目的 建立一種簡便、高效、準確的測定巖藻聚糖硫酸酯中巖藻糖的方法。方法 采用超聲處理(300 W 100%,20 ℃,20 min);三氟乙酸(4 mol/mL)水解(110 ℃、2 h);親水作用色譜-蒸發(fā)光檢測(HILIC-ELSD)法檢測,Waters XBridge^TM Amide(150 mm×4.6 mm,3.5 μm)色譜柱,流動相為乙腈-水-氨水(90:10:0.2),體積流量1 mL/min,柱溫60 ℃。結(jié)果 巖藻糖的線性范圍為0.100 4~1.004 mg/mL(r=0.999 4),平均加樣回收率95.22%(n=6,RSD=1.16%)。結(jié)論 該方法簡便、快速、準確,為巖藻聚糖硫酸酯的定量分析和質(zhì)量評價研究提供了依據(jù)。

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 XBridge^TM 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.

中國博士后科學基金(2012M511837)