超高效液相色谱法同时检测丹参中14种水溶性成分  

Simultaneous Detection of 14 Hydrophilic Components in Salvia miltiorrhiza by UPLC

作　　者：李垚 杨德智[1] 苏斌 杜冠华[3] 吕扬[1] LI Yao;YANG Dezhi;SU Bin;DU Guanhua;LYU Yang(Beijing Key Laboratory of Polymorphs Drugs Research,Institute of Materia Medica,Chinese Academy of Medical Sciences and Peking Union Medical College,Beijing 100050.China;Shandong Jishi Pharmacy Company,Laiwu 271100.China;Beijing Key Laboratory of Drug Target and Screening Research,Institute of Materia Medica,Chinese Academy of Medical Sciences and Peking Union Medical College,Beijing 100050.China)

机构地区：[1]北京协和医学院中国医学科学院药物研究所晶型药物研究北京市重点实验室,北京100050 [2]山东济世药业有限公司,莱芜271100 [3]北京协和医学院中国医学科学院药物研究所药物靶点研究和新药筛选北京市重点实验室,北京100050

出　　处：《医药导报》2019年第12期1624-1629,共6页Herald of Medicine

基　　金：中国医学科学院医学与健康科技创新工程重大项目(2016-I2M-3-007);国家“十三五”重点研发计划(2016YFC1000901);国家科技重大专项重大新药创制(20182X971101-003-022);中国医学与健康科技创新工程重大项目(2017-I2M-1-010)

摘　　要：目的建立超高效液相色谱法(UPLC)同时测定丹参不同部位中的丹参素、原儿茶酸、原儿茶醛、咖啡酸、阿魏酸、异阿魏酸、迷迭香酸、紫草酸、丹酚酸B、丹酚酸A、丹酚酸C、9 丹酚酸B单甲酯、9’丹酚酸B单甲酯、丹酚酸B二甲酯14种水溶性成分含量,并考察丹参药材直径和丹参植株部位对以上成分含量的影响。方法采用Waters ACQUITY UPLC BEH C18(2.1 mm×50 mm,1.7μm)色谱柱,以0.5%乙酸溶液(A)-乙腈(B)为流动相,按梯度洗脱:0~1.02 min,90%→80%A;>1.02~4.08 min,80%→72%A;>4.08~4.76 min,72%→55%A;>4.76~5.50 min,55%→90%A;>5.50~8 min,90%A。柱温30℃,进样量1μL,检测波长286 nm,流速为0.6 mL·min^-1。结果在8 min内,上述14种水溶性成分可实现完全分离且浓度与峰面积之间线性良好,仪器和方法重复性良好,其RSD均小于2.0%,可实现准确定量,丹参药材直径和参植株部位对水溶性成分含量有很大影响。结论所建立UPLC色谱法分离度好,灵敏度高,定量准确,直径为0.1~0.5 cm的丹参药材和丹参周皮中上述14种成分含量表现出较大优势。Objective To establish a UPLC method for the simultaneous determination of 14 hydrophilic components, including danshensu, protocatechuic acid, protocatechuic aldehyde, caffeic acid, ferulic acid, isoferulic acid, rosmarinic acid, glucursoric acid, salvianolic acid B, salvianolic acid A, salvianolic acid C, -saltanoic acid B monomethyl ester, 9’-salvianolic acid B monomethyl ester and salvianolic acid B dimethyl ester, in different parts of Salvia miltiorrhiza, and to investigate the effects of diameter and parts of Salvia miltiorrhiza on the contents of 14 components above. Methods The UPLC analysis was performed on a Waters ACQUITY UPLC BEH C18(2.1 mm×50 mm, 1.7 μm) column with the mobile phase of 0.5% acetic acid solution(A)-acetonitrile(B) at a flow rate of 0.6 mL·min^-1.The separation was achieved using the following gradient: 0-1.02 min, 90% A-80% A;1.02-4.08 min, 80% A-72% A;4.08-4.76 min, 72% A-55% A;4.76-5.50 min, 55% A-90% A;5.50-8 min, 90% A-90% A.The injection volume was 1 μL and the detection wavelength was set at 286 nm.The column temperature was kept at 30 ℃. Results The above 14 hydrophilic components were completely separated within 8 min and each substance had a good linearity.The instrument and method had a good repeatability with RSD below 2.0%, thus accurate quantification was achieved.The diameter and parts of Salvia miltiorrhiza had significant influences on the contents of hydrophilic components. Conclusion The established UPLC chromatographic method had good resolution, high sensitivity and accurate quantitative determination.Roots of Salvia miltiorrhiza with diameters between 0.1 cm and 0.5 cm and periderms of Salvia miltiorrhiza had advantages over others in the content of the hydrophilic components.

关 键 词：丹参 水溶性成分 含量测定 色谱法 超高效液相 

分 类 号：R917[医药卫生—药物分析学] R284.1[医药卫生—药学]