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Sertaconazole nitrate EUROPEAN PHARMACOPOEIA 7.0 D. To 1 mL of a 10 g/L solution of the substance to be examined in a test-tube, add 5 mL of a 20 g/L solution of sodium periodate R. Heat on a water-bath and collect the vapour on glass wool moistened with water R and inserted in the opening of the test tube. After heating for 5 min, transfer the glass wool to a test-tube containing 1 mL of a 15 g/L solution of chromotropic acid, sodium salt R and 3 mL of sulfuric acid R. Heat on a water-bath for 10 min. A violet-red colour is produced. TESTS Solution S. Dissolve 2.5 g in distilled water R and dilute to 50 mL with the same solvent. Appearance of solution. Solution S is clear (2.2.1) and not more intensely coloured than reference solution BY6 (2.2.2, Method II). Specific optical rotation (2.2.7). Dissolve 2.50 g in dilute hydrochloric acid R and dilute to 25.0 mL with the same acid. The specific optical rotation is + 14.0 to + 16.0, calculated with reference to the dried substance. Ninhydrin-positive substances. Examine by thin-layer chromatography (2.2.27), using a TLC silica gel plate R. Test solution (a). Dissolve 0.10 g of the substance to be examined in 0.1 M hydrochloric acid and dilute to 10 mL with the same acid. Test solution (b). Dilute 1 mL of test solution (a) to 50 mL with water R. Reference solution (a). Dissolve 10 mg of serine CRS in 0.1 M hydrochloric acid and dilute to 50 mL with the same acid. Reference solution (b). Dilute 5 mL of test solution (b) to 20 mL with water R. Reference solution (c). Dissolve 10 mg of methionine CRS and 10 mg of serine CRS in 0.1 M hydrochloric acid and dilute to 25 mL with the same acid. Apply to the plate 5 μL of each solution. Develop over a path of 15 cm using a mixture of 20 volumes of glacial acetic acid R, 20 volumes of water R and 60 volumes of butanol R. Allow the plate to dry in air, spray with ninhydrin solution R and heat at 100 °C to 105 °C for 15 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). The test is not valid unless the chromatogram obtained with reference solution (c) shows two clearly separated spots. Chlorides (2.4.4). Dilute 5 mL of solution S to 15 mL with water R. The solution complies with the limit test for chlorides (200 ppm). Sulfates (2.4.13). Dilute 10 mL of solution S to 15 mL with distilled water R. The solution complies with the limit test for sulfates (300 ppm). Ammonium (2.4.1). 50 mg complies with limit test B for ammonium (200 ppm). Prepare the standard using 0.1 mL of ammonium standard solution (100 ppm NH4) R. Iron (2.4.9). In a separating funnel, dissolve 1.0 g in 10 mL of dilute hydrochloric acid R. Shake with three quantities, each of 10 mL, of methyl isobutyl ketone R1, shaking for 3 min each time. To the combined organic layers add 10 mL of water R and shake for 3 min. The aqueous layer complies with the limit test for iron (10 ppm). Heavy metals (2.4.8). Dissolve 2.0 g in water R and dilute to 20 mL with the same solvent. 12 mL of the solution complies with limit test A for heavy metals (10 ppm). Prepare the standard using lead standard solution (1 ppm Pb) R. 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 0.100 g in 3 mL of anhydrous formic acid R. Add 30 mL of anhydrous acetic acid R. Using 0.1 mL of naphtholbenzein solution R as indicator, titrate with 0.1 M perchloric acid until the colour changes from brownish-yellow to green. 1 mL of 0.1 M perchloric acid is equivalent to 10.51 mg of C3H7NO3. STORAGE Store protected from light. 01/2008:1148 corrected 6.1 SERTACONAZOLE NITRATE Sertaconazoli nitras C20H16Cl3N3O4S Mr 500.8 [99592-39-9] DEFINITION (RS)-1-[2-[(7-Chloro-1-benzothiophen-3-yl)methoxy]-2-(2,4- dichlorophenyl)ethyl]-1H-imidazole nitrate. Content : 98.5 per cent to 101.0 per cent (anhydrous substance). CHARACTERS Appearance : white or almost white powder. Solubility : practically insoluble in water, soluble in methanol, sparingly soluble in ethanol (96 per cent) and in methylene chloride. IDENTIFICATION First identification: A, C. Second identification: A, B, D, E. A. Melting point (2.2.14) : 156 °C to 161 °C. B. Ultraviolet and visible absorption spectrophotometry (2.2.25). Test solution. Dissolve 0.1 g in methanol R and dilute to 100 mL with the same solvent. Dilute 10 mL of this solution to 100 mL with methanol R. Spectral range : 240-320 nm. Absorption maxima : at 260 nm, 293 nm and 302 nm. Absorbance ratio : A302/A293 = 1.16 to 1.28. C. Infrared absorption spectrophotometry (2.2.24). Preparation : dry the substances at 100-105 °C for 2 h and examine as discs of potassium bromide R. Comparison : sertaconazole nitrate CRS. D. Thin-layer chromatography (2.2.27). Solvent mixture : concentrated ammonia R, methanol R (10:90 V/V). Test solution. Dissolve 40 mg of the substance to be examined in the solvent mixture and dilute to 10 mL with the solvent mixture. Reference solution (a). Dissolve 40 mg of sertaconazole nitrate CRS in the solvent mixture and dilute to 10 mL with the solvent mixture. Reference solution (b). Dissolve 20 mg of miconazole nitrate CRS in reference solution (a) and dilute to 5 mL with reference solution (a). Plate : TLC silica gel G plate R. 2894 See the information section on general monographs (cover pages) EUROPEAN PHARMACOPOEIA 7.0 Sertraline hydrochloride Mobile phase : concentrated ammonia R, toluene R, dioxan R (1:40:60 V/V/V). Application : 5 μL. Development : over a path of 15 cm. Drying : in a current of air for 15 min. Detection : expose to iodine vapour for 30 min. System suitability : reference solution (b) : — the chromatogram shows 2 clearly separated spots. Results : the principal spot in the chromatogram obtained with the test solution is similar in position, colour and size to the principal spot in the chromatogram obtained with reference solution (a). E. About 1 mg gives the reaction of nitrates (2.3.1). TESTS Appearance of solution. The solution is clear (2.2.1) and not more intensely coloured than reference solution Y5 (2.2.2, Method II). Dissolve 0.1 g in ethanol (96 per cent) R and dilute to 10 mL with the same solvent. Related substances. Liquid chromatography (2.2.29). Test solution. Dissolve 10.0 mg of the substance to be examined in the mobile phase and dilute to 10.0 mL with the mobile phase. Reference solution (a). Dilute 5.0 mL of the test solution to 100.0 mL with the mobile phase. Dilute 1.0 mL of this solution to 20.0 mL with the mobile phase. Reference solution (b). Dissolve 5.0 mg of sertaconazole nitrate CRS and 5.0 mg of miconazole nitrate CRS in the mobile phase and dilute to 20.0 mL with the mobile phase. Dilute 1.0 mL of this solution to 50.0 mL with the mobile phase. Column : — size : l = 0.25 m, Ø = 4.0 mm; — stationary phase : nitrile silica gel for chromatography R1 (10 μm). Mobile phase : acetonitrile R1, 1.5 g/L solution of sodium dihydrogen phosphate R (37:63 V/V). Flow rate : 1.6 mL/min. Detection : spectrophotometer at 220 nm. Injection : 20 μL. Run time : 1.3 times the retention time of sertaconazole. Retention time : nitrate ion = about 1 min ; miconazole = about 17 min; sertaconazole = about 19 min. System suitability : reference solution (b) : — resolution : minimum 2.0 between the peaks due to miconazole and sertaconazole. Limits : — impurities A, B, C : for each impurity, not more than the area of the principal peak in the chromatogram obtained with reference solution (a) (0.25 per cent) ; — total : not more than twice the area of the principal peak in the chromatogram obtained with reference solution (a) (0.5 per cent) ; — disregard limit : 0.2 times the area of the principal peak in the chromatogram obtained with reference solution (a) (0.05 per cent ) ; disregard the peak due to the nitrate ion. Water (2.5.12) : maximum 1.0 per cent, determined on 0.50 g. Sulfated ash (2.4.14) : maximum 0.1 per cent, determined on 1.0 g. ASSAY Dissolve 0.400 g in 50 mL of a mixture of equal volumes of anhydrous acetic acid R and methyl ethyl ketone R. Titrate with 0.1 M perchloric acid, determining the end-point potentiometrically (2.2.20). Carry out a blank titration. 1 mL of 0.1 M perchloric acid is equivalent to 50.08 mg of C20H16Cl3N3O4S. STORAGE Protected from light. IMPURITIES Specified impurities : A, B, C. A. (1RS)-1-(2,4-dichlorophenyl)-2-(1H-imidazol-1-yl)ethanol, B. R = Br : 3-(bromomethyl)-7-chloro-1-benzothiophen, C. R = OH: (7-chloro-1-benzothiophen-3-yl)methanol. 01/2011:1705 SERTRALINE HYDROCHLORIDE Sertralini hydrochloridum C17H18Cl3N Mr 342.7 [79559-97-0] DEFINITION (1S,4S)-4-(3,4-Dichlorophenyl)-N-methyl-1,2,3,4- tetrahydronaphthalen-1-amine hydrochloride. Content : 97.5 per cent to 102.0 per cent (anhydrous substance). CHARACTERS Appearance : white or almost white, crystalline powder. Solubility : slightly soluble in water, sparingly soluble or slightly soluble in anhydrous ethanol, slightly soluble in acetone and in 2-propanol. It shows polymorphism (5.9). IDENTIFICATION Carry out either tests A, B, C or tests B, C, D. A. Specific optical rotation (2.2.7) : + 38.8 to + 43.0 (anhydrous substance), measured at 25 °C. Solvent mixture. Dilute 1 volume of a 103 g/L solution of hydrochloric acid R to 20 volumes with methanol R. Dissolve 0.250 g in the solvent mixture and dilute to 25.0 mL with the solvent mixture. B. Infrared absorption spectrophotometry (2.2.24). Comparison : sertraline hydrochloride CRS. If the spectra obtained in the solid state show differences, record new spectra using 10 g/L solutions in methylene chloride R. C. Dissolve 10 mg in 5 mL of anhydrous ethanol R and add 5 mL of water R. The solution gives reaction (a) of chlorides (2.3.1). D. Enantiomeric purity (see Tests). General Notices (1) apply to all monographs and other texts 2895 2_Volume2_E.pdf 44-S-E.pdf toc Serinum TESTS Solution S. Dissolve 2.5 g in distilled water R and dilute to 50 Appearance of solution. Solution S is clear (2.2.1) and not more Specific optical rotation (2.2.7). Dissolve 2.50 g in dilute hyd Ninhydrin-positive substances. Examine by thin-layer chromatogra Chlorides (2.4.4). Dilute 5 mL of solution S to 15 mL with water Sulfates (2.4.13). Dilute 10 mL of solution S to 15 mL with dist Ammonium (2.4.1). 50 mg complies with limit test B for ammonium Iron (2.4.9). In a separating funnel, dissolve 1.0 g in 10 mL of Heavy metals (2.4.8). Dissolve 2.0 g in water R and dilute to 20 Loss on drying (2.2.32). Not more than 0.5 per cent, determined Sulfated ash (2.4.14). Not more than 0.1 per cent, determined on ASSAY STORAGE Sertaconazole nitrate Sertaconazoli nitras DEFINITION CHARACTERS IDENTIFICATION TESTS Appearance of solution. The solution is clear (2.2.1) and not mo Related substances. Liquid chromatography (2.2.29). Water (2.5.12): maximum 1.0 per cent, determined on 0.50 g. Sulfated ash (2.4.14): maximum 0.1 per cent, determined on 1.0 g ASSAY STORAGE IMPURITIES Sertraline hydrochloride Sertralini hydrochloridum DEFINITION CHARACTERS IDENTIFICATION