顶空固相微萃取-气质联用法测定热加工食品中的呋喃

Determination of furan in heated foods by headspace solid-phase microextraction-gas chromatography-mass spectrometry

目的:建立顶空固相微萃取(HS-SPME)结合气相色谱质谱(GC/MS)测定热加工食品中呋喃的方法。方法:试样中加入d4-呋喃内标和2 g氯化钠,采用75μm CAR/PDMS萃取头,25℃下萃取30 min后,在气相色谱质谱仪进样口280℃解吸2 min,PLOT Q毛细管柱气相色谱分离,选择离子监测(SIM)模式定量测定。结果:方法线性范围为1 ng/g～50 ng/g,方法检出限(S/N≥3)为0.2 ng/g,定量检出限(S/N≥10)为1.0 ng/g;不同基底样品中加标回收率为87.8%～92.5%,相对标准偏差值(RSD)为1.2%～3.1%。结论:该方法灵敏度高、准确可靠,可分析热加工食品中呋喃的含量。

Objective：To develop a method for the determination of furan in heated foods by gas chromatography/mass spectrometry after headspace solid-phase microextraction（HS-SPME）.Methods：After addition of deuterated internal standard（d4-furan） and 2 g sodium chloride,samples were extracted with 75 μm fibres coated with carboxen/polydimethysiloxane（30min at 25℃） and finally inserted into the injection port of the GC/MS（2 min at 280℃） for desorption.The analytes were separated on a PLOT Q capillary column,identified and quantified by mass spectrometry in SIM mode.Results：The correlation coefficients were good in the concentration range of 1 ng/g^50 ng/g,with a limit of detection（S/N≥3） of 0.2 ng/g and limit of quantification（S/N≥10） of 1.0 ng/g.The average recoveries of the method were 87.8%~92.5%,and the relative standard deviation（RSD） were in the range of 1.2%~3.1%.Conclusion：The method is sensitive,precisive and suitable for determination of furan in heated foods.