实验旨在建立以D4-呋喃为内标测定热加工食品中呋喃的顶空气相色谱一质谱法。方法首次以NaCl溶液作为样品基质,加入内标物D4-呋喃,通过顶空70℃恒温30min后提取出呋喃,用HP-PLOTQ石英毛细管柱气相色谱分离,采用选择性离子检测质谱扫描模式进行定性定量分析。结果显示:方法的工作曲线的线性范围为5-1200ng,相关系数为0.9993;方法的定性检测限(S/N≥3)为0.4ng/g,定量检测限(S/N≥10)为1.0ng/g;不同基底样品中高低添加浓度的加标回收率在86.8%-104.7%之间,相对标准偏差(RSD)均〈10%。检测我国市场上11类经热加工的食品(共有133份样品),呋喃检出浓度为〈1.0-210.7ng/g。该方法处理样品简单,灵敏度、准确度高,抗干扰能力强,适合我国各类热加工食品中呋喃的常规检测,能满足对我国热加工食品中呋喃污染状况的调杏工作要求。
The aim of this study was to develop a headspace gas chromatography-mass spectrometry method (HS-GC-MS) for the determination of furan in thermal processed foods, with D4-furan as an internal standard. This was the first time to use NaC1 solution as the sample matrix,with a headspace sampler to extract furan at 70℃ for 30 min. The method of standard additions with D4-furan as the internal standard was used to quantitate furan, with the HP-PLOT Q capillary column, using the selection of ion monitoring (MS1 SIM) of the MS scan mode, using qualitative and quantitative analysis by mass spectrometry. The results showed that the furan ranged from 5 to 1 200 ng had a good linearity, with correlation coefficient of 0.999 3 ;the limit of detections (S/N≥3 ) was 0.4 ng/g, and the limit of quantitation (S/N≥10) was 1.0 ng/g; The recoveries in different sample matrixes were 86.8% - 104.7%, and the relative standard deviation (RSD) were less than 10%. Finally,this method was applied to the a- nalysis of furan in 11 kinds of thermal processed foods (totally 133 samples) ,and furan levels ranging from lower than the detection limit to 210.7 ng/g were found. The method was accurate, reliable, high sensitivity, suitable for determination of! any kinds of thermal processed foods in our country, and can meet the investigation requirements of furan pollutAnt in food commodities the