Flavonoid glycosides from the water extract of Artemisia annua L / 药学学报

Twenty one flavonoid glycosides were isolated and purified from n-butanol portion of the water extract of A. annua by various chromatographic techniques such as HP-20 macroporous adsorption resin, silica gel, ODS, Sephadex LH-20 gel column chromatography and preparative high performance liquid chromatography. Their structures were identified by analysis of physicochemical properties and spectral data, and determined as axillarin-7-O-β-D-xylopyranosyl-(1→6)-β-D-glucopyranoside (1), orientin (2), apigenin-6-C-β-D-glucopyranosyl-8-C-β-L-arabinopyranoside (3), apigenin-6-C-β-D-galactopyranosyl-8-C-β-L-arabinopyranoside (4), apigenin-6-C-β-L-arabinopyranosyl-8-C-β-D-glucopyranoside (5), apigenin-6-C-α-L-arabinofuranosyl-8-C-β-D-glucopyranoside (6), quercetin-3-O-β-D-glucopyranosyl-(1→2)-β-D-glucopyranoside (7), apigenin-6-C-α-L-arabinopyranosyl-8-C-β-D-glucopyranoside (8), vicenin-2 (9), patuletin-7-O-β-D-glucopyranoside (10), luteolin-6-C-glucopyranoside (11), vitexin (12), kaempferol-3-O-β-galactopyranosyl-(1→2)-β-glucopyranoside (13), quercetin-7-O-β-D-glucopyranoside (14), patuletin-3-O-β-D-glucopyranoside (15), 7-O-methyl-quercetagetin-6-O-β-D-glucopyranoside (16), quercetin-3-O-β-D-glucopyranoside (17), nepitrin (18), rutin (19), kaempferol-3-O-β-sophoroside (20), and patuletin-3-O-rutinoside (21). Compound 1 is a new compound, compounds 2, 4, 6, 7, 10, 11, 13, 15, 16, 18, 20 and 21 are isolated from A. annua for the first time. In the anti-inflammatory assay, compound 1 inhibited the release of IL-6 from LPS-induced RAW264.7 cells to significantly degrees with the high (100 μmol·L-1), medium (50 μmol·L-1), low (25 μmol·L-1) concentration.

Bibenzyls from Dendrobium officinale / 中国中药杂志

Fifteen bibenzyls were isolated and purified from the ethyl acetate extract of the stems of Dendrobium officinale by macroporous resin, MCI, silica gel, Sephadex LH-20, and ODS column chromatographies, as well as preparative thin-layer chromatography and preparative HPLC. The structures of compounds were identified according to the spectra data of ~1H-NMR, ~(13)C-NMR, and MS, and the physical and physiochemical properties: dendrocandin X(1), 3,4'-dihydroxy-4,5-dimethoxybibenzyl(2), 6″-de-O-methyldendrofindlaphenol A(3), 3,4-dihydroxy-4',5-dimethoxybibenzyl(4), dendrosinen B(5), 3,4,4'-trihydroxy-5-methoxybibenzyl(6), 3,3'-dihydroxy-4,5-dimethoxybibenzyl(7), 3,4'-dihydroxy-5-methoxybibenzyl(8), moscatilin(9), gigantol(10), 4,4'-dihydroxy-3,5-dimethoxybibenzyl(11), 3,4',5-trihydroxy-3'-methoxybibenzyl(12), 3-O-methylgigantol(13), dendrocandin U(14), and dendrocandin N(15). Compound 1 was a novel compound. Compound 2 was isolated from Dendrobium species for the first time. Compounds 3-7 were isolated from D. officinale for the first time.

Chemical constituents from Crotalaria sessiliflora L / 药学学报

In this study, we isolated and purified the extracts of the whole plant of Crotalaria sessiliflora L. by column chromatographic. Twelve compounds were isolated and identified as followings: sessiliflorin B (1), quercetin (2), kaempferol (3), soyasapogenol B (4), fernenol (5), neoechinulin A (6), ethyl 4-hydroxybenzoate (7), ethyl caffeate (8), 5,7-dihydroxychromone (9), crotadihydrofuran A (10), butesuperin B (11) and aurantiamide acetate (12). Compound 1 is a new compound, compound 3-12 were isolated from the plant for the first time.

Separation and authentication of tilianin and quality standards of semen of Dracocephalum moldavia / 中国中药杂志

Tilianin was separated and authenticated from the seeds of Dracocephalum moldavia, a Uygur medicine, by chromatographic technique and spectroscopic method. The purity of tilianin is more than 98% determined by HPLC area normalization method. Thin layer chromatography (TLC) method was used to separate tilianin from D. moldavia by mixture of chloroform-methanol (5: 1) as a developing solvent on high performance silicagel precoated plate (SGF254) and using aluminium trichloride as a chromogenic agent for qualitative identification of D. moldavia. To establish a HPLC method for quantitative analysis of D. moldavia, tilianin was used as a Quantitative marker and separated on a C18 (4.6 mm x 250 mm, 5 μm) column with acetonitrile-01% formic acid (25: 75) as the mobile phase and detected at 330 nm. The calibration curve of tilianin displayed ideal linearity over the range of 0.617 2-123.44 μg x mL(-1) with a regression equation of Y = 33.773X - 0.824 8 (r = 1). The average recovery of tilianin was 101.0% with RSD of 3.7%. The RSD values of intra-day and inter-day precision were less than 2%. The content of tilianin in 4 batches of the authenticated semen of D. Moldavia was between 0.016 and 0.187 mg x g(-1). The qualitative and quantitative method established is suitable for the quality evaluation and assessment of semen of D. Moldavia.

Quality standard study on Tibetan medicine Gentianae Urnulae Herba / 中国中药杂志

Gentianae Urnulae Herba, dried whole herb of Gentiana urnula,is a commonly used Tibetan medicine. However, only the character identification is used as quality control standard officially at present. As a part of project for the Chinese Pharmacopoeia (2015 edition), the quality standard of this species was established in this study. The tests of water content, total ash, acid-insoluble ash and ethanol-soluble extractives of the crude drugs were carried out following the methods recorded in appendix of Chinese Pharmacopeia (2010 edition, volume 1). The TLC identification method was established by using gentiournoside A as reference substance, and a mixture of ethyl acetate-methanol-water-formic acid(7:1. 5:1: 0. 2) as the developing solvent system on silica gel G TLC plate. The content of gentiournoside A was assayed by HPLC on an Agilent Zorbax SB-C18 (4.6 mm x 250 mm,5 μm) column, using acetonitrile-water (0.1% phosphoric acid) (26:74) as the mobile phase at a flow rate of 1.0 mL x min(-1). The column temperature is at 30 degrees C and the detection wavelength is at 240 nm. As a result, gentiournoside A and the other constituents were separated and presented the same fluorescence light comparing with the reference substance on TLC detected under the UV light(366 nm). The methodology validation for the assay of gentiournoside A showed that it was in a good linear correlation in the range of 0.009 95-0.398 g x L(-1) with the regression equation of Y = 1 467.1X +41.407(r = 0.999 9), and the average recovery was 98. 3% (RSD 2.2%). The mass fractions of gentiournoside A, water content, ethanol-soluble extractives of 15 batches samples were varied in the ranges of 0.175% -1.83%, 8.60% - 9.93% and 29.2% - 35.2%, respectively. Total ash and acid-insoluble ash were 10.2% - 17.2% and 5.26% - 10.8% detected from 10 batches samples. The recommended standards of quantitative indexes are that the mass fractions of gentiournoside A and extractives are not less than 0.80% and 26.0%, respectively; the water, total ash and acid-insoluble ash are not more than 12.0%, 15.0% and 8.0%, respectively.

Microbial glycosylation of cardamonin by Mucor spinosus / 药学学报

Microbial transformation of cardamonin by Mucor spinosus (CGMCC 3.3450) in preparative scale resulted in the isolation of two new products. Their structures were elucidated unambiguously by ESI-MS, 1H NMR, 13C NMR and 2D NMR spectra analyses as 4-O-beta-D-glucopyranosyl-6-hydroxy-2-methoxychalcone (1, 4-GluC) and 6-O-beta-D-glucopyranosyl-4-hydroxy-2-methoxychalcone (2, 6-GluC), respectively. The time-course of biotransformation by M. spinosus showed that both 4-GluC and 6-GluC appeared on the 2nd day. The optimal biotransformation temperature was 28 degrees C, the optimal biotransformation time was 72 h and the optimal concentration for cardamonin was 40 mg x mL(-1). This is the first time for successful microbial glycosylation of cardamonin in present research.

A new phenylpropanoid glycoside from Cirsium setosum / 药学学报

To study the chemical constituents of Cirsium setosum (Willd.) MB., 70% ethanol extract of the aerial parts was subjected to column chromatography. One new phenylpropanoid glycoside, sinapyl alcohol 9-O-(E)-p-coumaroyl-4-O-beta-D-glucopyanoside (1) was isolated, along with three known compounds: lycoperodine-1 (2), apigenin-7-O-(6"-(E)-p-coumaroyl)-beta-D-galactopyranoside (3) and quercetin (4). The structures were elucidated on the basis of spectral and chemical evidence. Compound 2 was obtained from Cirsium genus for the first time, compounds 3 and 4 were obtained from this plant for the first time.

One new galloyl glycoside from fresh leaves of Psidium guajava L / 药学学报

To investigate the chemical constituents of Psidium Guajava L, the EtOH/H2O extract of the fresh leaves was subjected to various chromatography. Five constituents with galloyl moiety were isolated and elucidated as 1-O-(1, 2-propanediol)-6-O-galloyl-beta-D-glucopyranoside (1), gallic acid (2), ellagic acid (3), ellagic acid-4-O-beta-D-glucopyranoside (4) and quercetin-3-O-(6"-galloyl) beta-D-galactopyranoside (5) by spectroscopic methods, including 2D NMR and HR-ESI-MS spectrometry as well as by comparison with published data. Compounds 4 and 5 were obtained from P. guajava for the first time, and compound 1 is a new polyhydroxyl compound.

Studies on alkalodial constituents in leaves of Uncaria hirsuta / 中国中药杂志

<p><b>OBJECTIVE</b>To study the alkaloidial constituents of the leaves of uncaria hirsuta.</p><p><b>METHOD</b>Some chromatographic methods were applied to isolate pure compounds and their structures were elucidated by spectroscopic methods.</p><p><b>RESULT</b>Eleven compounds were isolated and identified as 19-epi-3-iso-ajmalicine (1), 3-isoajmalicine (2), harman (3), mitraphylline (4), isomitraphylline (5), isorhynchophylline (6), corynoxine (7), rhynchophylline (8), isomitraphyllic acid (9), uncarine A (10) and uncarine B (11).</p><p><b>CONCLUSION</b>Compounds 1-9 were firstly isolated from this plant.</p>

Determination of beta-eudesmol in rhizome of Atractylodes lancea by RP-HPLC / 中国中药杂志

<p><b>OBJECTIVE</b>To develop a RP-HPLC method for determination of beta-eudesmol in rhizome of Atractylodes lancea, and to provide valuble data for quality control of A. lancea.</p><p><b>METHOD</b>The samples were separated on an Inertsil ODS-3 (4.6 mm x 250 mm, 5 microm) column with the mobile phase of acetonitrile-water (68:32). Flow rate was 1.0 mL x min(-1). The detection wavelength was set at 200 nm. Column temperature was 25 degrees C.</p><p><b>RESULT</b>The contents of beta-eudesmol determinated was 0.833-4.466 mg x g(-1), The linear range of beta-eudesmol was 0.048-1.200 microg (r = 0.999 9), the average recovery was 99.3%, RSD was 1.4% (n = 9).</p><p><b>CONCLUSION</b>The method for quantitation of beta-eudesmol in A. lancea was accurate and reliable, which can be used to evaluate the quality of rhizome of A. lancea.</p>

HPLC determination of acteoside in Radix Rehmanniae / 中国中药杂志

<p><b>OBJECTIVE</b>To develop an HPLC method for the determination of acteoside in Radix Rehmanniae.</p><p><b>METHOD</b>The chromatographic conditions were as follows: Polaris C18(4.6 mm x 250 mm, 5 microm) column, a mobile phase in gradient mode composed of acetonitrile 0.1% acetic acid solution, a flow rate of 1.0 mL x min(-1), and 334 nm as the detection wavelength.</p><p><b>RESULT</b>Acteoside showed good linear relationship at the range of 10-500 microg x mL(-1) (r = 0.9990). The average recovery was 100.1%, RS D 3.7%.</p><p><b>CONCLUSION</b>The proposed method promised to be applicable for the quality control of Radix Rehmanniae.</p>

Evaluation of antioxidant activity of Radix Linderae and other two Chinese drugs using TLC-bioautography / 药学学报

<p><b>AIM</b>To evaluate the antioxidant capacity and quality of traditional Chinese medicines using TLC-bioautography.</p><p><b>METHODS</b>Two chromatograms of each crude drug sample were obtained, after developing, by spraying with 1,1-diphenyl-2-picrylhydrazyl (DPPH) solution in ethanol and classical stained reagents, separately. The images sprayed with DPPH solution were captured under light after the plates were heated at 40 degrees C for 30 min, and scanned using video scan software to get peak areas of active compounds.</p><p><b>RESULTS</b>Total peak areas of the spots on TLC were calculated to evaluate the antioxidant capacity of the tested crude drugs from different habitats and sources. The results indicated that Radix Linderae cultivated in Tiantai (Zhejiang province), Cortex Magnoliae Officinalis cultivated in Liangshan (Sichuan province), and Fructus Perillae acquired in Shanghai have the highest scavenging properties towards DPPH in their respective TLC-autographic assays. Norisoboldine, magnolol and honokiol, luteolin, apigenin and an unknown compound "U" proved to be the major antioxidant components in the corresponding crude drugs as they contribute the dominating peak areas to the total ones.</p><p><b>CONCLUSION</b>TLC-bioautography can not only be used for screening of the components with antioxidant potency but also for the purpose of quality evaluation of traditional Chinese medicines at the same time, and the method proved to be selective, simple and reproducible.</p>

A study on quality standard for Herba Siegesbeckidae / 中国中药杂志

<p><b>OBJECTIVE</b>To establish the qualitative and quantitative methods of Herba Siegesbeckiae.</p><p><b>METHOD</b>A TLC method was used for qualitative identification and a HPLC analysis was applied for quantitative determination of Herba Siegesbeckiae with kirenol as the reference substances.</p><p><b>RESULT</b>Chloroform-methanol-formic acid (25:5:1) as a mobile phase of TLC, the spot of kirenol can be easily detected; Methanol extracts of Herba Siegebeckiae were separated on a Polaris C18 column with acetonitrile-water (25:75) as mobile phase and kirenol was separated well. The average content of kirenol in Herba Siegebeckiae was 0.14%. A good linear relationship between the peak areas and injected amounts of kirenol in the range of 0.19-14.9 microg and the average recovery was 100.0% (RSD = 2.4%).</p><p><b>CONCLUSION</b>The method can be used for qualitative identification and quantitation determination of Herba Siegesbeckiae.</p>

Determination of linderane in root tuber of Lindera aggregata by HPLC / 中国中药杂志

<p><b>OBJECTIVE</b>To provide scientific basis for quality control of Lindera aggregata.</p><p><b>METHOD</b>HPLC analytical method was established using a Lichrospher C18 column and acetonitrile-water (56:44) as the mobile phase, detected at 235 nm.</p><p><b>RESULT</b>The linear range of linderane is between 0.0642 - 0.5774 microg, the average recovery was 98.4%, RSD1.7% (n = 9).</p><p><b>CONCLUSION</b>Contents of linderane in commercially available and collected samples were from 0.028% to 0.123% and from 0.056% to 0.222% respectively.</p>

Quality evaluation of prepared slices of Paeonia lactiflon--determination of paeoniflorin by HPLC / 中国中药杂志

<p><b>OBJECTIVE</b>To establish the quality criteria of the prepared slices of Paeonia lactiflon.</p><p><b>METHOD</b>RP-HPLC was used for the determination of paeoniflorin in 10 lots of samples by ultrasound-assisted extraction.</p><p><b>RESULT</b>The samples were extracted with 50% methanol. Seperation of the solution was performed on an ODS column with a mobile phase of acetonitrile-water (18:82), detected at 230 nm.</p><p><b>CONCLUSION</b>The method is simple, repeatable, accurate and applicable.</p>

Phenolic compounds isolated from rhizoma of Aster tataricus / 中国中药杂志

<p><b>OBJECTIVE</b>To study the chemical constituents in root and rhizome of Aster tataricus.</p><p><b>METHODS</b>Compounds were isolated and purified by silica gel and sephadex LH-20 column chromatography. Their structures were identified by physicochemical properties and spectral analysis.</p><p><b>RESULT</b>Nine compounds were isolated and identified as quercetin (I), kaemferol (II), emodin (III), chrysophanol (IV), physcion (V), benzoic acid (VI), p-hydroxy-bezoic acid (VII), E-caffeic acid (VIII), E-ferulic acid hexacosyl ester (IX).</p><p><b>CONCLUSION</b>Compounds IV, V, VI, VII, VIII, IX were isolated from A. tataricus for the first time.</p>

Determination of shionone in Radix Asteris by HPLC / 中国中药杂志

<p><b>OBJECTIVE</b>To determine the content of shionone in Radix Aster from several different locations and markets.</p><p><b>METHOD</b>The HPLC analysis was used to determine shionone directly, using Polaris C18 column and acetonitrile as the mobile phase with a flow rate of 1.0 mL.min-1, and the UV detection wavelength was 200 nm.</p><p><b>RESULT AND CONCLUSION</b>The content of shionone was from 0.06% to 0.18%, depending on different locations and markets.</p>