超声辅助醇沉水提-高效液相色谱-蒸发光散射法测定铁皮石斛中的甘露糖含量  

Determination of Mannose in Dendrobium officinale by Ultrasound-assisted Alcoholic Precipitation and Aqueous Extraction Coupled with High Performance Liquid Chromatography-evaporative Light Scattering Method

作　　者：朱帅 阮小娇 张水锋 孙琦琦[1,2] ZHU Shuai;RUAN Xiaojiao;ZHANG Shuifeng;SUN Qiqi(Zhejiang Fangyuan Test Group Co.,Ltd.,Hangzhou,Zhejiang 310018,China;Food Safety Key Lab of Zhejiang Province,Hangzhou,Zhejiang 310018,China)

机构地区：[1]浙江方圆检测集团股份有限公司,浙江杭州310018 [2]浙江省食品安全重点实验室,浙江杭州310018

出　　处：《农产品加工》2025年第1期62-67,共6页Farm Products Processing

摘　　要：建立超声辅助醇沉水提-高效液相色谱-蒸发光散射法测定铁皮石斛中甘露糖含量的分析方法。将铁皮石斛粉末样品经高体积分数乙醇水溶液除去杂质,冷冻条件下快速沉降,离心后得到沉淀物,沉淀物置于烘箱中烘干。用水在沸水浴中提取沉淀物中多糖,得到的多糖溶液在盐酸水解条件下得到甘露糖,再用氢氧化钠溶液调pH值至中性,用水定容后得到甘露糖样品待测液,采用高效液相色谱-蒸发光散射直接检测,外标法定量。结果表明,在最优的试验条件下,方法的线性范围为20~1000 mg/L,检出限为0.1%,精密度RSD在1.1%~1.8%,与药典方法测得结果的相对偏差在1.3%~3.8%。该方法具有操作简便、色谱峰干扰少、无需衍生的特点,适用于铁皮石斛中甘露糖含量的快速批量测定。To establish an analytical method for the determination of mannose content in Dendrobium officinale by ultrasound-assisted alcoholic precipitation and aqueous extraction-high performance liquid chromatography-evaporative light scattering.The Dendrobium powder sample was subjected to high concentration of ethanol aqueous solution to remove impurities,rapidly settled under freezing conditions,centrifuged to obtain the precipitate,and the precipitate was dried in an oven.The polysaccharide in the precipitate was extracted with water in a boiling water bath,and the polysaccharide solution obtained was hydrolyzed with hydrochloric acid to obtain mannose,and then the pH was adjusted to neutral with sodium hydroxide solution,and the mannose sample was fixed with water to obtain the solution to be tested,which was detected directly by high-performance liquid chromatography-evaporative light scattering and quantified by external standard method.The results showed that under the optimal experimental conditions,the linear range of the method was 20~1000 mg/L,the detection limit was 0.1%,the RSD of precision ranged from 1.1%to 1.8%,and the relative deviation between this method and that obtained by Chinese Pharmacopoeia in the range of 1.3%~3.8%.The method was characterized by easy operation,low peak interference and no derivatization,and was suitable for the rapid batch determination of mannose content in Dendrobium officinale.

关 键 词：高效液相色谱 蒸发光散射 铁皮石斛 甘露糖 醇沉水提 

分 类 号：O657.7[理学—分析化学]