黄伟乾,吴俊发,覃天福,邓思怡,梁志森,吴敏莲.柱前衍生-高效液相色谱法测定乳及乳制品中5种乳糖衍生物[J].食品安全质量检测学报,2025,16(5):46-51 |
柱前衍生-高效液相色谱法测定乳及乳制品中5种乳糖衍生物 |
Determination of 5 kinds of lactose derivatives in milk and dairy products by pre-column derivatization-high performance liquid chromatography |
投稿时间:2024-11-11 修订日期:2025-02-18 |
DOI: |
中文关键词: 乳与乳制品 高效液相色谱 乳糖衍生物 3’-半乳糖基乳糖 4’-半乳糖基乳糖 6’-半乳糖基乳糖 3’-唾液酸乳糖 6’-唾液酸乳糖 |
英文关键词:milk and dairy products high performance liquid chromatography lactose derivatives |
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中文摘要: |
目的 建立柱前衍生-高效液相色谱法测定乳及乳制品中5种乳糖衍生物(3’-半乳糖基乳糖、4’-半乳糖基乳糖、6’-半乳糖基乳糖、3’-唾液酸乳糖、6’-唾液酸乳糖)含量的定量分析方法。方法 乳及乳制品经沉淀蛋白, 于55 ℃下5种乳糖衍生物与2-氨基苯甲酰胺反应120 min, 标记上荧光基团, 经高效液相色谱酰胺柱分离, 外标法定量5种乳糖衍生物的含量。结果 5种乳糖衍生物在0.025~5.000 mg/L质量浓度范围内线性关系良好, 相关系数(r)均大于0.999; 5种乳糖衍生物的检出限和定量限在3.5~7.5 mg/kg和12.0~25.0 mg/kg之间; 5种乳糖衍生物的的回收率在90.8%~103.3%, 检测结果的相对偏差在2.8%~5.3% (n=3)。结论 本方法的精密度和回收率良好, 灵敏度较好, 可用于乳与乳制品中5种乳糖衍生物含量的测定。 |
英文摘要: |
Objective To establish a quantitative analysis method for determining the content of 5 kinds of lactose derivatives (3’-galactosyllactose, 4’-galactosyllactose, 6’-galactosyllactose, 3’-sialyllactose, 6’-sialyllactose) in milk and dairy products by pre-column derivatization-high performance liquid chromatography. Methods The proteins in milk and dairy products were precipitated. The 5 kinds of lactose derivatives were reacted with 2-aminobenzamide at 55 ℃ for 120 min to label the fluorescent groups. The 5 kinds of lactose derivatives were separated by high performance liquid chromatography with an amide column and quantified by external standard method. Results The 5 kinds of lactose derivatives exhibited good linear relationships within the concentration range of 0.025–5.000 mg/L, with correlation coefficients (r) all exceeding 0.999. The limits of detection and quantification for the 5 kinds of lactose derivatives ranged from 3.5 to 7.5 mg/kg and 12.0 to 25.0 mg/kg, respectively. The recovery rates for the 5 kinds of lactose derivatives were between 90.8% and 103.3%, with relative deviations in detection results ranging from 2.8% to 5.3% (n=3). Conclusion This method demonstrates good precision, recovery rate, and sensitivity, making it suitable for determining the content of 5 kinds of lactose derivatives in milk and dairy products. |
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