医药辅料低聚木糖中5-羟甲基糠醛和糠醛含量测定及其限度确定

Determination of 5-hydroxymethylfurfural and furfural and validation of the limit of impurity detection in xylo-oligosaccharides

目的建立了低聚木糖中5-羟甲基糠醛和糠醛的HPLC分析方法,并确定了其限度。方法采用Agilent ZORBAX Eclipse XDB-C18(150mm×4.6mm,5μm)色谱柱分离;以甲醇-水(10∶90)溶液为流动相;流速为1.0mL·min^(-1),在紫外检测器284nm处检测。结果 5-羟甲基糠醛、糠醛的质量浓度分别在0.75~25.0μg·mL^(-1)(r=1.000 0)和0.099~3.3μg·mL^(-1)(r=0.999 9)范围内与峰面积呈良好线性关系,检出限分别为0.000 2%和0.000 3%,平均回收率分别为100.5%和99.0%,RSD值分别为0.32%和1.83%。结论该方法可用于低聚木糖中5-羟甲基糠醛和糠醛的测定,操作方便、专属性强、定量准确、重复性好。

Objective A method for detecting 5-hydroxymethylfurfural（5-HMF）and furfural in xylo-oligosaccharides by HPLC was described and the limit of impurity detection in xylo-oligosaccharides was validated.Methods Agilent ZORBAX Eclipse XDB-C18（150 mm×4.6 mm,5μm）was used for the separation.The mobile phase was methanol-water（10∶90）.The flow rate was 1.0 mL·min^-1 and the wavelength was 284 nm.Results There was a good linear relationship between the concentration and the peak area in the range of 0.75-25.0μg·mL^-1（r=1.000 0）for 5-HMF,0.099-3.3μg·mL^-1（r=0.999 9）for furfural.The limits of detection of 5-HMF and furfural were 0.000 2% and 0.000 3%,respectively.The average recoveries of the method were 100.5%and 99.0%,with RSD 0.32% and 1.83%（n=9）,respectively.Conclusion This method is simple,rapid,accurate and reproducible for detecting 5-HMF and furfuralin in xylo-oligosaccharides.