Trace Analysis of Doxylamine Succinate in Animal Feed, Human Urine, and Wastewater by GC Using a Rubidium-Sensitized Nitrogen Detector

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Abstract
Doxyiamine succinate, a drug used as a sleep-inducing agent, an antihistamine, and in a therapeutic formulation taken by pregnant women as an antinauseant, was scheduled for toxicological evaluation as part of a structure activity relationship study, with rats and mice, because a deficiency of such data exists with regard to many antihistamines. Analytical chemical procedures that ensure proper concentration, homogeneity, and stability of the drug in dosed feed, as well as the safety of personnel and the environment, were prerequisites for the toxicological tests. GC methods using a rubidium-sensitized nitrogen detector were developed for analysis of doxylamine succinate in animal feed, human urine, and wastewater at levels as low as 1 ppm, 100 ppb, and 100 ppb, respectively. Sample extracts were cleaned up by liquid-liquid partitioning, followed by additional cleanup on a column of silica gel. Data are presented concerning the stability of the drug in animal feed, extraction efficiencies, and the use of the silica gel cleanup column to separate the caffeine interference from doxylamine in extracts of human urine. Partition values and ancillary data concerning analysis of the drug in feed, by HPLC at levels as low as 10 ppm, are also reported.