 15 cm using a mixture of 10 volumes of methanol R and 90 volumes of methylene chloride R. Dry the plate in a current of cold air. Expose the plate to iodine vapour for 20 min. 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 reference solution (a) (0.5 per cent) and at most one such spot is more intense than the spot in the chromatogram obtained with reference solution (b) (0.1 per cent). Loss on drying (2.2.32). Not more than 0.5 per cent, determined on 1.000 g by drying over diphosphorus pentoxide R at 65 C at a pressure not exceeding 700 Pa for 3 h. Sulphated ash (2.4.14). Not more than 0.1 per cent, determined on 1.0 g.

General Notices (1) apply to all monographs and other texts

204 1