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Journal of Automatic Chemistry
Volume 13 (1991), Issue 3, Pages 115-117
http://dx.doi.org/10.1155/S1463924691000226

Comparison of capillary gas chromatographic method and automated spectrophotofluorometric methods for measuring content uniformity of conjugated oestrogens in pharmaceutical preparations

Analytical Research and Services, Wyeth-Ayerst Research, 64 Maple Street, Rouses Point, New York 12979, USA

Copyright © 1991 Hindawi Publishing Corporation. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

Abstract

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.