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

作　　者：黄伟乾 吴俊发 覃天福 邓思怡 梁志森 吴敏莲 HUANG Wei-Qian;WU Jun-Fa;QIN Tian-Fu;DENG Si-Yi;LINAG Zhi-Sen;WU Min-Lian(Guangzhou Inspection Testing and Certification Group Co.,Ltd.,Guangzhou 511447,China)

机构地区：[1]广州检验检测认证集团有限公司,广州511447

出　　处：《食品安全质量检测学报》2025年第5期46-51,共6页Journal of Food Safety and Quality

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。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.

关 键 词：乳及乳制品 高效液相色谱法 乳糖衍生物 

分 类 号：O657.72[理学—分析化学] TS252.7[理学—化学]