双氯芬酸钠bp2007

双氯芬酸钠bp2007 双氯芬酸钠 BP2007 Definition 按干燥品计，双氯芬酸钠含2-[(2,6-二氯苯基)氨基]苯基]醋酸钠的量为99.0%,101.0%。 性状 白色或微黄色结晶性粉末，具有轻微的吸湿性，少量溶于水，易溶于甲醇，可溶于酒精，微 溶于丙酮。 熔点在280?C，并且会分解。 鉴别 First identification A, D. Second identification B, C, D. A. 红外吸收光谱法检测 (2.2.24)，与双氯芬酸钠品比较，Examine the substances prepared as discs. B. 薄层色谱法检测 (2.2.27), 采用TLC硅胶GF254平板。 待测溶液 称量25 mg本品，用甲醇溶解，然后稀释到5 ml。 标准溶液 (a) 称量25 mg双氯芬酸钠标准品，用甲醇溶解，然后稀释到5ml。 标准溶液 (b) 称量10 mg吲哚美辛，用标准溶液(a)溶解并稀释至2 ml。 Apply to the plate 5 ml of each solution. Develop over a path of 10 cm using a mixture of 10 volumes of concentrated ammonia R, 10 volumes of methanol R and 80 volumes of ethyl acetate R. Allow the plate to dry in air. 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 reference solution (a). The test is not valid unless the chromatogram obtained with reference solution (b) shows 2 clearly separated spots. C. Dissolve about 10 mg in 10 ml of alcohol R. To 1 ml of the solution add 0.2 ml of a mixture, prepared immediately before use, of equal volumes of a 6 g/l solution of potassium ferricyanide R and a 9 g/l solution of ferric chloride R. Allow to stand protected from light for 5 min. Add 3 ml of a 10 g/l solution of hydrochloric acid R. Allow to stand, protected from light, for 15 min. A blue colour develops and a precipitate is formed. D. Dissolve 60 mg in 0.5 ml of methanol R and add 0.5 ml of water R. The solution gives reaction (b) of sodium (2.3.1). Tests Appearance of solution Dissolve 1.25 g in methanol R and dilute to 25.0 ml with the same solvent. The solution is clear (2.2.1). The absorbance (2.2.25) measured at 440 nm is not greater than 0.05. 有关物质 采用液相色谱实验(2.2.29). 待测溶液: 甲醇溶解50.0 mg本品，稀释到50.0 ml。 标准溶液(a): 吸取2.0 ml待测溶液，用甲醇稀释到100.0 ml。然后吸取1.0 ml，用甲醇稀释到10.0 ml。 标准溶液(b): 甲醇溶解1.0 mg的双氯芬酸杂质A标准品，加入1.0 ml待测溶液，然后用甲醇稀释至200.0 ml。 色谱程序: 柱子:0.25 m×4.6 mm，填充octylsilyl silica gel; 流动相:含有0.5 g/l 磷酸、0.8 g/l磷酸二氢钠的混合溶液34体积，用磷酸调节pH至 2.5， 与66 体积甲醇混合;流速:1 ml/min; 检测波长:254 nm. 注入20 ml的标准溶液(b)。双氯芬酸的保留时间约为25 min ，杂质A的约为12 min。调整 系统，使标准溶液(b)的峰高不低于满量程的一半，运行时间为双氯芬酸保留时间的1.5倍。 双氯芬酸和杂质A峰的分离度不低于6.5。 注入20 ml待测溶液和20 ml标准溶液(a)，检测溶液除主峰外的任意峰的峰面积均不得高于 标准溶液(a) (0.2%)主峰面积;除主峰外的所有峰的峰面积之和不得高于标准溶液(a) (0.5%) 主峰面积的2.5倍;标准溶液(a)中面积低于主峰面积0.25 倍的峰忽略不计。 Heavy metals (2.4.8) 2.0 g complies with limit test C (10 ppm). Use a quartz crucible. Prepare the standard using 2 ml of lead standard solution (10 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 100-105?C for 3 h. Assay Dissolve 0.250 g in 30 ml of anhydrous acetic acid R. Titrate with 0.1M perchloric acid, determining the end-point potentiometrically (2.2.20). 1 ml of 0.1M perchloric acid is equivalent to 31.81 mg of C14H10Cl2NNaO2. Storage In an airtight container, protected from light. Impurities A. 1-(2,6-dichlorophenyl)-1,3-dihydro-2H-indol-2-one, B. R1 = CHO, R2 = Cl: 2-[(2,6-dichlorophenyl)amino]benzaldehyde, C. R1 = CH2OH, R2 = Cl: [2-[(2,6-dichlorophenyl)amino]phenyl]methanol, D. R1 = CH2-CO2H, R2 = Br: 2-[2-[(2-bromo-6-chlorophenyl)amino]phenyl]acetic acid, E. 1,3-dihydro-2H-indol-2-one. Action and use Analgesic; anti-inflammatory. Preparations Diclofenac Tablets Slow Diclofenac Tablets