The analysis of drugs contained in biological matrices is generally pe
rformed by gas chromatography coupled with mass spectrometry. Because
of these complexity of these matrices a sample preparation step is nec
essary. Subcritical fluid extraction has been developed for the determ
ination of opiates (morphine, 6-monoacetylmorphine, codeine and ethylm
orphine) in urine and hair. This procedure has been compared to conven
tional techniques for this kind of matrice. For urine, classical solid
phase extraction with a mired mode silica is the method of choice, ev
en if subcritical fluid extraction gives some comparable results. In t
ire case of hair, which is a complementary matrice, subcritical fluid
extraction shows numerous advantages in regard to classical procedures
: analysis time reduced, sample handling simplified and on-line coupli
ng with chromatography possible. Finally, applications of real cases a
re presented for the analysis of opiates, cocaine and its major metabo
lite (the benzoylecgonine) and methadone contained in hair. In the cas
e of opiates, a quantitative determination has been carried out on a l
inear dynamic range of concentrations (between 0.25 to 5.0 ng/mg). Goo
d coefficients of variation (between 3 to 12%) have been obtained. The
limits of detection and quantification are respectively of 0.03 ng/mg
and 0.1 ng/mg for codeine, ethylmorphine and morphine. These values a
re multiplied by a factor of 2 for 6-monoacetylmorphine.