色谱 ›› 2020, Vol. 38 ›› Issue (2): 169-176.DOI: 10.3724/SP.J.1123.2019.05014

• 特别策划:第22届全国色谱学术报告会优秀论文专栏 • 上一篇    下一篇

基于非对称场流分离技术分离表征小米淀粉

张靖1, 郭攀攀1, 李惠丽2, 申世刚1,*(), 窦海洋1,2,*()   

  1. 1 河北大学化学与环境科学学院, 河北 保定 071002
    2 河北大学医学院, 河北 保定 071000
  • 收稿日期:2019-05-13 出版日期:2020-02-08 发布日期:2020-12-10
  • 通讯作者: 申世刚,窦海洋
  • 作者简介:窦海洋.E-mail:douhaiyang-1984@163.com
    申世刚.E-mail:shensg@hbu.edu.cn;
  • 基金资助:
    河北省高等学校科学技术研究重点项目(ZD2019009);河北省大学生创新创业项目(201910075070)

Separation and characterization of millet starch based on asymmetrical flow field-flow fractionation

ZHANG Jing1, GUO Panpan1, LI Huili2, SHEN Shigang1,*(), DOU Haiyang1,2,*()   

  1. 1 College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China
    2 College of Medicine, Hebei University, Baoding 071000, China
  • Received:2019-05-13 Online:2020-02-08 Published:2020-12-10
  • Contact: SHEN Shigang,DOU Haiyang
  • Supported by:
    Key Project of Hebei Education Department(ZD2019009);Undergraduate's Innovation Fund Project of Hebei Province(201910075070)

摘要:

基于非对称场流分离技术耦合多角度激光光散射检测器和示差折光检测器,建立了分离表征小米淀粉的方法。研究了进样量、交叉流流速、半衰期(t1/2)、载液离子强度和pH值对小米淀粉分离效果的影响;考察了该方法的重现性;探究了小米淀粉分子结构。结果表明,在进样体积为50 μL、进样质量浓度为0.50 g/L、交叉流流速为1.2 mL/min、t1/2=3 min、载液为10 mmol/L pH 7.00 NaNO3(含3 mmol/L NaN3)的条件下,小米淀粉分离效果最佳。该方法具有良好的重现性,得到的小米淀粉的回转半径相对标准偏差为3.4%、摩尔质量相对标准偏差为7.0%。

关键词: 非对称场流分离, 小米淀粉, 分离

Abstract:

A method based on asymmetrical flow field-flow fractionation (AF4) coupled with a multi-angle light scattering detector and a differential refractive detector was developed for the separation and characterization of millet starch. In this study, the effects of sample loading, cross-flow rate, half-life, and ionic strength and pH value of the carrier liquid on the AF4 analysis of millet starch were investigated. In addition, the molecular structure of millet starch was determined under the optimum conditions. The optimized operation conditions for the AF4 analysis of millet starch were as follows:injection mass concentration, 0.50 g/L; injection volume, 50 μL; cross-flow rate, 1.2 mL/min; half-life, 3 min; and the carrier liquid, demonized water containing 10 mmol/L pH 7.00 NaNO3 (add 3 mmol/L NaN3). The method developed in this study showed good reproducibility. The relative standard deviations for the radius of gyration (Rg) and molar mass (Mw) were 3.4% and 7.0%, respectively.

Key words: asymmetrical flow field-flow fractionation (AF4), millet starch, separation