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目的:建立白及葡甘露聚糖中单糖含量的亲水作用色谱-蒸发光散射检测(HILIC-ELSD)测定方法。方法:白及葡甘露聚糖水解条件:三氟乙酸浓度2.0mol·L-1,温度120℃,时间2h。采用Sugar-Dwaters色谱柱(4.6mm×250mm,5μm)分离,流动相为乙腈-水(体积比为85∶15),等度洗脱,流速1.0mL·min-1,柱温30℃。采用蒸发光散射检测器检测,漂移管温度40℃,雾化气(空气)压力350kPa。结果:D-甘露糖的线性范围为0.07765～1.553mg.mL-1(r=0.9983),检测限为0.4659μg,加标回收率(n=3)为99.4%～101.8%,RSD为1.3%～2.0%;D-葡萄糖的线性范围为0.08112～1.622mg.mL-1(r=0.9988),检测限为0.4730μg,加标回收率(n=3)为98.9%～102.0%,RSD为1.1%～2.1%。结论:该方法简便快速,结果准确,重复性好,可作为白及葡甘露聚糖中单糖含量及其组成测定的有效方法。
Objective: To establish a method for the determination of monosaccharide content in white and glucomannan by HILIC-ELSD. Methods: The hydrolysis conditions of white and glucomannan: trifluoroacetic acid 2.0mol·L-1, temperature 120 ℃, time 2h. It was separated on a Sugar-Dwaters column (4.6 mm × 250 mm, 5 μm) using a mobile phase of acetonitrile-water (85:15 by volume) with isocratic elution at a flow rate of 1.0 mL · min -1 and a column temperature of 30 ° C. Using evaporative light scattering detector detection, drift tube temperature 40 ℃, atomizing gas (air) pressure 350kPa. Results: The linear range of D-mannose was 0.07765 ~ 1.553 mg.mL-1 (r = 0.9983). The detection limit was 0.4659 μg. The recoveries were 99.4% -101.8% with RSD of 1.3% ~ 2.0% .The linear range of D-glucose was 0.08112 ~ 1.622mg.mL-1 (r = 0.9988) .The detection limit was 0.4730μg, the recovery was 98.9% ~ 102.0% with RSD of 1.1 % ~ 2.1%. Conclusion: The method is simple, rapid, accurate and reproducible. It can be used as an effective method for the determination of monosaccharide content and its composition in white and glucomannan.