Authors:L. Lv, L. Zhao, X. Wang, H. Zhang, Z. Zhu, Y. Chai, and G. Zhang
Epimedium pubescens Maxim. and Epimedium koreanum Nakai. are two common and confused species of Herba Epimedii in Chinese Pharmacopoeia 2010 edition. Different species and growing conditions lead to chemical differences between the two species which may result in the improper clinical usage. In this work, a new method based on rapid-resolution liquid chromatography combined with time-of-flight mass spectrometry (RRLC/TOFMS) has been developed for identification and differentiation of major flavonoids in two kinds of Epimedium extract and rat plasma. The compounds were identified effectively based on the accurate extract masses and formulae acquired by RRLC/TOFMS. The fragmentation rules deduced by collision-induced dissociation (CID) were successfully implemented in distinguishing some of the isomers, further validating the results. By using the combined analytical techniques, a total of 40 major flavonoids in extracts of two kinds of Epimedium were identified within 30 min, including 31 common components and 9 characteristic components. After oral administration, three prototype compounds in rat plasma were detected by comparing the constituents measured in vitro with those in vivo, and five metabolites were identified by contrasting the fragmentation rules. The identification and structural elucidation of the chemical constituents provided essential data for further pharmacological and clinical studies on different species of Epimedium.
Authors:W. Xiong, R.Q. Yan, Y.N. Liu, S.W. Peng, Z.Z. Jiang, X. Chai, A.D. Qi, and Y.F. Wang
Compound danshen preparations (CDPs) are used clinically for the treatment of cardiovascular and cerebrovascular diseases. By using the quantitative analysis of multi-components by single-marker (QAMS) method, sixteen compounds (danshensu, protocatechuic acid, protocatechuicaldehyde, caffeic acid, rosmarinic acid, lithospermic acid, notoginsenoside R1, salvianolic acid B, ginsenoside Rg1, ginsenoside Re, salvianolic acid A, salvianolic acid C, ginsenoside Rb1, ginsenoside Rd, cryptotanshinone, and tanshinone IIA were quantified on an ACQUITY ultraperformance liquid chromatography (UPLC) HSS T3 column (2.1 × 100 mm, 1.8 μm) with the mobile phase consisting of 0.1% formic acid aqueous solution (A) and acetonitrile (B) using a gradient elution at the flow rate of 0.30 mL/min in 30 min at 30°C, which was also validated by UPLC-diode array detection (DAD) and UPLC-electrospray ionization multistage/mass spectrometry (ESI-MS/MS) for assuring the feasibility and accuracy. Tested by robustness experiment under slightly changeable conditions, the stability of relative correction factor (RCF) proved to be stable, with RSDs below 5.69%, except for notoginsenoside R1 with relative standard deviation (RSD) 7.83%. This reliable and convenient QAMS method resolved the problem of standard substance insufficiency and improved the quality assessment of preparations consisting of complex compounds with different chemical structures, such as CDPs.