AEC柱前衍生-高压液相色谱-质谱联用法分析混合植物浓缩液中多糖

Qualitative analysis of polysaccharide in the plant concentrate by HPLC-MS/MS with pre-column derivatization using 3-amino-9-ethylcarbazole

目的建立多糖的高压液相色谱串联质谱检测方法,以提高多糖检测的特异性和准确性。方法以3-氨基-9-乙基咔唑(AEC)为柱前衍生试剂,反相C18色谱柱为分离柱,乙腈和乙酸铵水溶液为流动相,在波长254nm处,用LC-MS/MS同时分析植物及其提取物中多糖。结果 AEC对多糖的衍生效果好,无副产物产生;经过衍生化反应的多糖在高压液相色谱中得到了很好的分离;并用质谱仪对其相对分子量和结构进行了确定。结论该方法操作简单,灵敏度和准确度高,样品的污染和损失风险低,在植物多糖的结构分析、构效关系等研究上具有重要应用意义。

@@@@Objective In order to improve the detection specificity and accuracy of polysaccharide, a high pressure liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for detec-tion of polysaccharides in plants concentrate. Methods Samples were derivatized using 3-amino-9- ethylcar-bazole, separated by reverse phase C18 column using acetonitrile and ammonium acetate aqueous solution as mobile phase and detected by LC-MS/MS under the wavelength of 254 nm. Results 3-amino-9- ethylcarba-zole(AEC)was good for the derivatization of polysaccharides, without side products and the polysaccharide molecules with the derived group were separated by mass spectrometry to determine the relative molecular weight and structure. Conclusion the method is simple, sensitive and accurate and has lower risk of pollu-tion and loss. It has significance for structure analysis, structure-activity relationship of the plant polysaccha-ride.