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Part A: Speciation of aluminum metabolites in biological matrices employing chemical neutron activation analysis. Part B: Evaluation of methods for the determination of trimethylselenonium ion in urine
Abstract
(A) A method employing cation-exchange chromatography and neutron activation analysis was developed for the speciation of nonprotein Al metabolites in human urine. The developed procedure also provided an estimate of the amount of protein-bound Al. Urine samples, from 24 hr specimen collections, were adjusted to a pH 1 by treatment with trichloroacetic acid which also resulted in the precipitation of urinary proteins. Precipitated proteins and particulate matter were then separated by centrifugation. The supernatant was then loaded onto a polypropylene cation-exchange column and Al$\sp{3+}$ was selectively eluted from the column and assayed via irradiative neutron capture and gamma-ray spectrometry. Recoveries determined for the entire procedure by the addition of an Al spike were quantitative. (B) Trimethylselenonium (TMSe) was separated by dual-column ion-exchange chromatography and assayed by neutron activation analysis. The TMSe content was found to be $14\pm2\%$ of total urinary Se measured by instrumental neutron activation analysis and was consistent with literature values. An alternate, multi-step procedure employing Reineckate precipitation followed by decomposition/volatilization conversion of selenium to dimethyl selenide, and perchloric acid digestion to selenite with analysis by inductively coupled mass spectrometry was evaluated. A maximum recovery of TMSe was estimated at 32%. It has been suggested that losses in each step of a multi-step procedure yield low recoveries.
Subject Area
Analytical chemistry|Biochemistry
Recommended Citation
Shoop, David Mark, "Part A: Speciation of aluminum metabolites in biological matrices employing chemical neutron activation analysis. Part B: Evaluation of methods for the determination of trimethylselenonium ion in urine" (1996). ETD collection for University of Nebraska-Lincoln. AAI9628252.
https://digitalcommons.unl.edu/dissertations/AAI9628252