A phytochemical investigation was carried out on the extract of a medicinal plant Callicarpa nudiflora, resulting in the characterization of five new 3, 4-seco-isopimarane (1-5) and one new 3, 4-seco-pimarane diterpenoid (6), together with four known compounds. The structures of the new compounds were fully elucidated by extensive analysis of MS, 1D and 2D NMR spectroscopic data, and time-dependent density functional theory (TDDFT) calculation of electronic circular dichroism (ECD) spectra, and DFT calculations for NMR chemical shifts and optical rotations.
Abietanes/isolation & purification* ; Callicarpa/chemistry* ; Diterpenes/isolation & purification* ; Molecular Structure ; Phytochemicals/isolation & purification* ; Plant Leaves

This study is to investigate the chemical constituents from the whole plant Corydalis edulis. The chemical constituents were separated and purified by macroporous resin D101, silica gel, Sephadex LH-20, ODS, and semi-preparative HPLC. Their structures were determined by physicochemical properties and spectroscopic data. Four compounds were isolated from the dichloromethane and water extracts of the whole plant C. edulis, and identified as 6'-β-D-xylosylicariside B2(1),(3S,5R,6S,7E)-5,6-epoxy-3-hydroxy-7-megastigmen-9-one(2), loliolide(3), and 5,5'-dimethoxybiphenyl-2,2'-diol(4), respectively. Compound 1 is a new compound, of which the absolute configuration was established by electronic circular dichroism(ECD) calculations. Compound 4 is obtained from the plants of Papaveraceae family for the first time. Compounds 2 and 3 are firstly isolated from the Corydalis genus.
Chromatography, High Pressure Liquid ; Corydalis/chemistry* ; Glycosides/isolation & purification* ; Molecular Structure ; Phytochemicals/isolation & purification* ; Sesquiterpenes/isolation & purification*

A method was established for simultaneous determination of 21 active constituents including flavanols, isoflavones, flavonols, dihydroflavones, dihydroflavonols, chalcones, pterocarpan, anthocyanidins and phenolic acids in Spatholobi Caulis by ultra fast liquid chromatography with triple quadrupole linear ion trap mass spectrometry(UFLC-QTRAP-MS/MS). Then, it was employed to analyze and evaluate the dynamic accumulation of multiple bioactive constituents in Spatholobi Caulis. The chromatographic separation was performed on a XBridge®C_(18)(4.6 mm×100 mm, 3.5 μm) at 30 ℃ with a gradient elution of 0.3% formic acid aqueous solution-methanol, and the flow rate was 0.8 mL·min~(-1), using multiple-reaction monitoring(MRM) mode. A comprehensive evaluation of the multiple bioactive constituents was carried out by gray correlation analysis(GRA). The 21 target components showed good linearity(r>0.999 0) in the range of the tested concentrations. The average recovery rates of the 21 components were from 97.46% to 103.6% with relative standard deviations less than 5.0%. There were differences in the contents of 21 components in Spatholobi Caulis at diffe-rent harvest periods. Spatholobi Caulis had high quality from early November to early December, which is consistent with the local tradi-tional harvest period. This study reveals the rule of the dynamic accumulation of 21 components in Spatholobi Caulis and provides basic information for the suitable harvest time. At the same time, it provides a new method reference for the comprehensive evaluation of the internal quality of Spatholobi Caulis.
Chromatography, High Pressure Liquid ; Fabaceae/chemistry* ; Phytochemicals/isolation & purification* ; Plant Stems/chemistry* ; Plants, Medicinal/chemistry* ; Tandem Mass Spectrometry

The present work is to establish an HPLC characteristic chromatograms of Asarum heterotropoides var. mandshuricum(AH) and A. sieboldii(AS), combined with cluster analysis for the identification of the two species, and predict their potential anti-inflammatory related targets by network pharmacological method. Eighty-nine samples(12 batches of AS and 77 batches of AH) were analyzed, and 11 characteristic peaks were identified by reference substances, UV spectrum and LC-MS. Cluster analysis showed that AS and AH were divided into two groups, and the ratio of characteristic peak areas can be used to distinguish them. When the ratio of characteristic peak sarisan to kakuol was greater than 5, it was AS, and when the ratio was less than 2, it was AH. The network pharmacological analysis of 119 constituents of Asari Radix et Rhizoma suggested that the anti-inflammatory effect of Asari Radix et Rhizoma might be related to COX-2, COX-1, iNOS, MAPK14, NR3 C1, PPARG and TNF. Among them, COX-2 is a relatively key target, which interacted with the characteristic constituents, asarinin, sesamin, safrole, methyleugenol and sarisan. The characteristic constituents asarinin and sesamin also interacted with the iNOS and MAPK14. Safrole and sarisan can also interact with iNOS, COX-1 and LAT4 H. Methyleugenol also showed interaction with COX-1 and LAT4 H. Since asarinin and sesamin interacted with three targets, COX-2, iNOS and MAPK14, it implied that they were the main active constituents for the anti-inflammatory activity of Asari Radix et Rhizoma. The COX-2 inhibitory activities of asarinin and sesamin were further studied by molecular docking and bioassay. The HPLC method established was simple, feasible and reliable, with predicted anti-inflammatory targets and anti-inflammatory constituents, which could provide a reference for improving the quality evaluation system of Asari Radix et Rhizoma.
Anti-Inflammatory Agents/isolation & purification* ; Asarum/chemistry* ; Chromatography, High Pressure Liquid ; Molecular Docking Simulation ; Phytochemicals/isolation & purification* ; Rhizome/chemistry*

The chemical compounds in water extract of Spatholobi Caulis were further studied. The compounds were systematically isolated and purified by using various separation and analysis techniques including silica gel, macroporous adsorptive resins and Sephadex LH-20 column chromatographies, as well as reversed phase high-performance liquid chromatography(RP-HPLC). Twenty-three flavonoids and one chromone were identified by the spectroscopic analysis techniques combining their physicochemical properties, they were identified as isoduartin(1), sativan(2), 8-O-methylretusin(3), 7-hydroxydihydroflavone(4), odoratin(5), butesuperin A(6), biochanin A(7), 3'-methoxydaidzein(8), 7-hydroxychromone(9), calycosin(10), naringenin(11), dihydrocajanin(12),(6 aR,11 aR)-maackiain(13), 2'-hydroxygenistein(14),(6 aR,11 aR)-medicarpin-3-O-glucopyranoside(15),(-)-epiafzelechin(16),(-)-catechin(17),(-)-epicatechin(18), 4',8-dimethoxy-7-O-β-D-glucopyranosylisoflavone(19), ononin(20),(-)-gallocatechin(21), rutin(22), daidzin(23) and sphaerobioside(24). Compounds 4, 6, 8, 9, 11, 12, 14-16, 19 and 22-24 were isolated from Spatholobi Caulis for the first time.
Chromatography, High Pressure Liquid ; Drugs, Chinese Herbal/chemistry* ; Fabaceae/chemistry* ; Flavonoids/isolation & purification* ; Phytochemicals/isolation & purification*

An UPLC method was established for the direct determination of six major bioactive isosteroidal alkaloids, namely peimisine, imperialine, sipeimine-3-D-glucoside, verticinone, verticine and hupehenine from the bulbus of Fritillaria(Beimu), a commonly used antitussive traditional Chinese medicinal(TCM) herb. An Acquity UPLC~(TM) CSH C_(18) column(2.1 mm×100 mm, 1.7 μm) was used for all analysis. The investigated six compounds were all separated with gradient mobile phase consisting of 0.02% diethylamine-water-methanol at a flow rate of 0.3 mL·min~(-1). The temperature of sample manager was set at 20 ℃. Drift tube temperature was 45 ℃, and spray parameter was 40% with injection volume of 1 μL. Then, the further quality assessment of Beimu was carried out by cluster analysis(CA) and principal component analysis(PCA). The investigated all had good linearity(r≥0.998 9) over the tested ranges. The method is simple, accurate and reproducible, and can be used for determining the content of six major bioactive isosteroidal alkaloids.
Alkaloids/isolation & purification* ; Chromatography, High Pressure Liquid ; Drugs, Chinese Herbal/chemistry* ; Fritillaria/chemistry* ; Phytochemicals/isolation & purification* ; Plant Roots/chemistry*

Danshen, the dried root or rhizome of Salvia miltiorrhiza Bge., is a traditional and folk medicine in Asian countries, especially in China and Japan. In this review, we summarized the recent researches of Danshen in traditional uses and preparations, chemical constituents, pharmacological activities and side effects. A total of 201 compounds from Danshen have been reported, including lipophilic diterpenoids, water-soluble phenolic acids, and other constituents, which have showed various pharmacological activities, such as anti-inflammation, anti-oxidation, anti-tumor, anti-atherogenesis, and anti-diabetes. This article intends to provide novel insight information for further development of Danshen, which could be of great value to its improvement of utilization.
Diterpenes ; chemistry ; Drugs, Chinese Herbal ; chemistry ; isolation & purification ; pharmacology ; therapeutic use ; Hydroxybenzoates ; chemistry ; Molecular Structure ; Oils, Volatile ; chemistry ; Phytochemicals ; chemistry ; isolation & purification ; pharmacology ; therapeutic use ; Plant Roots ; chemistry ; Quality Control ; Salvia miltiorrhiza ; chemistry

The hydrogen peroxide generation system was used to analyze the scavenging activity of hydrogen peroxide by Liropes Radix from different origins by HPLC-UV-CL. The UV-CL fingerprints of Liropes Radix from different origins were evaluated,and the HPLC-UV and LC-CL fingerprints were systematically analyzed and evaluated. The results showed that the ether fractions of Liriope spicata var. prolifera and L. muscari had good scavenging activity of hydrogen peroxide,and the total activity of different origins varied greatly,while the similar samples had similar activities. The total antioxidant activity of L. muscari is higher than that of L. spicata var.prolifera. The similarity analysis of the two fingerprints was carried out by two different analytical methods. The chemical fingerprints and the active fingerprints have different characteristics. The contribution of each fingerprint to the total peak area and total activity is also different. There are significant differences between the two different fingerprint clustering results.
Chromatography, High Pressure Liquid ; Drugs, Chinese Herbal ; Free Radical Scavengers ; chemistry ; Hydrogen Peroxide ; isolation & purification ; Liriope Plant ; chemistry ; Phytochemicals ; chemistry ; Plant Extracts ; chemistry ; Plant Roots ; chemistry

Six compounds were isolated from the aerial part of cultivated Clerodendranthus spicatus in Hainan with various chromatographic techniques,and their structures were determined as:1-dehydroxy-1-oxo-rupestrinol(1),N-trans-feruloyltyramine(2),methyl 3,4-dihydroxyphenyllactate(3),caffein acid(4),methyl caffeate(5) and ethyl caffeate(6),via analysis of physicochemical properties and spectroscopic evidence.Compound 1 was a new compound,while compounds 2 and 3 were isolated from C.spicatus for the first time.Biological activity results showed that compounds 2-4 exhibited α-glucosidase inhibitory activity with different inhibition ratio.
China ; Glycoside Hydrolase Inhibitors ; isolation & purification ; pharmacology ; Lamiaceae ; chemistry ; Molecular Structure ; Phytochemicals ; isolation & purification ; pharmacology ; Sesquiterpenes, Eudesmane ; isolation & purification ; pharmacology

Eleven flavonoids were isolated from the twigs of Broussonetia papyrifera by column chromatography over silica gel,ODS,MCI gel,and Sephadex LH-20,as well as RP-HPLC.Their structures were identified by spectroscopic methods including NMR,MS,UV,and IR as broupapyrin A(1),5,7,3',4'-tetrahydroxy-3-methoxy-8-geranylflavone(2),8-prenylquercetin-3-methyl ether(3),broussonol D(4),broussoflavonol B(5),uralenol(6),broussonol E(7),8-(1,1-dimethylallyl)-5'-(3-methylbut-2-enyl)-3',4',5,7-tetrahydroxyflanvonol(8),broussoflavonol E(9),4,2',4'-trihydroxychalcone(10),and butein(11).Compound 1 is a new isoprenylated flavonol.Compounds 3,6,10,and 11 were obtained from the genus Broussonetia for the first time,and 4 and 7 were firstly discovered in B.papyrifera.Compounds 1-5 and 7-9 showed significant inhibitory effects on PTP1 B with IC50 values ranging from(0.83±0.30) to(4.66±0.83) μmol·L-1.
Broussonetia ; chemistry ; Chromatography, High Pressure Liquid ; Flavonoids ; isolation & purification ; pharmacology ; Magnetic Resonance Spectroscopy ; Phytochemicals ; isolation & purification ; pharmacology ; Protein Tyrosine Phosphatase, Non-Receptor Type 1 ; antagonists & inhibitors