HILIC-ELSD法测定岩藻聚糖硫酸酯中岩藻糖  

Determination of fucose in fucoidan by hydrophilic interaction chromatography coupled with evaporative light-scattering detector

作　　者：陈艳萍[1,2] 王宇 曾琪[1] 谭道鹏 曾令杰[1] 严启新 

机构地区：[1]广东药学院中药学院,广东广州510006 [2]深圳海王药业有限公司,广东深圳518057

出　　处：《药物评价研究》2014年第6期519-521,共3页Drug Evaluation Research

基　　金：中国博士后科学基金(2012M511837)

摘　　要：目的 建立一种简便、高效、准确的测定岩藻聚糖硫酸酯中岩藻糖的方法.方法 采用超声处理（300 W 100％,20℃,20 min）;三氟乙酸（4 mol/mL）水解（110℃、2h）;亲水作用色谱-蒸发光检测（HILIC-ELSD）法检测,Waters XBridgeTMAmide（150 mm×4.6 mm,3.5μm）色谱柱,流动相为乙腈-水-氨水（90∶10∶0.2）,体积流量1mL/min,柱温60℃.结果 岩藻糖的线性范围为0.100 4～1.004 mg/mL （r=0.999 4）,平均加样回收率95.22％（n=6,RSD=1.16％）.结论 该方法简便、快速、准确,为岩藻聚糖硫酸酯的定量分析和质量评价研究提供了依据.Objective The study aimed at providing an efficient and accurate approach for the determination of fucose in fucoidan. Methods After ultrasonic preprocess for 20 min at 20 ℃ and hydrolysing with trifluoroacetic acid （4 mol/mL, 110 ℃） for 2 h, the sample was separated on a Waters XBridgeTM Amide （4.6 × 150 mm, 3.5 μm） column at 60 ℃, with acetonitrile-water-ammonia （90：10：0.2） as the mobile phase at a flow rate of 1 mL/min, and detected through ELSD. Results The experimental results showed that, as for fucose, the linear detection range was 0.100 4 mg/mL -1.004 mg/mL （r = 0.999 4）, the average recoveries and RSD were 95.22%, and 1.16% respectively （n = 6）. Conclusion This method is quick, simple, and accurate, and can be used for the quantitative determination and quality control of fucoidan.

关 键 词：亲水作用色谱-蒸发光检测法 岩藻聚糖硫酸酯 岩藻糖 

分 类 号：R917[医药卫生—药物分析学]