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≥0.998 1) betweeen peak areas ratios and concentrations ratios of 3 analytes were obtained in the range of 25-5 000 μg/kg.The limits of detection(LOD) for 3 analytes were 20 μg/kg.And the limits of quantitation(LOQ) were 50 μg/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.
关键词
气相色谱-质谱(GC-MS)选择离子扫描(SIM)固相萃取(SPE)黄樟素香料添加剂食品
Keywords
gas chromatography-mass spectrometry(GC-MS)selected ion monitor(SIM)solid phase extraction(SPE)safrolespice additivesfoodstuffs
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