La. Adam, Confirmation of azaperone and its metabolically reduced form, azaperol, inswine liver by gas chromatography/mass spectrometry, J AOAC INT, 82(4), 1999, pp. 815-824
The method described confirms the use of the tranquilizer azaperone by dete
cting the parent compound and the metabolically reduced form, azaperol. Bot
h are confirmed in swine liver at a target concentration of 10 ppb by gas c
hromatography/mass spectrometry (GC/MS) with electron ionization in the sel
ected-ion-monitoring mode. Swine liver tissue is ground with dry ice. Aceto
nitrile is added to extract the drug from the tissue. Sodium chloride buffe
r is added to the extract in preparation for solid-phase extraction (SPE).
The aqueous extract is loaded onto an SPE cartridge designed to extract aci
dic and neutral drug residues from biological matrixes. The cartridge is wa
shed with methanol and conditioned with sodium phosphate buffer. Azaperone
and azaperol residues are eluted with a 2% ammonium hydroxide in ethyl acet
ate. The extracts are evaporated to dryness under a stream of nitrogen and
reconstituted in ethyl acetate for GC/MS analysis. A DB-I analytical column
is used to separate the compounds prior to electron ionization. The parent
ion, the base peak ion, and one diagnostic fragment ion are monitored for
both compounds. The method was validated with fortified tissue samples cont
aining both azaperone and azaperol. Azaperone-incurred tissues also were an
alyzed, and the presence of the parent drug and the metabolically reduced f
orm, azaperol, was confirmed.