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.
China ; Drugs, Chinese Herbal ; chemistry ; pharmacology ; standards ; Humans ; Medicine, Tibetan Traditional ; standards ; Plants, Medicinal ; chemistry ; Quality Control

OBJECTIVETo study the alkaloidial constituents of the leaves of uncaria hirsuta.

METHODSome chromatographic methods were applied to isolate pure compounds and their structures were elucidated by spectroscopic methods.

RESULTEleven 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).

CONCLUSIONCompounds 1-9 were firstly isolated from this plant.

Alkaloids ; chemistry ; Drugs, Chinese Herbal ; chemistry ; Plant Leaves ; chemistry ; Uncaria ; chemistry

OBJECTIVETo establish the qualitative and quantitative methods of Herba Siegesbeckiae.

METHODA 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.

RESULTChloroform-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%).

CONCLUSIONThe method can be used for qualitative identification and quantitation determination of Herba Siegesbeckiae.

Asteraceae ; chemistry ; Drugs, Chinese Herbal ; analysis ; Pharmacognosy ; standards ; Plants, Medicinal ; chemistry ; Quality Control

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.
Chromatography, High Pressure Liquid ; Chromatography, Thin Layer ; Drugs, Chinese Herbal ; chemistry ; isolation & purification ; standards ; Flavonoids ; chemistry ; isolation & purification ; standards ; Glycosides ; chemistry ; isolation & purification ; standards ; Lamiaceae ; chemistry ; Magnetic Resonance Spectroscopy ; Quality Control

OBJECTIVETo develop an HPLC method for the determination of acteoside in Radix Rehmanniae.

METHODThe 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.

RESULTActeoside 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%.

CONCLUSIONThe proposed method promised to be applicable for the quality control of Radix Rehmanniae.

Chromatography, High Pressure Liquid ; methods ; Glucosides ; analysis ; Phenols ; analysis ; Plant Roots ; chemistry ; Plants, Medicinal ; chemistry ; Quality Control ; Rehmannia ; chemistry ; Reproducibility of Results ; Sensitivity and Specificity

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.
Biotransformation ; Chalcones ; chemistry ; isolation & purification ; metabolism ; Glucosides ; chemistry ; isolation & purification ; Glycosylation ; Magnetic Resonance Spectroscopy ; Molecular Structure ; Mucor ; metabolism ; Spectrometry, Mass, Electrospray Ionization

OBJECTIVETo 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.

METHODThe 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.

RESULTThe 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).

CONCLUSIONThe 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.

Atractylodes ; chemistry ; Chromatography, High Pressure Liquid ; methods ; Plants, Medicinal ; chemistry ; Quality Control ; Reproducibility of Results ; Rhizome ; chemistry ; Sesquiterpenes, Eudesmane ; analysis ; standards

OBJECTIVETo study the chemical constituents in root and rhizome of Aster tataricus.

METHODSCompounds were isolated and purified by silica gel and sephadex LH-20 column chromatography. Their structures were identified by physicochemical properties and spectral analysis.

RESULTNine 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).

CONCLUSIONCompounds IV, V, VI, VII, VIII, IX were isolated from A. tataricus for the first time.

Anthraquinones ; chemistry ; isolation & purification ; Aster Plant ; chemistry ; Benzoic Acid ; chemistry ; isolation & purification ; Emodin ; analogs & derivatives ; chemistry ; isolation & purification ; Plants, Medicinal ; chemistry ; Rhizome ; chemistry

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.
Cirsium ; chemistry ; Flavonoids ; chemistry ; Glycosides ; chemistry ; Molecular Conformation ; Molecular Structure ; Plant Components, Aerial ; chemistry ; Plants, Medicinal ; chemistry ; Quercetin ; chemistry ; isolation & purification

AIM To establish an HPLC method for the simultaneous content determination of neochlorogenic acid,cryptochlorogenic acid,chlorogenic acid,caffeic acid,isochlorogenic acid B,isochlorogenic acid A and isochlorogenic acid C in the leaves of Artemisia argyi Levl.et Vant..METHODS The analysis of 50％ methanol extract of A.argyi leaves was performed on a 30 ℃ Prevail C1s column (4.6 mm ×250 mm,5 μmn),with the mobile phase comprising of acetonitrile-water flowing at 1.0 rnL/min in a gradient elution manner,and the detection wavelength was set at 325 nm.RESULTS Seven constituents showed good linear relationships within their own ranges (r ≥ 0.999 5),whose average recoveries were 98.28％-101.11％ with the RSDs of 1.04％-2.59％.CONCLUSION This simple,accurate and reproducible method can be used for the quality control of A.argyi leaves.