首页|柱前衍生—高效液相色谱荧光检测法测定乳制品中6种母乳寡糖

柱前衍生—高效液相色谱荧光检测法测定乳制品中6种母乳寡糖

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目的:建立一种普及性强、灵敏度高,并能同时测定乳制品中6种母乳寡糖的高效液相色谱一荧光检测分析方法。方法:样品经冰醋酸沉淀,滤纸过滤后,经2-氨基苯甲酰胺溶液衍生,离心后经有机滤膜过滤,用AdvanceBio Glycan Map 色谱柱分离,以乙腈-50 mmol/L甲酸铵溶液(pH 4。4)为流动相,梯度洗脱分离,并使用荧光检测器检测。结果:6种母乳寡糖在1。00~400。0 mg/L质量浓度范围内线性关系良好,相关系数均>0。999,方法检出限为4。1~10。9 mg/kg,回收率为71。3%~90。2%,日内相对标准偏差(RSD)为1。0%~6。3%,日间相对标准偏差<10。0%。结论:该方法简单、快捷,可有效降低衍生峰的干扰,适用于乳制品中3'-岩藻糖基乳糖、2'-岩藻糖基乳糖、乳糖-N-四糖、乳糖-N-新四糖、3'-唾液乳糖和6'-唾液乳糖6种母乳寡糖的日常检测。
Determination of six human milk oligosaccharides in dairy product by precolumn derivatization high performance liquid chromatography with fluorescence detection
Objective:To astablish a strong popularity,high sensitivity of six human milk oligosaccharides in dairy product by precolumn derivatization high performance liquid chromatography-fluorescence method.Methods:Aquatic product sample was precipitated with glacial acetic acid,filtration by using the filter paper.It was derived by 2-aminobenzamide solution.The extracts were centrifuged and filtered by using the organic filter membrane and analyzed by using a AdvanceBio Glycan Map column to be separated and detected,employing acetonitrile-50 mmol/L ammonium formate solution(pH 4.4)as the mobile phase for gradient elution.Results:Under the experimental conditions,six human milk oligosaccharides in dairy product were linear in the range of 1.00~400.0 mg/L,and the correlation coefficients were all over 0.999.The detection limit of the method was 4.1~10.9 mg/kg,the limits of quantification were 12.3~32.7 mg/kg,the mean recoveries rate was ranged from 71.3%to 90.2%with the intra-day precisions(n=6)in the range of 1.0%~6.3%and inter-day precisions(n=6)less than 10.0%.Conclusion:This method can meet the requirements of the daily detection of six human milk oligosaccharides due to its simplicity and sensitives.

precolumn derivatizationhuman milk oligosaccharidesdairy product2-aminobenzamide

李绮淇、黄嘉乐、穆姝夷、李绮珊、黄靖钧

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广州检验检测认证集团有限公司,广东广州 511447

国家加工食品质量检验检测中心[广东],广东广州 511447

柱前衍生法 母乳寡糖 乳制品 2-氨基苯甲酰胺

广东省市场监督管理局科技项目

2023CS03

2024

食品与机械
长沙理工大学

食品与机械

CSTPCD北大核心
影响因子:0.89
ISSN:1003-5788
年,卷(期):2024.40(4)
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