Abstract: A high-performance liquid chromatography method was developed to determine the contents of 5-hydroxymethylfurfural and furfural in liquid milk. The samples were extracted with oxalic acid solution in a boiling water bath, then the protein and fat were precipitated by adding trichloroacetic acid solution. The supernatant was separated on an XDB-C18 column (4.6 mm × 250 mm, 5 μm) using 10% acetonitrile solution as the mobile phase. The analytes were detection with an ultraviolet detector and quantified by the external standard method. The experimental results showed that the correlation coefficient of 5-hydroxymethylfurfural was 0.999 8, with a spiked recovery ranging from 84.6% to 94.3%, a limit of detection (LOD) of 0.005 mg/kg, and a coefficient of variation (CV) of 0.15% to 0.36%. For furfural, the correlation coefficient was 0.999 4, with a spiked recovery rate ranging from 73.7% to 92.0%, a LOD of 0.005 mg/kg, and a CV of 0.95% to 1.54%. This method is characterized by simple operation, low cost, and excellent separation performance, and it is suitable for the quantitative analysis of 5-hydroxymethylfurfural and furfural in liquid milk, providing technical support for the quality control and process optimization of dairy products.

Key words: furfural; 5-hydroxymethylfurfural; high-performance liquid chromatography; liquid milk

摘要： 基于高效液相色谱法建立液态乳中5-羟甲基糠醛与糠醛含量同步测定方法。样品经草酸溶液沸水浴提取后，三氯乙酸溶液沉淀蛋白和脂肪，取上清液经XDB-C18色谱柱（4.6 mm×250 mm，5 μm）分离，以10%（V/V）乙腈溶液作为流动相洗脱，紫外检测器检测，外标法定量。结果表明，在0～0.50 μg/mL线性范围内，5-羟甲基糠醛相关系数为0.999 8，加标回收率为84.6%～94.3%，检出限为0.005 mg/kg，变异系数（coefficient of variation，CV）为0.15%～0.36%；在0～0.25 μg/mL线性范围内，糠醛相关系数为0.999 4，加标回收率为73.7%～92.0%，检出限为0.005 mg/kg，CV为0.95%～1.54%。此方法前处理简便、分析成本低且分离效果优良，适用于液态乳中5-羟甲基糠醛和糠醛的定量分析，可为乳制品质量控制和工艺优化提供技术支持。

关键词: 糠醛；5-羟甲基糠醛；高效液相色谱；液态乳