Comparison of capillary gas chromatographic method and automatedspectrophotofluorometric methods for measuring content uniformity of conjugatedoestrogens in pharmaceutical preparations

摘要

To measure the content uniformity of conjugated cestrogens tablets, the USP XXII monograph specifies a capillary gas chromatographic method. This involves separation of the trimethylsilyl derivatives of the various oestrogens found in a typical conjugated oestrogens tablet using a fused-silica 0V 225 bonded phase column. Hydrogen is used as the carrier gas with FID detection. A more rapid spectrophotofluorometric method of analysis has been developed in which the oestrogens are extracted from the dosage form into water, then transferred into organic solvent as the dicyclohexylamine complex. Fluorescence is developed by heating the solution of the complex in the presence of 70% sulphuric acid. The chemistry and detection are carried out using a segmented-flow analyser.The spectrophotofluorometric method is preferred as a routine control for content uniformity because considerable time is saved during sample preparation and analysis compared to gas chromatography. Coefficients of variation show that both methods produce acceptable results. These results fall well within the USP XXII [1] monograph, limits and also well within the tighter limits imposed by the USP XXII, section 905.