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  • Author or Editor: J.W Guo x
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A rapid method has been used for simultaneous identification of both hydrophilic and lipophilic compounds from Radix Salviae Miltiorrhizae (RSM, the root of Salvia miltiorrhiza BGE.) by ultra-performance liquid chromatography/quadrupole time-offlight mass spectrometry (UPLC/Q-TOF-MS). A total of 58 compounds extracted by methanol were detected and tentatively identified within 20 min, including hydrophilic phenolics, lipophilic diterpenoids, a verbascose, and several organic acids. These compounds were separated on an Acquity UPLC BEH C18 column and identified based on tandem mass spectrometry (MS/MS) fragmentation patterns under the positive and negative ion modes, respectively. Among them, micranthin B and 9-oxo-10E,12Zoctadecadienoic acid were reported in RSM for the first time. Their fragmentation patterns in electrospray ionization (ESI)—MS/MS spectra were first investigated by matching their accurate molecular masses. This contribution presented one of the first reports on the analysis of hydrophilic phenolics and lipophilic diterpenoids from Radix Salviae Miltiorrhizae using UPLC/Q-TOF-MS. The results demonstrated that UPLC/Q-TOF-MS method could be applied to rapidly and expediently describe and provide comprehensive chemical information for simultaneous analysis of two different polar components in RSM.

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A method was developed for the preparative separation of two alkaloids from the crude extract of the radix of Rauvolfia verticillata (Lour.) Baill. in a single run. The two-phase solvent system composed of petroleum ether–ethyl acetate–methanol–water (5:5:2:8, v/v), where triethylamine (40 mmol/L) was added to the upper organic phase as the stationary phase and hydrochloric acid (10 mmol/L) was added to the lower aqueous phase as the mobile phase, was selected for this separation by pH-zone-refining counter-current chromatography (PZRCCC). For the preparative separation, the apparatus was rotated at a speed 850 rpm, while the mobile phase was pumped into the column at 2 mL/min. As a result, 112 mg of reserpine and 21 mg of yohimbine were obtained from 3 g of crude extract in a single run. The analysis of the isolated compounds was determined by high-performance liquid chromatography (HPLC) at 230 nm with purities of over 91.0%, and the chemical identification was carried out by the data of electrospray ionization–mass spectrometry (ESI–MS) and nuclear magnetic resonance (NMR) spectroscopy. The technique introduced in this paper is an efficient method for preparative separation of reserpine and yohimbine from devil pepper radix. It will be beneficial to utilize medicinal materials and also useful for the separation, purification, and pharmacological study of Chinese herbal ingredients.

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