» Troleandomycin contains the equivalent of not less than 750 µg of oleandomycin (C35H61NO12) per mg.
Packaging and storage Preserve in tight containers.
A: Dissolve about 10 mg in 5 mL of hydrochloric acid, and heat in a water bath: a greenish yellow color is produced.
B: Prepare a solution of it in methanol containing 10 mg per mL. Apply 5 µL of this test solution, 5 µL of a methanol solution of USP Troleandomycin RS containing 10 mg per mL (Standard solution), and 5 µL of a mixture of the two solutions (1:1) to a suitable thin-layer chromatographic plate (see Chromatography 621) coated with a 0.25-mm layer of chromatographic cellulose. Allow the spots to dry, and develop the chromatogram in a solvent system of ammonium carbonate solution (1 in 100) until the solvent front has moved three-fourths of the length of the plate. Remove the plate from the developing chamber, mark the solvent front, and allow the plate to dry. Expose the plate to iodine vapors in a closed chamber for about 20 minutes, and locate the spots: the RF value of the principal spot obtained from the test solution and from the mixture of the test solution and the Standard solution corresponds to that obtained from the Standard solution.
Crystallinity 695: meets the requirements.
pH 791: between 7.0 and 8.5, in a solution of alcohol and water (1:1) containing 100 mg per mL.
Loss on drying 731 Dry about 100 mg in vacuum at a pressure not exceeding 5 mm of mercury at 60 for 3 hours: it loses not more than 1.0% of its weight.
Residue on ignition 281: not more than 0.1%.
Content of acetyl Transfer about 30 mg, accurately weighed, to a three-neck, ground-glass jointed 50-mL flask fitted with a glass-stoppered funnel in the center neck, and a condenser and a gas inlet with a bubble counter in the other two necks. Add 2 mL of methanol to the flask to dissolve the Troleandomycin, and, slowly with swirling, add 1 mL of 2 N sodium hydroxide and a boiling chip. Allow nitrogen to flow into the flask at a rate of about 2 bubbles per second. Add about 5 mL of water to the funnel, and heat the flask. Allow to reflux for 30 minutes. Allow the assembly to cool slightly, and rinse the condenser with about 3 mL of water, collecting the rinsings in the flask. Change the condenser to the distillation position, and add water from the funnel to make a total of 5 mL added to the flask. Heat the flask, and collect about 5 mL of distillate in about 10 minutes. Discard the distillate, and allow the flask to cool slightly. Add 1 mL of 12 N sulfuric acid to the flask through the funnel. Heat the flask, and collect about 20 mL of distillate in about 20 minutes, adding more water from time to time through the funnel to maintain the volume in the flask at about 2 to 3 mL. As the distillation proceeds, treat the first fraction as follows. Boil gently for about 20 seconds, and add a few drops of barium chloride TS: no turbidity is produced. Add 1 drop of phenolphthalein TS, and titrate the solution with 0.015 N sodium hydroxide VS until a permanent pale pink color is produced. Collect a second, 10-mL, fraction, and treat it as directed for the first fraction, beginning with Boil gently for about 20 seconds. If the second fraction consumes more than 0.1 mL of 0.015 N sodium hydroxide, collect a third, 10-mL, fraction, and treat as directed for the first fraction, beginning with Boil gently for about 20 seconds. Each mL of 0.015 N sodium hydroxide is equivalent to 0.6458 mg of CH3CO: between 15.3% and 16.0% is found.
Assay Proceed with Troleandomycin as directed for troleandomycin under AntibioticsMicrobial Assays 81.
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USP32NF27 Page 3821