Determination of isophorone in food samples by solid-phase microextraction coupled with gas chromatography–mass spectrometry

A simple and sensitive method for the determination of isophorone in food samples was developed by headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography–mass spectrometry (GC–MS). Isophorone was separated within 10 min by GC–MS using a DB-1 capillary column and detected with selective ion monitoring mode. The HS-SPME using a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber provided effective sample enrichment, and was carried out by fiber exposition at 60 °C for 45 min. The extracted isophorone was easily desorbed by fiber exposition in the injection port of a capillary GC–MS system, and carryover was not observed. Using this method, the calibration curve of isophorone was linear in the range 20–1000 pg/mL, with a correlation coefficient 0.9996 (n = 18), and the detection limit (S/N = 3) was 0.5 pg/mL. The HS-SPME/GC–MS method showed 25,000-fold higher sensitivity than the direct injection method (1 μL injection). The within-day and between-day precisions (relative standard deviations) at the concentration of 1 ng/mL isophorone were 3.9% and 6.1% (n = 5), respectively. This method was successfully applied to the analysis of food samples without interference peaks. The recoveries of isophorone spiked into food sample were above 84% for a 50 or 500 pg/mL spiking concentration. The analytical results of the contents of isophorone in various food samples were presented.