HPLC-CAD法同时测定铁皮石斛中单糖和寡糖类成分的含量  

Simultaneous determination of monosaccharides and oligosaccharides in Dendrobii Officinalis Caulis by HPLC-CAD

作　　者：徐双双 吴思佳 卢文旭 李剑 王峥涛[1] 徐红[1] XU Shuang-shuang;WU Si-jia;LU Wen-xu;LI Jian;WANG Zheng-tao;XU Hong(Institute of Chinese Materia Medica,Shanghai University of Traditional Chinese Medicine,The Ministry of Education Key Laboratory for Standardization of Chinese Medicines,The State Administration of Traditional Chinese Medicine Key Laboratory for New Resources and Quality Evaluation of Chinese Medicine,Shanghai R&D Center for Standardization of Chinese Medicines,Shanghai 201203,China;Jinling Pharmaceutical Co.,Ltd.,Nanjing 210009,China)

机构地区：[1]上海中医药大学中药研究所,教育部中药标准化重点实验室,中药新资源与品质评价国家中医药管理局重点研究室,上海中药标准化研究中心,上海201203 [2]金陵药业股份有限公司,南京210009

出　　处：《药物分析杂志》2023年第8期1302-1311,共10页Chinese Journal of Pharmaceutical Analysis

基　　金：国家自然科学基金资助项目(82173958,U19A2009);国家重点研发项目(2017YFC1700801)。

摘　　要：目的:建立高效液相色谱-电喷雾式检测器(HPLC-CAD)法同时测定铁皮石斛中10个单糖和寡糖类成分含量。方法:采用Waters XBridge BEH Amide色谱柱(250 mm×4.6 mm,5μm),以乙腈-0.1%三乙胺水溶液为流动相,梯度洗脱,流速1.0 mL·min^(-1),柱温40℃,进样体积5~20μL。结果:该方法对铁皮石斛中10个糖类成分,包括单糖成分果糖、D-甘露糖和D-葡萄糖,寡糖成分蔗糖、麦芽糖和低聚麦芽糖系列麦芽三糖、麦芽四糖、麦芽五糖、麦芽六糖和麦芽七糖的分离度良好,在线性范围内呈现良好的线性关系,平均回收率为98.2%~100.5%,RSD为0.62%~3.0%;10个糖类成分的检测限分别为0.014、0.008、0.026、0.009、0.008、0.016、0.035、0.016、0.016、0.017μg·mL^(-1);精密度、稳定性和重复性的RSD均<3.0%。18批次不同产地的铁皮石斛中果糖、D-甘露糖、D-葡萄糖、蔗糖、麦芽糖、麦芽三糖、麦芽四糖、麦芽五糖、麦芽六糖和麦芽七糖的含量范围分别为0.05~11.92、0.01~2.82、0.07~16.49、0.38~23.14、0.02~3.17、0~4.08、0~3.78、0~2.30、0~7.53、0~6.02 mg·g^(-1),10个糖类成分的分布和含量与栽培地域具有一定相关性。结论:本研究建立的方法快速、灵敏、准确,重复性好且操作简单,可用于铁皮石斛中单糖和寡糖类成分的同时含量测定。Objective:To develop a high performance liquid chromatography-charged aerosol detector(HPLC-CAD)method for simultaneous determination of ten monosaccharides and oligosaccharides in Dendrobii Officinalis Caulis.Methods:The components were separated on a Waters XBridge BEH Amide column(250 mm×4.6 mm,3.5μm)with acetonitrile and 0.1%triethylamine aqueous solution as the mobile phase by gradient elution at a flow rate of 1.0 mL·min^(-1).The column temperature was 40℃.Results:The ten carbohydrate components in Dendrobii Officinalis Caulis,including three monosaccharides components fruc⁃tose,D-mannose and D-glucose,and oligosaccharide components sucrose,maltose and maltooligosacchar⁃ides maltotriose,maltotetraose,maltopentaose,maltohexaose and maltoheptaose,had good resolution with a good linear relationship within the linear range.The correlation coefficients were all above 0.999.The aver⁃age recoveries were 98.2%-100.5%with RSD within 0.62%-3.0%.The LODs of above ten carbohy⁃drate components were 0.014,0.008,0.026,0.009,0.008,0.016,0.035,0.016,0.016 and 0.017μg·g^(-1),respectively.The RSDs of precision,stability and repeatability were less than 3.0%.The content ranges of fructose,D-mannose,D-glucose,sucrose,maltose,maltotriose,maltotetraose,maltopentaose,maltohexaose and maltoheptaose were 0.05-11.92 mg·g^(-1),0.01-2.82 mg·g^(-1),0.07-16.49 mg·g^(-1),0.38-23.14 mg·g^(-1),0.02-3.17 mg·g^(-1),0-4.08 mg·g^(-1),0-3.78 mg·g^(-1),0-2.30 mg·g^(-1),0-7.53 mg·g^(-1)and 0-6.02 mg·g^(-1),respectively,in 18 batches of Dendrobii Officinalis Caulis.The distribution and contents of 10 carbohydrate components in Dendrobii Officinalis Caulis had a certain correlation with the cultivation area.Conclusion:The established method is rapid,accurate,reproducible and simple,and can be used for simultaneous determination of monosaccharide and oligosaccharide components in Dendrobii Officinalis Caulis.

关 键 词：高效液相色谱 电喷雾式检测器 铁皮石斛 单糖 寡糖 低聚麦芽糖 

分 类 号：R917[医药卫生—药物分析学]