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Marbofloxacin 在欧洲药典 EP 6.1 版 3496页 谢谢虫友。愿意拿三十金币求助 [ Last edited by shich68 on 2008-12-23 at 15:37 ] |
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2楼2008-12-23 15:51:29
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shich68(金币+2,VIP+0):新药版送上圣诞红包!欢迎继续支持新药版!
shich68(金币+2,VIP+0):新药版送上圣诞红包!欢迎继续支持新药版!
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DEFINITION 9-Fluoro-3-methyl-10-(4-methylpiperazin-1-yl)-7-oxo-2,3- dihydro-7H-pyrido[3,2,1-ij][4,1,2]benzoxadiazine-6-carboxylic acid. Content: 99.0 per cent to 101.0 per cent (dried substance). CHARACTERS Appearance: light yellow, crystalline powder. Solubility : slightly soluble in water, sparingly soluble or slightly soluble in methylene chloride, very slightly soluble in ethanol (96 per cent). IDENTIFICATION Infrared absorption spectrophotometry (2.2.24). Comparison : marbofloxacin CRS. TESTS Absorbance (2.2.25) : maximum 0.20, determined at 450 nm. Dissolve 0.400 g in borate buffer solution pH 10.4 R and dilute to 10.0 ml with the same buffer solution. Related substances. Liquid chromatography (2.2.29). Carry out the test protected from light. Solvent mixture : methanol R, water R (23:77 V/V). Test solution. To 0.100 g of the substance to be examined add 80 ml of the solvent mixture, sonicate until dissolution and dilute to 100.0 ml with the solvent mixture. Reference solution (a). Dilute 5.0 ml of the test solution to 100.0 ml with the solvent mixture. Dilute 1.0 ml of this solution to 50.0 ml with the solvent mixture. Reference solution (b). Dissolve 10 mg of marbofloxacin for peak identification CRS (containing impurities A, B, C, D and E) in the solvent mixture and dilute to 10 ml with the solvent mixture. Column: — size: l = 0.15 m, Ø = 4.6 mm; — stationary phase: end-capped polar-embedded octadecylsilyl amorphous organosilica polymer R (3.5 μm); — temperature: 40 °C. Mobile phase: mix 230 volumes of methanol R and 5 volumes of glacial acetic acid R with 770 volumes of a 2.70 g/l solution of sodium dihydrogen phosphate R containing 3.50 g/l of sodium octanesulphonate R and previously adjusted to pH 2.5 with phosphoric acid R. Flow rate: 1.2ml/min. Detection: spectrophotometer at 315 nm. Injection: 10 μl. Run time: 2.5 times the retention time of marbofloxacin. Relative retention with reference to marbofloxacin (retention time = about 33 min) : impurity B = about 0.5 ; impurity A = about 0.7 ; impurity C = about 0.9 ; impurity D = about 1.3; impurity E = about 1.5. System suitability : reference solution (b) : — resolution: minimum 1.5 between the peaks due to impurity C and marbofloxacin, and minimum 4.0 between the peaks due to marbofloxacin and impurity D. Limits : — correction factor : for the calculation of content, multiply the peak area of impurity E by 1.5; — impurities C, D, E: for each impurity, not more than twice the area of the principal peak in the chromatogram obtained with reference solution (a) (0.2 per cent) ; — impurities A, B: for each impurity, not more than the area of the principal peak in the chromatogram obtained with reference solution (a) (0.1 per cent) ; — unspecified impurities : for each impurity, not more than twice the area of the principal peak in the chromatogram obtained with reference solution (a) (0.2 per cent) ; — total : not more than 5 times the area of the principal peak in the chromatogram obtained with reference solution (a) (0.5 per cent) ; — disregard limit : the area of the principal peak in the chromatogram obtained with reference solution (a) (0.1 per cent). Heavy metals (2.4.8) : maximum 20 ppm. Dissolve 0.5 g in dilute acetic acid R and dilute to 30 ml with the same solvent. Adding 2 ml of water R instead of 2 ml of buffer solution pH 3.5 R, the filtrate complies with test E. Prepare the reference solution using 5 ml of lead standard solution (2 ppm Pb) R. Loss on drying (2.2.32) : maximum 0.5 per cent, determined on 1.000 g by drying at 105 °C for 4 h. Sulphated ash (2.4.14) : maximum 0.1 per cent, determined on 1.0 g in a platinum crucible. ASSAY Dissolve 0.300 g in 80 ml of glacial acetic acid R. Titrate with 0.1 M perchloric acid, determining the end-point potentiometrically (2.2.20). 1 ml of 0.1 M perchloric acid is equivalent to 36.24 mg of C17H19FN4O4. STORAGE Protected from light. [ Last edited by shich68 on 2008-12-23 at 16:31 ] |
3楼2008-12-23 15:54:42
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