三棱乙酸乙酯部位HPLC指纹图谱及4种酚类成分含量测定  

HPLC fingerprints of EtOAc extracts and determination of four phenolic compounds in Rhizoma Sparganii

作　　者：徐男[1,2] 曹铭晨 黄欣 王鹏[3] 孙蓉[1] 韩利文[4] 苏乐群[3] 李宏建[3] 时海燕[3] 

机构地区：[1]山东省中医药研究院,山东济南250014 [2]山东中医药大学中医学博士后流动站,山东济南250355 [3]山东省千佛山医院,山东济南250014 [4]山东省科学院生物研究所,山东济南250014

出　　处：《中国医院药学杂志》2017年第18期1783-1786,1791,共5页Chinese Journal of Hospital Pharmacy

基　　金：山东省自然科学基金项目(编号:ZR2015HL117);国家公益性行业专项(201507004-4);山东省自主创新和成果转化项目(编号:2014ZZCX02104);国家重点基础研究发展计划(973)中医基础理论专项资助项目(编号:2009CB522802);山东省科技平台建设项目课题(编号:2008GG2NS02021);山东省泰山学者工程专项经费资助项目

摘　　要：目的:建立醋炙三棱乙酸乙酯部位HPLC指纹图谱,并同时测定对羟基苯甲酸、香兰素、对香豆酸和阿魏酸4种酚类物质含量,为三棱药材的质量控制提供借鉴。方法:富集醋炙三棱乙酸乙酯部位,采用高效液相色谱(HPLC)法,应用Inert Sustain C18色谱柱(4.6 mm×250 mm,5μm),流动相甲醇-0.1%甲酸溶液进行梯度洗脱,检测波长254 nm,流速0.80 mL·min-1,测定对羟基苯甲酸、香兰素、对香豆酸和阿魏酸4种酚类物质的含量。结果:建立了三棱乙酸乙酯部位的HPLC指纹图谱,检出共有峰16个,各批次药材的相似度均大于0.9;通过与对照品比对,确定了指纹图谱中5,8,9,10号峰分别为对羟基苯甲酸、香兰素、对香豆酸和阿魏酸,并对其进行定量分析,结果对羟基苯甲酸的线性范围为0.008~0.924μg,平均回收率为98.5%,香兰素的线性范围为0.039~4.712μg,平均回收率为101.1%,对香豆酸的线性范围为0.054~6.572μg,平均回收率为100.3%,阿魏酸的线性范围为0.018~2.236 ng,平均回收率为101.0%。结论:HPLC指纹图谱方法与含量测定方法简便,结果准确,重复性好,可作为三棱的质量控制方法。OBJECTIVE To establish HPLC fingerprints of EtOAc extracts and simultaneously determine the contents of phydroxybenzoic acid,vanillin,p-coumaric acid and ferulic acid in Rhizoma Sparganii for quality control.METHODS Inert Sustain C18column（4.6 mm×250 mm,5μm）was used to elute with methanol-0.1%formic acid as mobile phase,at the detection wave length of 254 nm and flow rate at 0.80 mL·min^-1.RESULTS The chromatographic fingerprints of EtOAc extracts in Rhizoma Sparganii were established,and 16 peaks were detected.The similarity of each batch was more than 0.9.By comparing the reference substance,P-hydroxybenzoic acid,vanillin,p-coumaric acid and ferulic acid were confirmed.The linear range of p-hydroxybenzoic acid was 0.008-0.924 g and recovery was 98.5%,the linear range of vanillin was 0.039-4.712 g and recovery was 101.1%,the linear range of coumaric acid was 0.054-6.572 g and recovery was 100.3%,the linear range of ferulic acid was 0.018-2.236 g and recovery was 101.0%,respectively.CONCLUSION HPLC fingerprinting method and content determination method are simple,accurate and reproducible,and can be used as quality control methods for Rhizoma Sparganii.

关 键 词：三棱 乙酸乙酯部位 HPLC 指纹图谱 多成分含量测定 

分 类 号：R927.2[医药卫生—药学]