Troleandomycin
;)
Oleandomycin,triacetate (ester).
Triacetyloleandomycin [2751-09-9].
»Troleandomycin contains the equivalent of not less than 750µg of oleandomycin (C35H61NO12)per mg.
Packaging and storage—
Preserve in tight containers.
Identification—
A:
Dissolve about 10mg in 5mLof hydrochloric acid,and heat in a water bath:a greenish yellow color is produced.
B:
Prepare a solution of it in methanol containing 10mg per mL.Apply 5µLof this test solution,5µLof a methanol solution of USP Troleandomycin RScontaining 10mg per mL(Standard solution),and 5µLof a mixture of the two solutions (1:1)to a suitable thin-layer chromatographic plate (see Chromatography á621ñ)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 (1in 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 20minutes,and locate the spots:the RFvalue 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 á695ñ:
meets the requirements.
pHá791ñ:
between 7.0and 8.5,in a solution of alcohol and water (1:1)containing 100mg per mL.
Loss on drying á731ñ—
Dry about 100mg in vacuum at a pressure not exceeding 5mm of mercury at 60
for 3hours:it loses not more than 1.0%of its weight.
for 3hours:it loses not more than 1.0%of its weight.
Residue on ignition á281ñ:
not more than 0.1%.
Content of acetyl—
Transfer about 30mg,accurately weighed,to a three-neck,ground-glass jointed 50-mLflask 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 2mLof methanol to the flask to dissolve the Troleandomycin,and,slowly with swirling,add 1mLof 2Nsodium hydroxide and a boiling chip.Allow nitrogen to flow into the flask at a rate of about 2bubbles per second.Add about 5mLof water to the funnel,and heat the flask.Allow to reflux for 30minutes.Allow the assembly to cool slightly,and rinse the condenser with about 3mLof 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 5mLadded to the flask.Heat the flask,and collect about 5mLof distillate in about 10minutes.Discard the distillate,and allow the flask to cool slightly.Add 1mLof 12Nsulfuric acid to the flask through the funnel.Heat the flask,and collect about 20mLof distillate in about 20minutes,adding more water from time to time through the funnel to maintain the volume in the flask at about 2to 3mL.As the distillation proceeds,treat the first fraction as follows.Boil gently for about 20seconds,and add a few drops of barium chloride TS:no turbidity is produced.Add 1drop of phenolphthalein TS,and titrate the solution with 0.015Nsodium hydroxide VSuntil 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 20seconds.”If the second fraction consumes more than 0.1mLof 0.015Nsodium hydroxide,collect a third,10-mL,fraction,and treat as directed for the first fraction,beginning with “Boil gently for about 20seconds.”Each mLof 0.015Nsodium hydroxide is equivalent to 0.6458mg of CH3CO:between 15.3%and 16.0%is found.
Assay—
Proceed with Troleandomycin as directed for troleandomycin under Antibiotics—Microbial Assays á81ñ.
Auxiliary Information—
Staff Liaison:William W.Wright,Ph.D.,Scientific Fellow
Expert Committee:(PA7)Pharmaceutical Analysis 7
USP28–NF23Page 1996
Phone Number:1-301-816-8335