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Friday, July 10, 2009

contains 40,000 Units of antirachitic activity (vitamin D) in each mg]. Storage: Store in tightly-closed, light-resistant containers in

C28 H44 O in ergocalciferol RS, as appropriate. Determine the weight per ml of the oral solution, Appendix 8. 15, and calculate the percentage of cholecalciferol or ergocalciferol, weight in volume. CALCIFEROL TABLETSCalciferol Tablets contain Cholecalciferol or Ergocalciferol. Usual strengths: 250 pg; 1. 25 mg. [Cholecalciferol or Ergocalciferol contains 40,000 Units of antirachitic activity (vitamin D) in each mg]. Storage: Store in tightly-closed, light-resistant containers in a cool place. STANDARDSCalciferol Tablets contain not less than 90. 0 per cent and not more than 125. 0 per cent of the stated amount of cholecalciferol, C27H440 or ergocalciferol, C28H44d. Identification: Powder a tablet, extract with 5 ml of ethanol free chloroform, filter and to 1 ml of the filtrate add 9 ml of antimony trichloride solution; a brownish-red colour is produced. Uniformity of content: Comply with the requirements stated under Tablets using the following method of analysis. Carry out the Assay described under Ergocalciferol using the following solutions. Solution (1) is prepared in the following manner For tablets containing less than 250 ug, add 2 ml of water to one tablet in an amber-coloured flask and disperse with the aid of ultrasound. Add 6 ml of dimethyl sulphoxide, mix, extract with 25 ml of hexane by shaking for 30 minutes, centrifuge the hexane layer and use the clear supernatant liquid. For tablets containing more than 250 ug prepare the solution in the same manner but using 4 ml of water, 12 ml of dimethyl sulphoxide and 100 ml of hexane. Solution (2) contains 0.001% w/v of cholecalciferol RS or ergocalciferol RS, as appropriate, in hexane. For solution (3) dissolve 0. 5 g of cholecalciferol RS or ergocalciferol RS, as appropriate, in 2 ml of toluene, dilute to 10 ml with the mobile phase, heat under a reflux condenser in awater-bath at 90" for 45 minutes and cool. Calculate the content of cholecalciferol, C271-1440, or ergocalciferol, CssM^d, from the declared content Of C271-1440 in cholecalciferol RS or of C28h44o in ergocalciferol RS, as appropriate, and using peak heights. Other requirements; Comply with the requirements of tests stated under Tablets. Assay; Carry out the following procedure as rapidly as possible in subdued light and protected from air. Weigh and powder 20 or more tablets as required. Weigh accurately a quantity of the powder equivalent to about 6 mg of Ergocalciferol or Cholecalciferol, add 50 ml of ethanol (95%), 14 ml of glycerin and 20 ml of a 50% w/v solution of potassium hydroxide. Boil under a reflux condenser for 30 minutes, stirring occasionally, add 110 ml of water and allow to stand for 10 minutes with occasional stirring and carry out the Assay described under Calciferol Capsules beginning at the words "Cool and add sufficient ethanol (95%).... ". Calculate the content of cholecalciferol or ergocalciferol, in mg, from the average value so obtained and from the amount of cholecalaiferol or ergocalciferol in the reference solution and from the declared content of C27H44O in cholecalciferol RS or of C?SH440 in ergocalciferol RS, as appropriate. CALCIUM CARBONATE Precipitated ChalkCaC03 Mol. Wt 100. 09 Category: Antacid; pharmaceutical aid (excipient) Dose: 1 to 5 g. Description: Fine, white; microcrystallme powder. Solubility: Practically insoluble in water and in ethanol (95%), slightly soluble in water containing carbon dioxide, or any ammonium salt. It is soluble with effervescence. in dilute acids S.torage: Store in well-closed containers. STANDARDSCalcium. Carbonate contains not less than 98. 0 per cent and not more than 100. 5 per cent of CaC03, calculated with reference to the dried substance. Identification: A: Dissolve 5.0 g in 80 ml of 2M acetic acid. When effervescence ceases, boil the solution for 2 minutes, allow to cool, dilute to 100 ml with 2M acetic acid and filter, if necessary, through a smtered-glass filter reserving any residue for the test for Substances insoluble in acetic acid; 0. 2 ml of the filtrate (solution A) gives reactions A and B o1 calcium salts, Appendix 3. 1. B: Gives reaction A of carbonates, Appendix 3. 1. Substances insoluble in acetic acid: Wash any residue obtained in Identification test A with four quantities, each of 5 ml, of hot water and dry at 100° for 1 hou;, the residue weighs not more than 10 mg (0 2%) Arsenic: Dissolve 2. 5 g in 15 ml of brommated hydrochloric acid and 45 ml of water and remove the excess of bromine with a few drops of stannous chloride solution AsT. The resulting solution complies with the limit test for arsenic, Appendix 3. 9 (4 ppm). Heavy metals: Not more than 20 ppm, determined by Method A on a solution prepared in the following manner. To 1 g add 5 ml of water, and 8 ml of dilute hydrochloric acid, the latter being added slowly, shake and evaporate to dry ness on a water-bath. Dissolve the residue in 20 ml of water, filter, add to the filtrate 3 ml of dilute acetic acid and water to make 25 ml, Appendix 3. 12. Barium: Dissolve 0. 6 g in 10 ml of 2M acetic acid by boiling, cool and add 10 ml of calcium sulphate solution; the solution remains clear for not less than 15 minutes. Iron: Dissolve 0. 2 g in 5 ml water and 0. 5 ml of iron-free hydrochloric acid, boil and dilute to 40 ml with water, the solution complies with the limit test for iron, Appendix 3: 13 (200 PPm). Magnesium and alkali.metals: Dissolve 1. 0 g in 10 ml of dilute hydrochloric acid, neutralise the solution by adding dilute ammonia solution, heat the solution to boiling and add 50 ml of hot ammonium oxalate solution. Cool, dilute to 100 ml with water and

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