Authors:W. J. Duan, Z. J. Zheng, Y. L. Geng, J. H. Liu, and X. Wang
A preparative high-speed countercurrent chromatograph (HSCCC) method for the isolation and purification of C6-C2 natural alcohol and benzyl ethanol from Forsythia suspensa was successfully established. Cornoside, forsythenside F, forsythiaside, and acteoside were rapidly obtained for the first time by HSCCC with a two-phase solvent system ethyl acetate-n-butanol-methanol-water (5:1:0.5:5, υ/υ) in one-step separation. The purities of them were all above 97% as determined by high-performance liquid chromatography, and the combination of ESI-MS and NMR analysis confirmed the chemical structures of the four compounds.
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.
Citri Grandis Exocarpium (CGE) is a traditional Chinese medicine with a variety of biological activities. For efficient quality control of CGE, a simple, rapid, and accurate high-performance liquid chromatographic (HPLC) method was developed for simultaneous determination of four main compounds (naringin, rhoifolin, meranzin hydrate, and isoimperatorin) in this herb. These four compounds were separated on a C18 column by gradient elution with methanol and water. The flow rate was 1.0 mL·min−1, and the detection wavelength was 324 nm. The recoveries of the method ranged from 96.32% to 103.71%, and good linear relationships (r2 > 0.9998) over relative wide concentration ranges were obtained. Then this validated method was successfully applied to the analysis of nine batches of CGE samples.
Authors:Y. C. Xiao, L. T. Liu, J. J. Bian, C. Q. Yan, L. Ye, M. X. Zhao, Q. S. Huang, W. Wang, K. Liang, Z. F. Shi, and X. Ke
Shuganjieyu (SGJY) capsule is a classical formula widely used in Chinese clinical application. In this paper, an ultra-performance liquid chromatography coupled with electrospray ionization and ion trap mass spectrometry has been established to separate and identify the chemical constituents of SGJY and the multiple constituents of SGJY in rats. The chromatographic separation was performed on a C18 RRHD column (150 × 2.1 mm, 1.8 μm), while 0.1% formic acid–water and 0.1% formic acid–acetonitrile was used as mobile phase. Mass spectral data were acquired in both positive and negative modes. On the basis of the characteristic retention time (Rt) and mass spectral data with those of reference standards and relevant references, 73 constituents from the SGJY and 15 ingredients including 10 original constituents and 5 metabolites from the rat plasma after oral administration of SGJY were identified or tentatively characterized. This study provided helpful chemical information for further pharmacology and active mechanism research on SGJY.