高效液相法测定若羌红枣多糖的单糖组成  

Determination of monosaccharide composition in Ruoqiang jujube polysaccharide by high performance liquid chromatography

作　　者：赵非 牛莉娟 刘宗哲 孙永泽 王旭[1] ZHAO Fei;NIU Lijuan;LIU Zongzhe;SUN Yongze;WANG Xu(State Key Laboratory of Food Nutrition and Safe,Tianjin University of Science and Technology,Tianjin 300457;Harmonia Testing Technology(Tianjin)Limited Company,Tianjin 300457)

机构地区：[1]省部共建食品营养与安全国家重点实验室,天津科技大学,天津300457 [2]瀚盟测试科技(天津)有限公司,天津300457

出　　处：《食品科技》2019年第11期321-326,共6页Food Science and Technology

基　　金：天津市自然科学基金项目(16JCQNJC14400);食品营养与安全国家重点实验室开放基金项目(SKLFNS-KF-201820)

摘　　要：建立柱前衍生高效液相色谱法分离检测若羌红枣水溶性多糖的单糖组成和比例。利用单因素实验筛选出多糖提取、水解、衍生最优条件。通过优化条件对若羌红枣多糖的单糖组成进行定性、定量分析。结果表明,最优条件为多糖提取料液比为1:20,温度为80℃,热水浴超声时间100min。多糖水解三氟乙酸浓度为2 mol/L,料液比1:400,水解温度105℃,水解时间5 h。衍生化温度为70℃,时间60 min。分析方法线性关系良好,精密度RSD值低于2.4%,红枣多糖组分单糖的回收率为92.4%~103.5%。分析表明,若羌红枣多糖中可确定的单糖种类为甘露糖、鼠李糖、葡萄糖、半乳糖,质量比为甘露糖:鼠李糖:葡萄糖:半乳糖=1:6.46:11.20:6.24。Pre-column derivatization-high performance liquid chromatography method was established for the separation and determination of monosaccharide composition and proportion of water-soluble polysaccharides from Ruoqiang jujube. In this experiment, the optimum conditions for extraction, hydrolysis and derivation of polysaccharides were screened by single factor experiments. Qualitative and quantitative analysis of the monosaccharide composition from Ruoqiang jujube polysaccharide was conducted by optimized method. The results showed that the optimum conditions were as follows: the material to liquid ratio of extraction polysaccharide was 1:20, the temperature and time of the water bath through ultrasonic was 80 ℃ and 100 min respectively. 2 mol/L trifluoroacetic acid was used to hydrolysis of polysaccharide and solid-liquid ratio was 1:400. The hydrolysis temperature was 105 ℃ and the hydrolysis time was 5 h. The derivatization temperature was 70 ℃ and the time was 60 min. The linear relationship of the method was good and the recovery was between 92.4% and 103.5% with RSD value of less than 2.4%. The results showed that the monosaccharides were the contents of mannose, rhamnose, glucose and galactose. The mass ratio of four monosaccharides was 1:6.46:11.20:6.24.

关 键 词：柱前衍生 高效液相色谱 若羌红枣 多糖 单糖组成 

分 类 号：O657.7^+2[理学—分析化学]