色谱

色谱 ›› 2014, Vol. 32 ›› Issue (12): 1380-1384.DOI: 10.3724/SP.J.1123.2014.07052

• 研究论文 • 上一篇    下一篇

高效阴离子交换色谱-脉冲安培检测法测定乳粉中的低聚果糖

耿丽娟1,2, 黄峻榕1, 冯峰2, 蒋萍萍2, 储晓刚2, 张峰2, 凌云2   

  1. 1. 陕西科技大学生命科学与工程学院, 陕西 西安 710021;
    2. 中国检验检疫科学研究院, 食品安全研究所, 北京 100123
  • 收稿日期:2014-07-31 修回日期:2014-08-25 出版日期:2014-12-08 发布日期:2014-11-28
  • 通讯作者: 黄峻榕,E-mail:huangjunrong2000@163.com;张峰,E-mail:fengzhang@126.com
  • 基金资助:

    质检总局公益性行业科研专项项目(2012104002);质检总局科技计划项目(2013IK198);国家软科学研究计划项目(2010GXS5B153).

Determination of fructooligosaccharides in milk powder using high performance anion-exchange chromatography coupled with pulsed amperometric detection

GENG Lijuan1,2, HUANG Junrong1, FENG Feng2, JIANG Pingping2, CHU Xiaogang2, ZHANG Feng2, LING Yun2   

  1. 1. College of Life Science and Engineering, Shaanxi University of Science and Technology, Xi'an 710021, China;
    2. Institute of Food Safety, Chinese Academy of Inspection and Quarantine, Beijing 100123, China
  • Received:2014-07-31 Revised:2014-08-25 Online:2014-12-08 Published:2014-11-28

PDF

220

被引次数

12

摘要：

建立了测定乳粉中低聚果糖的高效阴离子交换色谱-脉冲安培检测(HPAEC-PAD)方法。样品经50%(v/v)乙醇水溶液提取,On Guard RP柱除脂,CarboPac PA200阴离子交换色谱柱(250 mm×3 mm)分离。采用水、0.2 mol/L NaOH溶液和0.4 mol/L NaAc溶液三元梯度淋洗,流速为0.4 mL/min,柱温为30 ℃,进样量为25 μL,脉冲安培检测器检测。蔗果三糖、四糖、五糖在0.05~10 mg/L范围内线性关系良好,相关系数(r2)> 0.9993;定量限分别为0.02、0.005和0.02 mg/L。在0.5、1.0、5.0 mg/L添加水平下,蔗果三糖、四糖、五糖的平均回收率为86.0%~114.0%。该方法处理简单、结果准确、灵敏度高,适用于乳粉中低聚果糖的测定。

关键词: 低聚果糖, 高效阴离子交换色谱, 脉冲安培检测, 乳粉

Abstract:

Fructooligosaccharides (FOS) are usually added in milk powder as a kind of prebiotic. Thus, quantitative analysis of the FOS is very important for the quality control of milk powder. In this study, a simple method for the simultaneous determination of three FOS components with degrees of polymerization (DP) 3-5 in milk powder was developed by high performance anion-exchange chromatography coupled with pulsed amperometric detection (HPAEC-PAD). The samples were extracted with 50%(v/v) ethanol aqueous solution and defatted by an On Guard RP pretreatment column. The separation was performed on a CarboPac PA200 column by gradient elution using deionized water, 0.2 mol/L NaOH solution and 0.4 mol/L NaAc solution as the mobile phases. The flow rate was 0.4 mL/min. The column temperature was 30 ℃; and the injection volume was 25 μL. Good linear response was observed in the concentration range of 0.05-10 mg/L (r2>0.9993). The limits of quantification were 0.02, 0.005 and 0.02 mg/L for 1-kestose, nystose and fructofuranosyl-nystose, respectively. The mean recoveries varied from 86.0% to 114.0% at three spiked levels of 0.5, 1.0 and 5.0 mg/L. The short-chain fructooligosaccharides from inulooligosaccharides (IOS) were successfully separated by the developed HPAEC-PAD method. The method is simple, accurate, sensitive, and helpful for the quality control of milk powder.

Key words: fructooligosaccharides (FOS), high performance anion-exchange chromatography (HPAEC), milk powder, pulsed amperometric detection (PAD)

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