Determination of Safrole and its Derivatives in Foodstuffs by Gas Chromatography-Mass Spectrometry

KeyWord:gas chromatography-mass spectrometry(GC-MS)  selected ion monitor(SIM)  solid phase extraction(SPE)  safrole  spice additives  foodstuffs

Abstract:

      An analytical method was developed for the determination of safrole(SFL),isosafrole(DSFL) and dihydrosafrole(ISFL) in 18 foods including condiment,tomato,sauce,soy sauce,pepper,carbonated beverage,milk drink,juice,sausage,canned meat,meat soup,jelly,jam,dried fish,canned fish,fish slime,potato chip,candy and chocolate by gas chromatography-mass spectrometry(GC-MS).The sample was extracted with dichloromethane-acetonitrile in the presence of sodium chloride salt-out.Water and polar substances were removed with anhydrous sodium sulfite florisil column.For complex matrices,further purification was performed with a PRiME HLB solid phase extraction columns.The separation was carried out on a 5%phenyl-95% methyl polysiloxane capillary GC column.The detection of compounds was completed in the selected ion monitoring mode(SIM).The quantification analysis was performed by the internal standard method.Good linear relationships(r2¡Ý0.998 1) betweeen peak areas ratios and concentrations ratios of 3 analytes were obtained in the range of 25-5 000 ¦Ìg/kg.The limits of detection(LOD) for 3 analytes were 20 ¦Ìg/kg.And the limits of quantitation(LOQ) were 50 ¦Ìg/kg.The average recoveries of the method varied from 77.6% to 100.9% at 3 different spiked levels,with relative standard deviations(RSD) of 3.7%-13.6%.By measuring real samples,the results showed that this method was accurate and reliable for quantification and confirmation of SFL,DSFL and ISFL in foodstuffs.