Single-drop microextraction and gas chromatography/mass spectrometric determination of anisaldehyde isomers in human urine and blood serum

The application of single-drop microextraction (SDME) followed by gas chromatography/chemical ionization mass spectrometry (GC/CI-MS) was investigated for the determination of anisaldehyde isomers in human urine and blood serum. The effects of extraction solvent, sample agitation rate, salt addition, sampling time and temperature on the extraction efficiency were examined and optimized. Analytical parameters such as linearity, reproducibility, detection limit and relative recovery were evaluated under the optimized experimental conditions. Good reproducibilities of replicate extractions (n = 5) were obtained, with relative standard deviation (RSD) values below 6%. The limits of detection (LOD) using an extraction time of 5 min were found to be in the range 2-5ng/mL under the selected ion monitoring (SIM) mode of GC/MS. Recoveries of 82-98% were achieved after 5 min extraction. Copyright (C) 2004 John Wiley Sons, Ltd.