基于非对称场流分离技术分离表征小米淀粉  

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

作　　者：张靖[1] 郭攀攀 李惠丽 申世刚[1] 窦海洋[1,2] ZHANG Jing;GUO Panpan;LI Huili;SHEN Shigang;DOU Haiyang(College of Chemistry and Environmental Science,Hebei University,Baoding 071002,China;College of Medicine,Hebei University,Baoding 071000,China)

机构地区：[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

出　　处：《色谱》2020年第2期169-176,共8页Chinese Journal of Chromatography

基　　金：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)~~

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50μL、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%。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.

关 键 词：非对称场流分离 小米淀粉 分离 

分 类 号：O658[理学—分析化学]