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Loganin, sweroside, and morroniside, three main iridoid glycosides fromFructus Corniwere successfully separated by macroporous resin column chromatography and countercurrent chromatography (CCC). In the first step, D101 macroporous resin was selected for cleaning-up, water was used to elute the column to remove the undesired constituents and then 50% aqueous ethanol was used to elute the targets. The total content of three iridoid glycosides was 51.1% in this process. In the second step, the obtained crude sample was then isolated by CCC using a two-phase solvent system composed of dichloromethane-methanol-n-butanol-water-acetic acid (5:5:2:4:0.1,v/v/v/v/v). From 100 mg of a crude sample, 12.6 mg of loganin, 5.9 mg of sweroside, and 28.5 mg of morroniside were obtained with purities of 98.6%, 97.3%, and 99.1% and total recoveries of 90.4%, 91.8%, and 89.1%, respectively, after a two-step purification. The HPLC quantitative analysis and response surface methodology were used for optimization of the separation condition and the target compounds were identified by ESI-MS,1H NMR, and13C NMR. [ABSTRACT FROM PUBLISHER]

Selective and efficient analytical methods for authentication and quality evaluation of herbal medicines are significant and necessary. An expeditious method combining multi-components determination and fingerprinting based on ultra-performance liquid chromatography-photo diode array-tandem mass spectrometry (UPLC-PDA -MS/MS) and chemometrics for authentication and quality evaluation of Cornus Officinalis Sieb. et Zucc was developed. Tandem mass spectrometer operating in multiple reaction monitoring (MRM) was used for determination of three characteristic constituents (morroniside, sweroside, and loganin) in C. Officinalis. Meanwhile, UPLC fingerprint of C. Officinalis was established and the data set was submitted for classification to a suite of chemometrics method. Combing main biologically active components content level and chemometrics analysis, the effects of cultivation area, harvesting, and storage time on the quality of C. Officinalis were investigated. The study reveals that multi-components determination coupled with fingerprinting could be applied for authentication and quality evaluation of C. Officinalis which is accurate, efficient, and reliable. [ABSTRACT FROM AUTHOR]

By using a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (2:2:2:2, v/v/v/v), a high-speed counter-current chromatography technique was successfully used for isolation and purification of three alkaloids from Picrasma quassiodes (D. Don) Benn. for the first time. A total of 22.1 mg of 3-methylcanthin-2,6-dione, 4.9 mg of 4-methoxy-5-hydroxycanthin-6-one and 1.2 mg of 1-methoxycarbonyl-β-carboline were obtained from 100 mg of crude extract of Picrasma quassiodes (D. Don) Benn. in less than 5 hr, with purities of 89.30%, 98.32%, and 98.19%, respectively. The target compounds were identified by ESI-MS, 1H NMR, and 13C NMR. [ABSTRACT FROM AUTHOR]

Coupled with evaporative light scattering detection, a high-speed counter-current chromatography (HSCCC) method was developed for preparative isolation and purification of three glycine-conjugated cholic acids, glycochenodeoxycholic acid (GCDCA), glycohyodeoxycholic acid (GHDCA), and glycohyocholic acid (GHCA) from Pulvis Fellis Suis (Pig gallbladder bile) for the first time. The separation was performed with a two-phase solvent system consisted of chloroform-methanol-water-acetic acid (65:30:10:1.5, v/v/v/v) by eluting the lower phase in the head-to-tail elution mode. The revolution speed of the separation column, flow rate of the mobile phase, and separation temperature were 800 rpm, 2 mL/min and 25°C, respectively. In a single operation, 33 mg of GCDCA, 38 mg of GHDCA, and 23 mg of GHCA were obtained from 200 mg of crude extract with the purity of 95.65%, 96.72%, and 96.63%, respectively, in one-step separation. The HSCCC fractions were analyzed by high-performance liquid chromatography (HPLC) and the structures of the three glycine-conjugated cholic acids were identified by ESI-MS, 1H NMR, and 13C NMR. [ABSTRACT FROM PUBLISHER]

Coupled with evaporative light scattering detection, high-speed countercurrent chromatography was successfully applied for the first time for separation and purification of four triterpene saponins including esculentosides A, B, C, and D from the roots of Radix phytolaccae. The separation was performed with an optimized two-phase solvent system composed of chloroform-methanol-water (4:4:2,v/v), using the lower phase as the mobile phase at a flow rate of 1.5 mL/min. From 150 mg of crude extract, 46.3 mg of esculentoside A, 21.8 mg of esculentoside B, 7.3 mg of esculentoside C, and 13.6 mg of esculentoside D were obtained at purities of 96.7%, 99.2%, 96.5%, and 97.8%, respectively, as determined by HPLC analysis. The structures of the four triterpene saponins were identified by ESI-MS,1H NMR and 13C NMR. [ABSTRACT FROM AUTHOR]

Two saponins: scrokoelziside A (1), scrokoelziside B (2), one iridoid glycoside, eurostoside (3), and two flavonoids: nepitrin (4) and homoplantaginin (5), were isolated from the leaves of Scrophularia ningpoensis for the first time. Moreover, eight known compounds: cane sugar (6), harpagide (7), aucubin (8), 6-O-methylcatalpol (9), harpagoside (10), angoroside C (11), β-sitosterol (12) and β-sitosterol glucoside (13) were isolated from the roots of S. ningpoensis. Furthermore, the antimicrobial activity of the extracts of the leaves of S. ningpoensis and the 10 compounds (1, 2, 3, 4, 5, 7, 8, 9, 10, 11) was studied in vitro against eight reference strains of bacteria by using the disc-diffusion method and micro-well dilution assay. The extracts of leaves and scrokoelziside A are effective against beta-haemolytic streptococci but had no effect against other strains. The extract of roots and other compounds showed no activity against all bacterial strains at the test concentration. [ABSTRACT FROM AUTHOR]

In this study, we reported a high throughout isolation procedure of pinoresinol diglucoside (PDG) and liriodendrin (SDG) from the traditional Chinese medical plant Eucommia ulmoides Oliv. by high speed countercurrent chromatography. The solvent system consisted of n‐butanol‐acetic acid‐water(4∶1∶5, v/v/v), in which the lower phase was used as the mobile phase at a flow‐rate of 2.0 mL · min-1 in the head to tail elution mode. The method yielded 21 mg of PDG at 96.7% purity and 16 mg of liriodendrin at 95.5% purity from 200 mg of crude extract in a one step. The purity and identity of the isolated compounds were checked by high performance liquid chromatography (HPLC) analysis, in combination with mass spectrometry (MS), infrared spectrum (IR), and NMR measurements. [ABSTRACT FROM AUTHOR]