顶空-气相色谱-质谱法测定热加工食品中4种呋喃类化合物的含量  

Determination of 4 Furan Compounds in Hot Processed Foods by Headspace-Gas Chromatography-Mass Spectrometry

作　　者：何绍志 杨诗嘉 钟慈平 李澍才 张丽平[2] HE Shaozhi;YANG Shijia;ZHONG Ciping;LI Shucai;ZHANG Liping(Sichuan Institute of Food Inspection,Key Laboratory of Baijiu Supervising Technology for State Market Regulation,Chengdu 610097,China;Chengdu Textile College,Chengdu 611731,China)

机构地区：[1]四川省食品检验研究院,国家市场监管重点实验室(白酒监管技术),成都610097 [2]成都纺织高等专科学校,成都611731

出　　处：《理化检验(化学分册)》2025年第1期46-51,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：四川省科技重点研发项目(2023YFS0398);四川省科技重点研发项目(2023YFS0403)。

摘　　要：提出了顶空气相色谱-质谱法测定热加工食品中呋喃、2-甲基呋喃、3-甲基呋喃、2,5-二甲基呋喃等4种呋喃类化合物含量的方法。取粉碎混匀后的样品(液体样品5.00 g或固体样品1.00 g)置于20 mL顶空瓶中,加入适量的(液体样品加入5 mL,固体样品加入10 mL)20%(质量分数)氯化钠溶液和1.0 mg·L^(-1)混合内标溶液100μL,拧盖密封后混匀,于60℃平衡30 min,在HP-PLOTQ毛细管色谱柱上按照柱升温程序分离,质谱分析采用电子轰击离子(EI)源、选择离子监测(SIM)模式。结果表明,4种呋喃类化合物的质量浓度在0.1~20μg·L^(-1)内和内标的质量浓度之比与两者对应的定量离子峰面积之比呈线性关系,检出限(3S/N)为0.003~0.010μg·kg^(-1)。按照标准加入法进行回收试验,回收率为100%~115%,测定值的相对标准偏差(n=6)均小于10%。方法用于98份热加工食品样品的分析,呋喃、2-甲基呋喃、3-甲基呋喃、2,5-二甲基呋喃的总检出率分别为98.0%,94.9%,9.20%,40.8%。A method for determination of 4 furan compounds,including furan,2-methylfuran,3-methylfuran,and2,5-dimethylfuran in hot processed foods by headspace-gas chromatography-mass spectrometry was proposed.The crushed and mixed sample (5.00 g of liquid sample or 1.00 g of solid sample) was taken and placed in a 20 mL-headspace vial.An approriate amount of 20%(mass fraction) sodium chloride solution (5 mL for liquid sample and 10 mL for solid sample) and 100μL of1.0 mg·L^(-1) mixed internal standard solution were added and the bottle was sealed.The mixture was mixed well and equilibrated at 60℃for 30 min,and separated on a HP-PLOTQ capillary chromatographic column according to the column heating program.Electron impact ion (EI) source and selected ion monitoring (SIM) mode were adopted in mass spectrometry analysis.As shown by the results,the ratios of the mass concentration of 4 furan compounds in the range of 0.1-20μg·L^(-1) to the mass concentration of the internal standard was linearly related to the ratios of their corresponding quantitative ion peak areas,with detection limits(3S/N) in the range of 0.003-0.010μg·kg^(-1).Test for recovery was made by the standard addition method,giving results in the range of 100%-115%,with RSDs (n=6) of the determined values less than 10%.This method was used for the analysis of98 samples of hot processed foods,the total detection rates of furan,2-methylfuran,3-methylfuran,and 2,5-dimethylfuran were98.0%,94.9%,9.20%,and 40.8%,respectively.

关 键 词：顶空气相色谱-质谱法 热加工食品 呋喃类化合物 

分 类 号：O657.63[理学—分析化学]