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Application of the Zimmermann reaction to paper chromatography of 17-keto steroids

Ľ. Stárka

Endokrinologisches Forschungsinstitut, Prag

 

Abstract: For paper-chromatographic sepn. of 17-keto steroids prior to colorimetric estn. by the Zimmermann reaction (Z.r.), 30% aq. triethylene glycol is best as the stationary phase, and petr. ether-CCl4 for the mobile phase. With dehydroepiandrosterone (I) as standard, 4 methods of quant. evaluation of chromatograms were tested: (a) elution, without detection, with MeOH, and colorimetric estn. of the evapd. sample by Z.r.; (b) detection by Z.r., elution with EtOH, and direct colorimetry; (c) detection by Z.r., elution with a mixt. of CHCl3 and 1% AcOH, evapn. of the eluate, repeated Z.r., and colorimetry after extn. into CHCl3; and (d) direct densitometry of spots 30 min. after detection by Z.r. and planimetric evaluation of the densitograms. For individual methods, standard deviations and coeffs. of variance for 20-γ samples of I were as follows: a (0.8, 4); b (1.0, 5); c (2.5, 12.5); d (1.5 γ, 7.5%). Although a is the most accurate, b and d are best suited for routine analysis.

Full paper in Portable Document Format: 178a550.pdf (in Czech)

 

Chemical Papers 17 (8) 550–555 (1963)

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