亲水色谱蒸发光散射检测器电喷雾四级杆飞行时间串联质谱法测定低聚麦芽糖化学成分

建立亲水色谱-蒸发光散射检测器-电喷雾-四级杆-飞行时间串联质谱（HILIC-ELSD-ESI-Q-TOF/MS）技术用于工业低聚麦芽糖中化学成分的快速鉴别及其含量测定的方法。以低聚麦芽糖为研究对象，采用HILIC法对低聚麦芽糖进行快速分离，ESI-Q-TOF/MS法对多种化合物进行鉴别，依据其精确分子质量、MS/MS裂解特征、色谱保留行为等信息，结合对照品信息和文献报道等对其进行验证，并采用HILIC-ELSD对已知成分进行定量测定。结果表明，采用亲水色谱法进行测定，低聚麦芽糖中各成分分离度较好；应用ESI-Q-TOF/MS鉴定出工业低聚麦芽糖中的10种成分；其中7种化合物（葡萄糖、麦芽糖、麦芽三糖、麦芽四糖、麦芽五糖、麦芽六糖、麦芽七糖）回归方程的相关系数均优于0.9990，表明线性关系良好；平均回收率在95.66%~99.00%范围内，相对标准偏差在1.11%~4.93%范围内；检出限在0.004~0.070 μg/mL之间，定量限在0.013~0.233 μg/mL之间。对7种成分定量测定表明，麦芽七糖的含量（14.31%±0.13%）最高，其次为麦芽三糖（9.34%±0.14%），麦芽六糖（7.49%±0.09%）。麦芽糖、麦芽三糖、麦芽四糖、麦芽五糖、麦芽六糖和麦芽七糖的总含量则达到了43.39%±0.35%。该方法分离度好、灵敏度高，可以对多种不同聚合度低聚麦芽糖成分进行定性和定量分析，为低聚麦芽糖工业化生产及应用的质量控制提供了一种分析方法支持。

Determination of Multiple Components in Maltooligosaccharide by HILIC-ELSD-ESI-Q-TOF/MS

A rapid identification and determination method of chemical components in industrial maltooligosaccharide was established by HILIC-ELSD-ESI-Q-TOF/MS technology.Taking maltooligosaccharide as the research object,the rapid separation of maltooligosaccharide was carried out by HILIC method,and a variety of compounds were identified by ESI-Q-TOF/MS method.Based on the accurate molecular weight,MS/MS fragmentation characteristics,chromatographic retention behavior and other information,combined with reference material information and literature reports,the known components were quantitatively determined by HILIC-ELSD.The results showed that the separation of the components in maltooligosaccharide was good by hydrophilic chromatography.Ten components in maltooligosaccharides were identified by ESI-Q-TOF/MS,the correlation coefficients of the regression equations of the seven compounds(glucose,maltose,maltotriose,malttetrasaccharide,maltpentasaccharide,malthexose,maltohexaose)were all better than 0.9990,indicating a good linear relationship.The average recoveries were in the range from 95.66%to 99.00%with relative standards deviation between 1.11%and 4.93%.The limits of detection ranged from 0.004 to 0.070μg/mL and limit of quantitation between of 0.013~0.233μg/mL.The quantitative determination of seven components showed that the content of maltose was the highest(14.31%±0.13%),followed by maltotrisaccharide(9.34%±0.14%)and maltohexose(7.49%±0.09%).The total contents of maltose,maltotrisaccharide,maltotrisaccharide,maltopentose,maltohexose and maltoheptoglycose reached 43.39%±0.35%.The method had good resolution and high sensitivity,and could be used for qualitative and quantitative analysis of maltose with different degree of polymerization.It provides an analytical method support for the industrial production and application of maltooligosaccharides.