Determination of Doxepin by Electron-Capture Gas Chromatography

A method is described for the determination of low nanogram concentrations of doxepin, plus its primary active metabolite desmethyldoxepin, in small amounts of serum. The procedure employs a hexane extraction of the biologic specimen after salting out the drug from the biologic matrix with sodium ca...

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Bibliographic Details
Published in:Journal of analytical toxicology 1978-03, Vol.2 (2), p.44-49
Main Authors: Wallace, Jack E., Hamilton, Horace E., Olivares, Rebecca, Harris, Steven C.
Format: Article
Language:English
Subjects:
Drugs
Gas chromatography
Metabolites
n-Hexane
Powder
Quantitation
Sodium bicarbonate
Sodium carbonate
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Summary:A method is described for the determination of low nanogram concentrations of doxepin, plus its primary active metabolite desmethyldoxepin, in small amounts of serum. The procedure employs a hexane extraction of the biologic specimen after salting out the drug from the biologic matrix with sodium carbonate/sodium bicarbonate powder. Doxepin and desmethyldoxepin are derivatized with 2′,2′,2′,trichloroethylchloroformate to form a single product that is highly sensitive to the electron-capture detector. The recovery of doxepin and desmethyldoxepin from serum after derivatization with the polyhalogenated chloroformate reagent is 95 ± 2.5%. Quantitation is based upon the utilization of dothiepin, a compound that has a molecular structure similar to that of doxepin, as the internal standard.
ISSN:0146-4760
1945-2403
DOI:10.1093/jat/2.2.44