Determination of benzo(a)pyrene residue in smoked fish by subcritical water extraction and gas chromatography-mass spectrometry

Abstract:

A method was developed for the B(a)P determination in smoked fish by gas chromatography-mass spectrometry (GC-MS) method with subcritical water extraction(SCWE). B(a)P were extracted by water under the extraction temperature of 100 ℃ for 5 min,transferred into cyclohexane-ethylacetate (1:1, V/V) and then cleaned up by the Gel Permeation Chromatography (GPC). The GC separation was performed on a Rtx-5MS capillary column. The B(a)P were determined by MS in selected ion monitoring(SIM) mode. The method showed good linearity over the range of 0 to 100 ng/mL with the correlation coefficient of 0.9999. The limit of quantification (S/N>10) was 2.5 ng/g,the limit of detection (S/N>10) was 1 ng/g and the precision(RSD) was between 7.95% and 10.56%. The average blank spike recoveries at three levels of 2.5, 5 and 10 ng/g ranged from 74.89% to 114.01% (n=8). The sensitivity,accuracy and precision of the method are suitable for the determination of the B(a)P in smoked fish.