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Simultaneous determination of 5′-deoxy-5-fluorouridine, 5-fluorouracil and 5,6-dihydro-5-fluorouracil in plasma by gas chromatography-mass spectrometry

✍ Scribed by Carlo G. Zambonin; Antonio Guerrieri; Francesco Palmisano

Publisher
Elsevier Science
Year
1996
Tongue
English
Weight
779 KB
Volume
329
Category
Article
ISSN
0003-2670

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✦ Synopsis

A gas chromatography-mass spectrometry (GC-MS) method for the simultaneous determination of 5'-deoxy-Sfluorouridine (doxifluridine, 5'-dFUR), 5fluorouracil (5-FU) and its main catabolite 5,6-dihydro-5-fluorouracil

(5-FUH*) in human plasma has been developed. Sample preparation consisted of protein precipitation with ammonium sulphate followed by analyte extraction with ethyl acetate/isopropanol (90/10, v/v) mixture. Extracts were then analysed by GC-MS in positive electron impact mode after derivatization with N,O-bis(trimethylsilyl)trifluoroacetamide/pyridine (l/l, v/v). The trimethylsilyl (TMS) derivative of 5'-dFWR was proved to be stable so that no interference in 5-FU determination was observed. Mass spectra of TMS derivatives of 5'-dFUR, 5-FU and 5-FWH2 are discussed. Analyte response was linear over two decades of concentration and detection limits were typically 20ng/ml of plasma.

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