摘要
目的对当归芍药散中化学成分进行研究。方法采用液相色谱-四级杆-飞行时间质谱(LC-Q-TOF-MS)和液相色谱-离子阱-质谱(LC-IT-MSn)对当归芍药散70%乙醇-水提物进行分析,色谱柱为Agilent Zorbax SB-C18、Rapid Resolution HT(50 mm×4.6 mm,1.8μm),流动相为0.05%甲酸水(A)-乙腈(B),梯度洗脱,体积流量为0.6 mL/min。结合LC-Q-TOF-MS提供的化合物准确相对分子质量和LC-IT-MS分析获得的化合物多级质谱信息,对当归芍药散化学成分进行结构推测鉴定,并对化合物的药材来源进行归属。结果共鉴定了当归芍药散中30个成分,其中14个为首次在当归芍药散中发现,包括以绿原酸(8)和没食子酰蔗糖(5~7)为代表的6个有机酸及其苷类化合物,以16-氧化泽泻醇A 23-乙酸酯(22)为代表的2个原萜烷型三萜类化合物,以环四(异)亮氨酸(14)为代表的4个环肽类化合物以及N-(1-deoxy-D-fructos-1-yl)pyroglutamic acid(1)和腺苷(3)等。结论研究结果加深了对当归芍药散化学组成的理解,为其药效物质基础研究及质量控制提供了一定的理论依据。
Objective To study the constituents in Danggui-Shaoyao-San （DSS, a powder prescription with Angelicae Sinensis Rad＆, Paeoniae Radix Alba, Atractylodis Macrocephalae Rhizoma, Poria, Alismatis Rhizome, and Chuanxiong Rhizome）. Methods To analyze the 70% ethanol-water extract from DDS by LC-Q-TOF-MS and LC-IT-MS. The analysis was performed on an Agilent Zorbax SB-CI8 column and Rapid Resolution HT column （50 mm × 4.6 mm, 1.8 μm） with gradient elution of 0.05% formic acid （A）-acetonitrile （B） at the flow rate of 0.6 mL/min. The constituents from DSS were identified according to the relative molecule weight by LC-Q-TOF-MS and multistage MS informatics by LC-IT-MS. All the peaks were assigned to the corresponding traditional Chinese medicinal materials. Results Thirty compounds from DDS could be identified, and 14 of them were identified for the first time in DSS including six organic acids, such as chlorogenic acid （8） and galloylsucrose （5-7）; two protostane trierpenoids, such as 16-oxoalisol A 23-acetate （22）; four cyclopeptides, such as cyclo tetraleucyl （or isoleucyl） （14） and other types of compounds, such as N-（1-deoxy-D-fructos-l-yl） pyroglutamic acid （1） and adenosine （3）. Conclusion This work investigates the compounds from DSS, and the results could provide the evidence for the research on active constituents and quality control of DSS.
出处
《中草药》
CAS
CSCD
北大核心
2014年第8期1056-1062,共7页
Chinese Traditional and Herbal Drugs
基金
国家重大新药创制科技重大专项(2011ZX09307-002-01)
