A solid-phase microextraction (SPME) protocol was developed for the qu
antitative analysis of monocyclic aromatic amines from biological flui
ds, me headspace SPME sampling technique was optimized for extraction
and concentration of five target analytes (aniline, o-toluidine, 2-chl
oroaniline, 2,6-dimethylaniline, 2,4,6-trimethylaniline) from urine, b
lood, and milk. The temperature, pH, and ionic strength of the matrix
sample were modified to allow maximum adsorption of the analytes onto
the SPME fiber. This method is rapid yet sensitive and can be complete
d in 15 min on a 5-mL sample. SPME/GC/MS analysis yielded good reprodu
cibility (RSD >11%) for each analyte from urine, blood, and milk, Meth
od detection limits for the various biological fluids were determined
and ranged from 0.40 ppb for 2,4,6-trimethylaniline in urine to 7.7 pp
b for aniline in blood. This SPME sampling protocol can be applied to
the biomonitoring of monocyclic aromatic amines from occupational, env
ironmental, and medical exposure.