乳业科学与技术 ›› 2020, Vol. 43 ›› Issue (1): 9-14.DOI: 10.15922/j.cnki.jdst.2020.01.003

• 分析检测 • 上一篇    下一篇

离子色谱法测定婴幼儿配方乳粉中的糖类

李莉, 曹文军, 薛伟锋, 刘明   

  1. 大连市检验检测认证技术服务中心, 辽宁 大连 116600, 中检(大连)测试技术有限公司, 辽宁 大连 116600, 大连海关技术中心, 辽宁 大连 116600
  • 出版日期:2020-01-01 发布日期:2021-11-02
  • 基金资助:
    辽宁省自然科学基金面上项目(20170540025);辽宁省博士启动基金项目(2019-BS-008)

Determination of Sugars in Infant Formula by Ion Chromatography

LI Li, CAO Wenjun, XUE Weifeng, LIU Ming   

  1. (1.Dalian Inspection and Certification Technology Service Center, Dalian 116600, China; 2.China Inspection (Dalian) Test Technology Co. Ltd., Dalian 116600, China; 3.Dalian Customs Technology Center, Dalian 116600, China)
  • Published:2020-01-01 Online:2021-11-02

摘要: 为建立操作简便、快速有效、同时分析婴幼儿配方乳粉中多种糖类的离子色谱分析方法,采用高效阴离子交换柱分离-脉冲安培检测法建立婴幼儿配方乳粉中葡萄糖、蔗糖、乳糖、低聚半乳糖三糖、蔗果三糖、低聚半乳糖五糖、蔗果四糖和蔗果五糖的分析方法。考察色谱柱、柱温、检测波形和淋洗液(NaOH、NaAc)浓度及流速对8 种糖分离效果的影响。结果表明:选用CarboPac PA20阴离子交换柱,包括分析柱(3 mm×150 mm)和保护柱(3 mm×30 mm),流速0.30 mL/min,柱温30 ℃,在选定的流动相梯度洗脱程序条件下实现高效分离;本方法对葡萄糖、蔗糖、乳糖、低聚半乳糖三糖、蔗果三糖、低聚半乳糖五糖、蔗果四糖和蔗果五糖的检出限为3.0~12.0 μg/L,精密度实验相对标准偏差小于3%,豆浆样品中8 种糖类的加标回收率为78.0%~96.8%,表明该方法可行。

关键词: 离子色谱, 脉冲安培检测, 梯度洗脱, 婴幼儿配方乳粉, 多种糖类

Abstract: The purpose of this study is to establish a simple, rapid and effective method for the simultaneous analysis of various saccharides (glucose, sucrose, lactose, galactooligotrisaccharide, kestose, galactooligopentasaccharide, nystose and 1F-fructofuranosyl nystose) in infant formula by high performance anion exchange chromatography with pulsed amperometric detection (HPAEC-PAD). The effect of chromatographic columns, column temperature, detector waveforms, eluent concentration and flow rate on the separation of the 8 saccharides was evaluated. The analysis was performed on a CarboPac PA20 analytical column (3 mm × 150 mm) coupled with a guard column (3 mm × 30 mm) at a 0.30 mL/min flow rate. Column temperature was set as 30 ℃. Efficient separation was achieved using gradient elution. Under the optimal conditions, the detection limit was 3.0–12.0 μg/L for all analytes. The precision, expressed as relative standard deviation (RSD), was less than 3%. The recoveries of the 8 saccharides in spiked soymilk were 78.0%–96.8%, indicating the feasibility of this method.

Key words: ion chromatography, pulsed amperometric detection, gradient elution, infant formula, a variety of sugars

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