Friday, July 10, 2009

add this solution to the prepared silamsed diatomaceous support and evaporate the solvent under reduced pressure

mixture. Dissolve over a 5-hourperiod 0.4 g of low-vapour pressure hydrocarbons (type L) (such as Apiezon L) in 60 ml of toluene, add this solution to the prepared silamsed diatomaceous support and evaporate the solvent under reduced pressure while slowly rotating the mixture. Allow the temperature of the column to increase from 100° to 200° at a constant rate of 6' per minute with the inlet port at 220° and the detector at 300° .Use a flow rate of 30 ml per minute for the carrier gas. Record the chromatogram for at least 2 5 times the retention time of the principal peak The area of any secondary peak is not greater than 0.3% and the sum of the areas of any secondary peaks is not greater than 1 % by normalisation. Sulphated ash: Not more than 0.1 % Appendix 3.22. Water. Not more than 0 5% w/w, determined on 2 g, Appendix 3.24. Assay: Weigh accurately about 0.15 g, dissolve in a mixture of 5.0 ml of 0.01 M hydrochloric acid and 50 ml of ethanol (95%) and titrate with 0.1 M sodium hydroxide determining the end-point potentiometrically. Record the volume used between the two inflections. Each ml of 0.1M sodium hydroxide is equivalent to 0.01S77 g of C10H17,HCI AMANTADINE HYDROCHLORIDE CAPSULESUsual strength : 100 mg. Storage: Store in tightly-closed containers in a cool place. STANDARDSAmantadme Hydrochlonde Capsules contain not less than 95.0 per cent and not more than 105.0 per cent of the stated amount of amantadme hydrochlonde, C10H17N,HCI. Identification: To the contents of one capsule add 2 ml of pentane and shake well. Collect the undissolved solids on a smtered-glass filter, wash with two portions, each of 1 ml, of pentane and dry in air, the residue so obtained complies with the tests described under Amantadme Hydrochlonde. Other requirements Comply with the requirements of tests stated under Capsules Assay Weigh accurately a quantity of the mixed contents of 20 capsules equivalent to about 0.12 g of Amantadme Hydrochlonde and warm in a mixture of 30 ml of anhydrous glacial acetic acid and 10 ml of mercuric acetate solution. Carry out Method B for non-aqueous titration, Appendix 3. 45, using crystal violet solution as indicator. Perform a blank determination and make any necessary correction . Each ml of 0 1M perchloric acid is equivalent to 0.01877 g of C10H17N,HCI. Amikacm is (S)-O-3-amino-3-deoxy- α -D-glucopyranosyl(6)-O-[6-amino-6-deoxy-α-D-glucopyranosyl(1 D4)]N"-(4-amino-2-ydroxy-l-oxobutyl)-2-deoxy-D-streptamine. Category: Antibacterial Dose By intramuscular or slow intravenous injection or by infusion, upto 1.5 g daily, in two divided doses. Description: White crystalline powder, almost odourless. Solubility Sparingly soluble in water. Storage: Store in tightly-closed containers. STANDARDSAmikacm contains not less than 9001µg of C22H43N5O13 per mg, calculated with reference to the anhydrous substance. Identification: A: Carry out the method for thin-layer chromatography, Appendix 4. 6, using silica gel G as the coating substance and a mixture of 60 volumes of methanol, 30 volumes of strong ammonia solution and 25 volumes of chloroform as the mobile phase. Apply separately to the plate 3 µl of each of the following solutions. Solution (1) is a 0.6% w/v solution of the substance being examined. Solution (2) is a 0.6% w/v solution of amikacm RS. Solution (3) is a mixture of equal volumes of solutions (1) and (2). After removal of the plate, allow it to dry in air, heat it at 110° for 15 minutes and immediately spray it with a 1 % w/v solution of mnhydrm in a mixture of 100 volumes of l-butanol and 1 volume of pyndine. The principal pink-coloured spot in the chromatogram obtained with solution (1) corresponds to those in the chromatograms obtained with solutions (2) and (3). B: To 1 ml of a 1 % w/v solution add 1 ml of 2M sodium hydroxide, mix and add 2 ml of a 1 % w/v solution of cobalt nitrate; a violet colour is produced. C: To a solution of 50 mg in 5 ml of water add 4 ml of a 0.035% w/v solution of anthrone in sulphuric acid; a bluish-violet colour is produced. pH: Between 9.5 and 11.5, determined in a 1 % w/v solution in carbon dioxide free water, Appendix 8.11. . Specific optical rotation: Between +97° and +105°, determined in a 2.0% w/v solution, Appendix 8.9. Sulphated ash: Not more than 1.0%, the charred residue being moistened with 2 ml of nitric acid and 5 drops of sulphuric acid, Appendix 3.22. Water: Not more than 8.5% w/w, determined on 0.2 g, Appendix 3.24 Assay Carry out the microbiological assay of antibiotics, Method B, Appendix 9.1, and express the result in µg of Amikacin, C22H43N5O13, per mg. (S)-O-3-amino-3-deoxy-a-D-glucopyranosyl-(1 □6)-O-[6-ammo-6-deoxy- -gluco-pyranosylN'-(4-amino-2-hydroxyoxobutyl)-2-deoxy-D-streptamine sulphate (1:2 or 1:1. 8)(salt). Category: Antibacterial. Dose: By intramuscular or slow intravenous injection or by infusion, upto 1.5 g daily, in two divided doses. Description: White

1 comment:

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