A Warm a quantity of the powdered tablets equivalent to 10 mg of Busulphan with 10 ml of acetone

with 50 ml of water Boil under a reflux condenser for 30 minutes and, if necessary, restore the initial volume with water Allow to cool and titrate with 0.1M sodium hydroxide, using 0.3 ml of dilute phenolphthalein solution as indicator, until a pink colour is produced Each ml of 0.1M sodium hydroxide is equivalent to 0.01232 g of C4H14O6S2 BUSULPHAN TABLETS Usual strength 2 mg Storage: Store in well-dosed, light-resist ant containers. STANDARDSBusulphan Tablets contain not less than 90 0 per cent and not more than 115.0 per cent of the stated amount of busulphan. C6H14O6S2 The tablets are coated Identification: A Warm a quantity of the powdered tablets equivalent to 10 mg of Busulphan with 10 ml of acetone, filter and evaporate the filtrate to dryness. Dry the residue at 60° at a pressure not exceeding 0.7 kPa for 1 hour The infra-red absorption spectrum of the residue, Appendix 5. 4. is concordant with the reference spectrum of busulphan or with the spectrum obtained from busulphan RS.B: In the Assay, the principal peak in the chromatogram obtained with solution (1) has the same retention time as that of the peak in the chromatogram obtained with solution (2) Disintegration Maximum time, 15 minutes, Appendix 7.1. Uniformity of content. Comply with the requirements stated under Tablets using the following method of analysis. Carry out the method for gas chrornatography. Appendix 4.2, using the following solutions For solution (1) add 1 ml of water to one tablet in a 50-m1 volumetric flask and place in an ultrasonic bath until completely dispersed. Add 30 ml of acetone, shake for 15 minutes and dilute to 50.0 ml with acetone Centrifuge and dilute a quantity of the supernatant liquid with acetone to produce a solution containing 0.0001 % w/v of Busulphan To 5.0 ml of the resulting solution add 5 ml of a 30% w/v solution of sodium iodide in acetone, stopper the flask lightly and heat in a water-bath at 50° for 90 minutes Cool, add 10 ml of a 0.0001% w/v solution of 1,5-di-iodopentane (internal standard) in acetone, mix. add 10 ml of water and 20 ml of hexane, shake vigorously for 1 minute and allow to separate Use the hexane layer For solution (2) add 5 ml of a 30% w/v solution of sodium iodide in acetone to 5 ml of a 0.0001% w/v solution of busulphan RS in acetone, stopper the flask lightly and heat in a water-bath at 50° for 90 minutes Cool, add 10 ml of the internal standard solution, mix. add 10 ml of water and 20 ml of hexane, shake vigorously for 1 minute and allow to separate. Use the hexane layer Prepare solution (3)- in the same manner as solution (2) but using 10 ml. of acetone in place of internal standard solution The chromalographic procedure may be carried out using a glass column (1 5 m x A mm) packed with acid-washed, diatomaceous support (30 to 100 mesh) coated with 3% w/v of phenyl methyl silicone fluid (50% phenyl), maintained at 1 40° and an electron capture detector.Calculate the content of C6H14O6S2) from the declared content of C6H14Q5S2 in busulphan RS Other requirements: Comply with the requirements of tests staled under Tablets Assay. Weigh and powder 20 tablets Carry out the method of analysis described under Uniformity of content but preparing solution (1) in the following manner Weigh accurately a quantity of Ihe powdered tablets equivalent to 2.5 mg of Busulphan. add 5 ml of water and place in an ultrasonic bath until completely dispersed Add 150 ml of acetone, shake for 15 minutes and dilute to 250.0 ml with acetone Centrifuge and dilute 10.0 ml of the supernatant liquid to 100.0 ml with acetone To 5.0 ml of the resulting solution add 5 ml of a 30% solution of sodium iodide in acetone, stopper the flask lightly and heat in a water- bath at 50° for 90 minutes. Cool, add 10 ml of the internal standard solution, mix. add 10 ml of water and 20 ml of hexane, shake vigorously for 1 minute and allow to separate. Use the hexane layer Calculate the content of from the declared content of C6Hl4O6S2 in busulphan RS BUTYLATED HYDRQXYAWISOLE Mol. Wt. 180.25 Butylated Hydroxyanisole is 1,1-dimethylethyl-4-methoxyphenol containing a variable amount of 2,2-dimethylethyl4-methoxyprienol.Category Pharmaceutical aid (antioxidant).Descriptioin White or almost white, crystalline powder or yellowish-white, waxy solid, odour, aromatic Solubility Freely soluble in ethanol 05%), in 1,2-propanediol, in arachis oil and in solutions of alkali hydoxides; practically insoluble in water.Storage Store in welt-dosed, light-resistant containers. STANDARDS Identification A Dissolve about 01 g m 10 ml of ethanol (95%), add 2 ml of a 2 0% w/v solution of sodium tetraborate and a few crystals of2.6dichloquinone-4-chlorimide, a blue colour is produced (distinction from butylated hydroxytolueneJ.B Dissolve a few crystals in 10 ml of ethanol (95%), add 0.5 ml of a 0.2% w/v solution of potassium ferr.cyanide and 0.5 ml of a 05% w/v solution of ferric ammonium sulphate in 0.5M sulphuric acid; a green to blue colour is produced C Melts between 62"and 65°. Appendix 8.8 Hydroquinone. Carry out the method for thin-layer chromatography, Appendix 4.6. using silica gel G as the costing substance and a mixture of 4 volumes of chloroform and 1 volume of ethyl acetate as the mobile phase Apply separately to the plate 3 P1 of each of two solutions in ether containing (1)5.0% w/v of the substance being examined and (2) 0.01% w/v of hydroqunione After removal of the plate, allow it to dry in air for a few