A polarographic method and an ultraviolet irradiation method for the determination of dienestrol in pharmaceuticals are presented. Both methods are capable of producing results of a hi her degree of accuracy and precision than those oftainable by the U.S.P. XVI method.
VARIETY OF methods have been proposed for A the determination of the synthetic estrogens including nitration, diazotization, reduction, and the formation of addition compounds (1-9).
Wessely and Wratil (10) and Goulden and Warren (11) determined cis-and trans-stilbene polarographically; however, a#-dimethylstilbene, diethylstilbestrol, and dienestrol were not reduced polarographically. Gry (12) polarographically determined dienestrol and diethylstilbestrol in addition to some steroidal estrogens by means of their nitroso derivatives according t o the methods reported by Baggesgaard-Rasmussen (13-17).
Gottlieb (18) presented basic data on the nitrosophenol reaction for several synthetic estrogens and subsequently developed a colorimetric procedure for the determination of diethylstilbestrol in pharmaceuticals (19). Goodyear et al. (20) introduced an ultraviolet irradiation technique for the determination of diethylstilbestrol in tablets which was later modified by Banes (Zl), who observed that dienestrol also produced a yellow color upon ultraviolet irradiation. The U.S.P. XVI procedure for dienestrol in tablets utilizes the Folin-Denis reagent in a colorimetric procedure. This reaction is not particularly specific because difficulties are encountered in the presence of reducing substances. This investigation was undertaken in an effort to develop a method of greater specificity than that based on the Folin-Denis color reaction. EXPERIMENTAL Polarographic Assay Apparatus Sargent niodel XX L recording polar~~graph : both the large (X-rnl. sample volume) and s n d ( 3 -d . sample volume) H-type cells were used. The saturated calomel electrode (SCE) is separated from the sample compartment by an agar plug and fritted