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Energy-dispersive X-ray fluorescence spectrometry following sample decomposition and preconcentration was developed to determine selenium in crude drugs. Samples were decomposed with conc. HNO3 and conc. H2SO4 in a flask with a reflux condenser. Evaporation of HNO3 had to be avoided to prevent serious loss of this element. Selenium was preconcentrated from the digestion liquid by two-step reduction with 4M HCl and ascorbic acid, the elemental selenium formed was adsorbed on activated carbon and then collected on a Nuclepore membrane filter for direct irradiation in an X-ray spectrometer. This analytical method (detection limit, 0.03 ppm) was used to determine selenium in many kinds of crude drugs. The analytical results indicated vegetable drugs to be low in selenium content: more than 0.5 ppm in only a limited number of samples and less than detection limit (0.03 ppm) in nearly all the samples. Animal drugs contain selenium at higher levels, Lumbricus and Cantharis being 7.46 and 1.67 ppm, respectively.

Inorganic chemical approaches to pharmacognosy. VIII. Determination of selenium in crude drugs by energy-dispersive X-ray fluorescence spectrometry.