保健食品中5-羟甲基糠醛快速筛查定性定量分析方法研究

目的：建立保健食品中5-羟甲基糠醛（5-hydroxymethyl furfural，5-HMF）快速筛查定性定量分析方法。方法：样品经色谱甲醇提取富集，气相色谱-质谱联用（GC-MS），Scan模式进行定性，SIM选择离子扫描模式进行定量检测。采用DB-5 ms毛细管色谱柱（30 m×0.25 mm×0.25 μm），程序升温：初始温度70 ℃（保持2 min），8 ℃·min^-1升至100 ℃，再以6 ℃·min^-1升至125 ℃（保持3 min），再以25 ℃·min^-1升至280 ℃（保持2 min）；选择EI离子源，溶剂延迟2 min，质谱扫描范围50~600 amu。结果：5-羟甲基糠醛在2.050~102.5 μg·mL^-1范围内均呈良好的线性关系，相关系数为0.9995；检出限（S/N=3）为0.02 μg·mL^-1 ，加标回收率为84.0%~96.5%；样品筛查结果发现7批含糖口服液中检测出5-羟甲基糠醛。结论：该法简便、快速、准确，专属性强，可用于保健食品质量控制中检测5-羟甲基糠醛的残留量。

Objective: To develop a qualitative and quantitative analytical method for rapid screening of 5-hydroxymethyl furfural (5-HMF) in health food. Methods: Methanol solvent extraction was used to get the enrichment of samples.Qualitative analysis was carried out by GC-MS and scan mode,quantitative detection was performed by selected ion monitoring (SIM) mode.The analytical capillary column was DB-5 ms (30 m×0.2 5 mm×0.25 μm).The oven temperature was set at 70 ℃ (maintained for 2 min) initially,which was programmed to rise up to 100 ℃ by 8 ℃·min^-1,then rise up to 125 ℃(maintained for 3 min) by 6 ℃·min^-1,then rise up to 280 ℃(maintained for 2 min) by 25 ℃·min^-1.The EI ion source was adopted,and the solvent was delayed for 2 min.The MS scanning range was 50-600 amu. Results: The method showed good linearity within the range of 2.050-102.5 μg·mL^-1 (r> 0.9995) for 5-HMF.The limit of detection was 0.02 μg·mL^-1(S/N=3).The recoveries were 84.0%-96.5%.5-hydroxymethyl furfural was identified in seven batch samples of sugar-containing oral liquid. Conclusion: This method is convenient,fast,accurate and highly selective,which is suitable for the determination of 5-HMF residue in health food.