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;)
434.51
,16
)-.
,16,17,21-tetrahydroxypregna-1,4-diene-3,20-dione cyclic 16,17-acetal with acetone
[76-25-5].
, excursions permitted between 15 and 30.
197K
: recrystallized from methanol.
781S:
between +118 and +130.
731—
Dry it in vacuum at 60 for 4 hours: it loses not more than 1.5% of its weight.
until thoroughly charred. Cool, add to the contents of the crucible 5 drops of sulfuric acid and 2 mL of nitric acid, cautiously heat until reaction has ceased, then ignite in a muffle furnace at 500 to 600 until the carbon is entirely burned off. Cool, add 2 mL of hydrochloric acid, and slowly evaporate on a steam bath to dryness. Moisten the residue with 1 drop of hydrochloric acid and 5 mL of hot water, and digest for 2 minutes. Add 1 drop of phenolphthalein TS, then add 6 N ammonium hydroxide dropwise until the reaction is alkaline. Render the solution acid with 1 N acetic acid, then add 1 mL of excess, transfer to a beaker, and add water to make 10 mL. Pipet 2.5 mL (equivalent to 25 µg of lead) of Standard Lead Solution (see Lead 231) into a second beaker, add 3 mL of water and 1 drop of phenolphthalein TS, render just alkaline with 6 N ammonium hydroxide, then render acid with 1 N acetic acid, and add 1 mL in excess. Dilute with water to 10 mL. To each beaker add 5 mL of freshly prepared hydrogen sulfide TS, mix, and allow to stand for 5 minutes. Pass each solution through a separate, acid-resistant, white, plain membrane filter of 0.22-µm pore size and 25 mm in diameter, collecting the precipitates on the filter disks: the color of the precipitate from the solution under test is not darker than that from the control. The heavy metals limit is 0.0025%.
621).
621)—
The liquid chromatograph is equipped with a 254-nm detector and a 3.9-mm × 30-cm column that contains packing L1. The flow rate is about 1.5 mL per minute. Chromatograph the Test solution, and record the peak responses as directed for Procedure: the resolution, R, between triamcinolone acetonide and any impurity peak is not less than 1.0.
467:
meets the requirements.
621) operated at room temperature, by means of a suitable microsyringe or sampling valve. Adjust the operating parameters with Mobile phase on the column so that the separation of triamcinolone acetonide and internal standard is optimized, with a retention time of about 14.5 minutes for triamcinolone acetonide. Typically, the apparatus is fitted with a 4-mm × 30-cm column containing packing L1 and is equipped with a UV detector capable of monitoring absorbance at 254 nm, and a suitable recorder. In a suitable chromatogram, the coefficient of variation for five replicate injections of a single specimen is not more than 3.0%; and the resolution factor, R (see Chromatography 621), between the peaks for triamcinolone acetonide and fluoxymesterone is not less than 2.0. Measure the heights of the internal standard and triamcinolone acetonide peaks at the same retention times obtained from the Assay preparation and the Standard preparation. Calculate the quantity, in mg, of C24H31FO6 in the portion of Triamcinolone Acetonide taken by the formula: