黄精多糖中果糖含量的精确测定方法

Precise Determination of Fructose Content in Polygonatum sibiricum Polysaccharides

为准确测定黄精多糖中果糖的含量,采用亲水色谱-电雾式检测分析(hydrophilic interaction liquid chromatography-charged aerosol detector,HILIC-CAD)法,系统地考察多糖浓度、酸浓度、水解温度及水解时间4个多糖水解单因素,并结合正交试验获得黄精多糖的最佳水解条件。结果表明,黄精多糖的最佳水解条件为1.0 mg/mL黄精多糖在0.100 mol/L三氟乙酸溶液中,于80℃水解30 min,果糖可被完全释放,且未转变为其他物质。采用HILIC-CAD结合柱前衍生-反相色谱法,测定山东、安徽、甘肃、四川和陕西5个产地黄精多糖中果糖及其它6种单糖的含量,其中安徽产地的黄精多糖果糖含量较低(51.74%),其它4个产地黄精多糖中果糖含量较高且含量相似(78.71%~83.08%)。

This study aimed to accurately determine the fructose content in Polygonatum sibiricum polysaccharides.A hydrophilic interaction liquid chromatography-charged aerosol detector(HILIC-CAD)method was employed to systematically investigate the four single factors on polysaccharide hydrolysis,i.e.,polysaccharide concentration,acid concentration,temperature,and hydrolysis time.Optimal hydrolysis conditions were determined through orthogonal testing.The results indicated that the optimal conditions for the hydrolysis of P.sibiricum polysaccharides were as follows:1.0 mg/mL P.sibiricum polysaccharides were hydrolyzed in a 0.100 mol/L trifluoroacetic acid solution at 80℃ for 30 min.Under these conditions,fructose was completely released without conversion to other substances.By combining HILIC-CAD with pre-column derivatization and reverse-phase chromatography,the exact content of fructose and six other monosaccharides in P.sibiricum polysaccharides from five different regions(Shandong,Anhui,Gansu,Sichuan,and Shaanxi)was determined.It was found that the fructose content in the P.sibiricum polysaccharides from Anhui was relatively low(51.74%),while the fructose content from the other four regions was higher and similar(78.71%-83.08%).