Polygonflavanol B(1), a new flavonostilbene glycoside, was isolated from the roots of Polygonum multiforum(Polygonaceae) by various column chromatography methods including macroporous resin HP-20, silica gel, Sephadex LH-20, and preparative HPLC. The structure with absolute configuration of the new compound was identified by its physicochemical properties, spectroscopic data, ECD calculation, and chemical method.
Fallopia multiflora/chemistry* ; Flavonols/isolation & purification* ; Glycosides/isolation & purification* ; Plant Roots/chemistry* ; Stilbenes/isolation & purification*

AIMTo study the chemical constituents of Dryopteris sublaeta Ching et Hsu.

METHODSFresh plant of Dryopteris sublaeta ching et hsu was extracted twice with boiling water, concentrated to small volume under reduced pressure at 50 degrees C. The concentrated material was partitioned with ether, ethyl acetate, and n-butanol. The fraction of ethyl acetate extract was chromatographed over macroporous adsorption resin (Diaion HP-20) eluted with a mixture of H2O and MeOH in increasing MeOH content. Their fractions from resin were repeatedly chromatographed over Toyopearl HW-40, Sephadex LH-20 and silica gel column chromatography. The compounds were identified on the basis of their physiochemical and spectral data.

RESULTSFour compounds were obtained and identified as 3,5-dihydroxy-stilbene-3-O-neohesperidoside (1), 3,5-dihydroxy-stilbene-3-O-beta-D-glucoside (2), polydotin peceid (3) and 3,5,4'-trihydroxy-bibenzyl-3-O-beta-D-glucoside (4).

CONCLUSIONCompound 1 is a new compound, the others were isolated from Dryopteris for the first time.

Dryopteris ; chemistry ; Glycosides ; chemistry ; isolation & purification ; Molecular Structure ; Plants, Medicinal ; chemistry ; Stilbenes ; chemistry ; isolation & purification

AIMTo study the chemical constituents of the stem of Cassia siamea.

METHODSThe compounds were isolated by chromatography on silica gel, and identified on the basis of spectral analysis.

RESULTSFive compounds were isolated and identified as: beta-sitosterol (I), sucrose (II), n-octacosanol (III), 2-methyl-5-(2'-hydroxypropyl)-7-hydroxy-chromone-2'-O-beta-D-glucopyranoside (IV) and piceatannol (V).

CONCLUSIONCompound IV is a new compound. Compounds II, III and V were obtained from this plant for the first time.

Cassia ; chemistry ; Chromones ; chemistry ; isolation & purification ; Fatty Alcohols ; chemistry ; isolation & purification ; Monosaccharides ; chemistry ; isolation & purification ; Plant Stems ; chemistry ; Plants, Medicinal ; chemistry ; Stilbenes ; chemistry ; isolation & purification

The investigation on the stem bark of Morus wittiorum was carried out to find its chemical constituents possessing anti-oxidative activity. The isolation and purification were performed by various chromatographies such as silica gel, Sephadex LH-20, RP-C18 column chromatography and so on. Based on the spectral analysis such as NMR, MS, etc., seven 2-arylbenzofuran derivatives were identified as wittifuran D (1), wittifuran E (2), moracin C (3), moracin M (4), moracin P (5), 2-(3,5-dihydroxyphenyl)-5,6-dihydroxybenzofuran (6) and mulberroside C (7). Compounds 1-7 were isolated from this plant for the first time. Among them, 1 and 2 were new compounds. Compounds 3-7 were used to assay antioxidant activity, the inhibitory ratios of compounds 3, 4, 6, at a concentration of 1 x 10(-5) mol x L(-1), to malondialdehyde (MDA) produced during microsomal lipid peroxidation induced by ferrous-cysteine were 73%, 69% and 89% respectively.
Antioxidants ; isolation & purification ; pharmacology ; Benzofurans ; chemistry ; isolation & purification ; pharmacology ; Lipid Peroxidation ; Malondialdehyde ; chemistry ; Molecular Structure ; Morus ; chemistry ; Plant Bark ; chemistry ; Plants, Medicinal ; chemistry ; Stilbenes ; chemistry ; isolation & purification ; pharmacology

A reasonable and practicable quality standard was developed for mori liquid extract from different sources by TLC, HPLC and fingerprint technology. In TLC method, the compounds were separated on polyamide film using glacial acetic acid-water (1: 3) as mobile phase at a UV wavelength of 365 nm. All qualified samples had the spots of the same color as the control herb and substance. The RP-HPLC method was used to determine the content of mulberroside A with mobile phase of methanol-water (25: 75) at a wave-length of 326 nm. The mulberroside A was in good linear with a regression equation of Y = 46.965X (r = 0.999 6) in the range of 4.6 - 228 mg x L(-1). In 14 batches of samples, the mulberroside A in 4 batches of them was less than 0.5 g x L(-1), and was more than 2.0 g x L(-1) in the other batches. It was suggested that the content limit of mulberroside A should be no less than 1.5 g x L(-1). The HPLC fingerprints were evaluated by the similarities. It has found that the similarities of different mori liquid extracts were very low and the chemical diversity of mori cortex was the major factor of similarity. Moreover, the process impact was minimal. Thus the fingerprint was not included in this quality standard.
China ; Chromatography, High Pressure Liquid ; Disaccharides ; chemistry ; isolation & purification ; Drugs, Chinese Herbal ; chemistry ; isolation & purification ; standards ; Morus ; chemistry ; Quality Control ; Stilbenes ; chemistry ; isolation & purification

OBJECTIVETo study the conditions and parameters of purifying 2,3,5,4'-tetrahydroxy-stilbene-2-O-beta-D-glycoside from Polygonum multiflori.

METHODAbsorption capacity of four resins for 2,3,5,4'-tetrahydroxy-stilbene-2-O-beta-D-glycoside was compared. With the adsorption ability as indexes, the process of absorbing and purifying 2,3,5,4'-tetrahydroxy-stilbene-2-O-beta-D-glycoside from P. multiflori with S-8 macroporous resin absorbent was selected by orthogonal design.

RESULTThe S-8 resin was the best of the four resins. The optimum process condition was 50% ethanol as eluting solvent, the flow rate at 1.5 mL x min(-1), pH at 7-8, and the solution concentration at 0.2 g x mL(-1). The absorption capacity by this process was 36.89 mg x g(-1).

CONCLUSIONThe process is simple and convenient and the regeneration of resin is easy, so this method of purification is advisable.

Absorption ; Glycosides ; chemistry ; isolation & purification ; Plant Extracts ; chemistry ; isolation & purification ; Plants, Medicinal ; chemistry ; Polygonum ; chemistry ; Resins, Synthetic ; chemistry ; Stilbenes ; chemistry ; isolation & purification

OBJECTIVETo study the technological parameters of the purification process for effective part from Polygonum cuspidatum.

METHODUsing adsorption capacities and desorption rates of polydatin, resveratrol,emodin,physcion and total anthraquinone as the primary screening indexes, six resins were surveyed,and the optimized conditions of adsorption and desorption of the effective ingredients were studied.

RESULTResin D101 gave good separation performance and was selected to purify the effective part in Polygonum cuspidatum. The optimum parameters were established as the following: 1 BV (bed volume) sample extract was passed through the column with a flow rate of 2.4 BV x h(-1), 30 min later,the column was washed with 2 BV water, 2 BV 20% ethanol, 5 BV 50% ethanol, 2 BV 70% ethanol and 5 BV 95% ethanol, respectively. The combined 50% and 95% ethanolic elutes were concentrated to yield the purified effctive part.

CONCLUSIONThe purity of the total effective ingredients in the product was up to 36. 87%. Macroporous resin D101 could be well used in separating and purifying the effective part from Polygonum cuspidatum.

Adsorption ; Anthraquinones ; chemistry ; isolation & purification ; Drugs, Chinese Herbal ; chemistry ; isolation & purification ; Emodin ; analogs & derivatives ; isolation & purification ; Fallopia japonica ; chemistry ; Glucosides ; isolation & purification ; Plants, Medicinal ; chemistry ; Resins, Synthetic ; chemistry ; Stilbenes ; isolation & purification ; Technology, Pharmaceutical ; methods ; Temperature

OBJECTIVETo optimize the ultrahigh pressure extraction (UPE) process of polydatin and resveratrol from Polygonum cuspidatum by using uniform design.

METHODOn the basis of single factor screening, the uniform design was adopted for getting the optimal technique parameters. The optimum result of UPE was compared with conventional extractions.

RESULTThe optimal conditions of UPE for polydatin and resveratrol were that the solvent was 55% ethanol, the ratio of solvent to material( mL: g) was 30, the extraction pressure was 170 MPa, and the extraction time was 120 second. With this extracting process, the extraction yield of polydatin and resveratrol were 14.29 and 2.53 mg x g(-1), respectively. The extraction yield of polydatin was 46.1% higher than the heat reflux extraction, 6.4% higher than the ultrasonic extraction and 28.5% higher than the microwave extraction, while the yield of resveratrol was 67.5% higher than the heat reflux extraction, 29.7% higher than the ultrasonic extraction and 24.6% higher than the microwave extraction, respectively.

CONCLUSIONAs a novel extraction technology for Chinese herbal medicine, the UPE procedure has higher extraction yield, lower extracting temperature, shorter extacting time and less power consumption. The UPE has provided a brand-new method for extraction of polydatin and resveratrol from P. cuspidatum.

Calibration ; Chemical Fractionation ; methods ; Fallopia japonica ; chemistry ; Glucosides ; analysis ; isolation & purification ; Pressure ; Reproducibility of Results ; Solvents ; chemistry ; Stilbenes ; analysis ; isolation & purification ; Time Factors

AIMTo study the metabolite of stilbene glucoside in the Chinese traditional medicine Polygonum multiflornm in mice and elucidate its chemical structure by liquid chromatography tandem-mass spectrometry.

METHODSThe stilbene glucoside was injected into the tail vein of mice. Blood samples were collected from artery in the eyepit. The methanol-protein-precipitated plasma sample was introduced into the liquid chromatography-tandem mass spectrometer directly. The analytical column was C18 column (250 mm x 4.6 mm ID, 5 microns). The mobile phase consisted of acetonitrile-methanol-water-formic acid (15:18:66:1) for ES+, acetonitrile-methanol-water (15:18:67) for ES-. The UV detection wavelength was set at 320 nm. The mass ion source type was ESI. HV capillary was 3 kV. The dry gas was nitrogen gas and the flow rate was set at 318 L.h-1. The ion source temperature was 150 degrees C.

RESULTSThe stilbene glucoside and its metabolite were separated completely under the chromatography condition. The ions at m/z 600 and m/z 605 were detected under positive ion polarity while the ions at m/z 581 and m/z 402 were detected under negative ion polarity.

CONCLUSIONIt was proposed that the metabolite of stilbene glucoside injected in vein was its glucuronide conjugate.

Animals ; Chromatography, Liquid ; methods ; Female ; Glucosides ; blood ; isolation & purification ; metabolism ; Male ; Mice ; Plants, Medicinal ; chemistry ; Polygonum ; chemistry ; Spectrometry, Mass, Electrospray Ionization ; methods ; Stilbenes ; blood ; chemistry ; isolation & purification ; metabolism

OBJECTIVETo optimize the extraction process of root of Polygoni multflori and validate the interrelation between antioxdative capacity and the content of 2,3,4,5-tetrahydroxystilbene-2-O-beta-D-glucoside in root of P. multiflori.

METHODThe optimum extraction was abserved with the orthogonal design; 2,3,4,5-tetrahydroxystilbene-2-O-beta-D-glucoside was determined by HPLC and the antioxidative capacity by using photochemiluminescence detection method with the Photochem supplied by Analytik Jena AG; the concentration of ethanol, amount of ethanol, extraction time and extraction times were the four factors in the extraction.

RESULTThe concentration of ethanol and extraction times had significant effect on the content of 2,3,4,5-tetrahydroxystilbene-2-O-beta-D-glucoside and the antioxidative capacity of the crude extract.

CONCLUSIONThe best extraction process is to extract three times by using 10 fold EtOH(60%), refluxing at 85 degrees C and to extract one and half hours each time.

Antioxidants ; isolation & purification ; pharmacology ; Chromatography, High Pressure Liquid ; Drugs, Chinese Herbal ; isolation & purification ; pharmacology ; Ethanol ; Glucosides ; analysis ; isolation & purification ; Plant Roots ; chemistry ; Plants, Medicinal ; chemistry ; Polygonum ; chemistry ; Stilbenes ; analysis ; isolation & purification ; Technology, Pharmaceutical ; methods ; Time Factors