基于柱前衍生化反相色谱分析的枸杞多糖产品的掺杂检测  

Adulteration detection of lycium barbarum polysaccharide products based on per-column derivatization reversed-phase liquid chromatography

作　　者：李文德 陈尚卫[2] 杨浩 戴军[2] 陈安平 徐一达 LI Wen-de;CHEN Shang-wei;YANG Hao;DAI Jun;CHEN An-ping;XU Yi-da(Zhejiang Jianfeng Health Technology Co.,Ltd.,Jinhua 321000;State Key Laboratory of Food Science and Technology,Jiangnan University,Wuxi 214122)

机构地区：[1]浙江尖峰健康科技有限公司,金华321000 [2]江南大学食品科学与技术国家重点实验室,无锡214122

出　　处：《中国食品添加剂》2019年第12期181-188,共8页China Food Additives

摘　　要：为建立枸杞多糖产品的掺杂检测方法,采用多糖完全水解结合柱前PMP衍生化反相色谱分析的方法,研究发现正常枸杞多糖提取物与其掺杂样品中的葡萄糖、半乳糖、阿拉伯糖和氨基葡萄糖这4个标志性单糖组分的相对百分比具有显著性差异,据此特征可进行枸杞多糖产品的掺杂鉴别;应用酶解和醇沉的方法去除糊精或可溶性淀粉的干扰,再将枸杞多糖完全水解,并进行柱前PMP衍生化反相色谱分析,即可实现掺杂枸杞多糖提取物产品的确证检测及其枸杞多糖实际含量的准确测定。其测定方法加标平均回收率为89.8%,相对标准偏差为2.48%(n=5)。该测定方法比起现有的苯酚流酸法,不仅在样品前处理方法上可以完全排除糊精或可溶性淀粉的干扰,且消除了用葡萄糖作标品测定杂多糖含量的苯酚硫酸法固有的较大误差,因此本方法更为科学合理、准确可信。In order to adulteration detection of Lycium barbarum polysaccharide(LBP)products,complete hydrolysates of polysaccharide extracted from Lycium barbarum was analyzed by reversed phase liquid chromatography(RPLC)coupled per-column derivatization with 1-phenyl-3-methyl-5-pyrazolane(PMP),and compared with doped LBP samples.Relative percentage of four signature monosaccharide components(glucose,galactose,arabinose and glucosamine)were found as characteristics of LBP and may be used to identify adulterated samples.By enzymatic hydrolysis and alcohol precipitation to remove interference of dextrin or soluble starch and then completely hydrolyzing the polysaccharides in the sample,adulteration of LBP sample can be confirmed and its true content can be obtained according to change and total amount of monosaccharide component.In terms of the total amount of monosaccharide,average recovery of the method determinated was 89.8%,and the relative standard deviation was 2.48%(n=5).Compared with the existing phenol hydrochloric acid method,this method can not only completely exclude the interference of dextrin or soluble starch in the sample pretreatment,but also eliminate inherent error in the determination of heteropolysaccharide by using glucose as standard,so this method is more scientific,reasonable and accurate.

关 键 词：枸杞多糖 掺杂检测 反相液相色谱 柱前衍生化 酶解和醇沉 

分 类 号：TS201.2[轻工技术与工程—食品科学]