[关键词]
[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 ℃、2 h);亲水作用色谱-蒸发光检测(HILIC-ELSD)法检测,Waters XBridgeTM Amide(150 mm×4.6 mm,3.5 μm)色谱柱,流动相为乙腈-水-氨水(90:10:0.2),体积流量1 mL/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。
[Key word]
[Abstract]
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.
[中图分类号]
[基金项目]
中国博士后科学基金(2012M511837)