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A study on the derivatization technique for tamoxifen metabolites in human urine by gas chromatography/mass spectrometry  

Kim, Yunje (Doping Control Center, Korea Institute of Science and Technology)
Lee, Yoonjung (Doping Control Center, Korea Institute of Science and Technology)
Publication Information
Analytical Science and Technology / v.17, no.4, 2004 , pp. 322-336 More about this Journal
Abstract
The improved derivatization technique of tamoxifen metabolite in human urine is described for the acylation method that they are substituted by derivatization reagent like acyl anhydride for use of gas chromatography/mass spectrometry. The hydroxyl group of tamoxifen metabolite was derivatized by trifluoroacetic anhydride (TFAA), pentafluoroacetic anhydride (PFPA) and heptaflorobutylic anhydride (HFBA). It was investigated to the gas chromatography/mass spectrometry (GC/MS) technique use negative ion chemical ionization (NCI), positive ion chemical ionization (PCI) and electron impact (EI). In acylation of the metabolites of tamoxifen, the effective reaction temperature and time were shown to be at $50^{\circ}C$ for 30 min. The 4-hydroxytamoxifen, which is known to major metabolite of tamoxifen, was not detected in human urine, whileas the hydroxymethoxytamoxifen was detected. We thought that this result was from the single dose of tamoxifen.
Keywords
Tamoxifen; metabolite; gas chromatography/mass spectrometry; acylation; derivatization; electron impact; chemical ionization;
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