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目的建立酰胺基亲水作用色谱的高效液相色谱-蒸发光散射法(HPLC-ELSD)测定壳寡糖低聚木糖胶囊中的低聚木糖。方法选用Waters XBridge Amide(4.6 mm×250 mm,3.5μm)色谱柱,以乙腈-0.2%三乙胺为流动相进行梯度洗脱,流速1.0 m L·min~(-1),进样量20μL,柱温45℃。结果对照品和样品溶液中木糖和低聚木糖7个组分得到很好的分离,各组分在0.05~0.5 mg·m L~(-1)内线性良好,相关系数r=0.999 4~0.999 9;7个组分在高低水平的添加回收率(n=6)为90.6%~103.2%,RSD<4.0%;3批样品中低聚木糖含量X2~X7分别为313,312,310 mg·g~(-1),X2~X4分别为282,279,278 mg·g~(-1)。结论本方法操作简单快速、灵敏度高、重复性好,为低聚木糖制品的质量控制及生产工艺研究提供更准确可靠的新方法。
OBJECTIVE To establish amido-based hydrophilic interaction chromatography (HPLC-ELSD) for the determination of xylooligosaccharides in chitosan oligosaccharide xylose capsules. Methods Waters XBridge Amide (4.6 mm × 250 mm, 3.5 μm) column was used with gradient elution with acetonitrile-0.2% triethylamine as the mobile phase at a flow rate of 1.0 mL · min -1. The injection volume was 20 μL , Column temperature 45 ℃. Results The seven components of xylose and xylo-oligosaccharides were separated well in the reference and sample solutions. The linearity of each component was good in 0.05-0.5 mg · mL -1 with a correlation coefficient of 0.999 4 ~ 0.999 9; The recoveries (n = 6) of the 7 components were 90.6% -103.2% at high and low levels with a RSD <4.0%. The content of xylo-oligosaccharides in three batches of samples was 313, 312 and 310 mg · g ~ (-1) and X2 ~ X4 were 282,279 and 278 mg · g ~ (-1), respectively. Conclusion The method is simple and rapid in operation with high sensitivity and good reproducibility. It provides a more accurate and reliable new method for the quality control and production technology research of XOS.