Journal of Chromatography B 2008-11-15

Sensitive determination of monoterpene alcohols in urine by HPLC-FLD combined with ESI-MS detection after online-solid phase extraction of the monoterpene-coumarincarbamate derivates.

Roland J W Meesters, Mike Duisken, Heike Jähnigen, Juliane Hollender

Index: J. Chromatogr. B. Analyt. Technol. Biomed. Life Sci. 875(2) , 444-50, (2008)

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Abstract

A method was developed for the determination of the monoterpene alcohols verbenol, myrtenol, perillyl alcohol, alpha-terpineol, Delta(3)-carene-10-ol, thymol and p-alpha,alpha-trimethylbenzylalcohol in urine samples. After an enzymatic cleavage of their glucuronide- and sulfate conjugates the monoterpene alcohols were converted in the urine matrix with 7-diethylaminocoumarin-3-carbonylazide into monoterpene-[7-(diethylamino)-coumarin-3-yl]-carbamate derivates prior to analyses. Enrichment of the monoterpene alcohols from the urine matrix was achieved by online-solid phase extraction (SPE) with restricted-access material (RAM). After removal of excess derivatization reagent and urine matrix components, the monoterpene derivatives were separated by high-performance liquid chromatography (HPLC) in combination with fluorescence (FLD) detection and simultaneous mass spectrometric (MS) identification. Detection limits (LOD) for studied monoterpene alcohols ranged between 22 and 197 ng/L. The method was validated and successfully applied to urine samples from human subjects orally exposed to monoterpenes trough an intake of cough medication containing monoterpenes as active medicinal ingredients.