宫慧丽，段国霞，刘丽君*，刘春霞，陈 静，武伦玮，刘 旺，唐 烁，李翠枝，吕志勇
（内蒙古伊利实业集团股份有限公司，国家市场监管重点实验室（乳及乳制品检测与监控技术），内蒙古自治区 呼和浩特 010110）
摘要：建立了高效液相色谱法测定乳与乳制品中甲醛含量的方法，样品以2，4-二硝基苯肼溶液-乙酸钠缓冲溶液（pH=5）为衍生液，超声提取10 min，置于60℃恒温振荡器中，以150r/min 振摇1h，使甲醛转化为相应稳定的甲醛-2，4-二硝基苯腙。生成物经C18 色谱柱分离，流动相采用乙腈-水（60∶40，V∶V），在365nm 波长下，经紫外检测器检测，外标法定量。结果表明，甲醛在浓度0～5μg/mL 内线性关系良好，相关系数为0.999。奶粉、液奶和酸奶3 个加标水平甲醛含量的相对标准偏差（RSD）分别为0.46%～2.67%、0.91%～3.86%和1.93%～3.11%，奶粉、液奶和酸奶中甲醛不同水平的回收率分别为90.2%～91.7%、98.5%～101%和98.0%～101%。该方法简单、快速、准确、重复性好，提供了一种测定乳与乳制品中甲醛含量的方法。
关键词：高效液相色谱法；乳与乳制品；甲醛
Determination of Formaldehyde in Milk and Dairy Products by High Performance Liquid Chromatography
GONG Hui-li，DUAN Guo-xia，LIU Li-jun*，LIU Chun-xia，CHEN Jin，WU Lun-wei，LIU Wang，TANG Shuo，LI Cui-zhi，LYU Zhi-yong
（Inner Mongolia Yili Industrial Group Co.Ltd. Hohhot 010010，China）
Abstract: A high performance liquid chromatographic （HPLC） method was developed for the determination offormaldehyde in milk and dairy products. The test samples were derivatized with 2，4-dinitrophenylhydrazine solutionsodiumacetate buffer solution（pH=5），extracted by sonication for 10min，placed in a constant temperature shaker at60℃ and shaken at 150 r/min for 1 h to convert the formaldehyde to the corresponding stable formaldehyde- 2，4-dinitrophenylhydrazone.The generated product was separated on a C18 column with the mobile phase of acetonitrilewater（60∶40，V∶V），detected by UV detector at 365 nm detection wavelength，and quantified by external standardmethod.The results showed that formaldehyde had a good linear relationship in the concentration range of 0 μg/mL-5μg/mL with a correlation coefficient of 0.999. The relative standard deviations （RSDs） of formaldehyde in milkpowder，liquid milk and yogurt at the three spiked levels were 0.46%～2.67%，0.91%～3.86% and 1.93%～3.11%，respectively，and the recoveries of formaldehyde in milk powder，liquid milk and yogurt at the three spiked levelswere 90.2%～91.7%，98.5%～101% and 98.0%～101%，respectively.The test method is simple，rapid，accurate andreproducible，and provides a method for the determination of formaldehyde content in milk and dairy products.
Key words: high performance liquid chromatography；milk and dairy products；formaldehyde
中图分类号：TS207.5 文献标志码：A 文章编号：1007-7871（2024）05-0030-04
2024，Vol.27，No.5