1.Chemical constituents from Rehmannia glutinosa.
Xingnuo LI ; Mengyu ZHOU ; Peiqiang SHEN ; Jianbing ZHANG ; Chu CHU ; Zhiwei GE ; Jizhong YAN
China Journal of Chinese Materia Medica 2011;36(22):3125-3129
OBJECTIVETo study the chemical constituents from the roots of Rehmannia glutinosa.
METHODThe compounds were isolated by various chromatographic methods and identified by spectroscopic analysis.
RESULTTwelve compounds were isolated and their structures were identified as 5-hydroxymethyl-pyrrole-2-carbaldehyde (1), 5-hydroxymethyl furfural (2), tyrosol (3), 5,6-dihydroxy-beta-ionone (4), 6-O-E-feruloyl ajugol (5), acteoside (6), leucosceptoside A (7), martynoside (8), isomartynoside (9), purpureaside C (10), jionoside A1 (11), and jionoside B1 (12).
CONCLUSIONCompounds 1, 3 and 9 were isolated from the genus Rehmannia for the first time.
Glycosides ; analysis ; Rehmannia ; chemistry
2.Determination of two stilbene glycoside in five processed products of Rheum palamatum.
Li LI ; Cun ZHANG ; Yongqing XIAO ; Dongdong CHEN ; Guofang TIAN ; Yun WANG
China Journal of Chinese Materia Medica 2010;35(11):1415-1417
OBJECTIVETo compare of the contents of two stilbene glycoside in five processed products of Rheum palamatum.
METHODThe contents of trans-3, 5, 4'-trihydroxystilbene-4'-O-beta-D-glucopyranoside (a) and trans-3, 5, 4'-trihydroxystilbene-4'-Obeta-D-(6"-O-galloyl)-glucopyranoside (b) were determined by HPLC analysis at 35 degrees C with methanol-1% acetic acid as mobile phase, the wavelengths were set at 280, 300 nm, the flow rate was 1.0 mL x min(-1).
RESULTThe two components could be detected in five processed products, and their contents were more close in the no-parched pieces, the vinegar roasts pieces and the wine roast pieces. However, the contents reduced significantly in other two kinds of pieces which were lower than 80 percent of no-parched pieces.
CONCLUSIONHigh temperature may result in a significant reduction on glycoside in the pieces of rhubarb, and we have received similar results from determination of other glycoside compounds. Further analysis and comparison with the content of their corresponding aglycones, can provide a scientific basis to explain the variation of the material basis in the processed products of rhubarb.
Glycosides ; analysis ; Plant Extracts ; analysis ; Rheum ; chemistry ; Stilbenes ; analysis
3.Simultaneous determination of five constituents in Scrophularia ningpoensis by HPLC.
Xuemei ZHANG ; Rui WANG ; Rui AN ; Ximin WU ; Xinhong WANG ; Yiming LI
China Journal of Chinese Materia Medica 2011;36(6):709-711
OBJECTIVETo develop an HPLC method for the simultaneous quantitation of five constituents in Scrophularia ningpoensis.
METHODSamples were analyzed on an Agilent SB-C18 column(4.6 mm x 250 mm, 5 microm) eluted with acetonitrile and water containing 0.03% phosphate acid as mobile phases in a linear gradient mode. The flow rate was kept at 1.0 mL x min(-1), and the column temperature was set to 30 degrees C. The DAD detector wavelengths were 210, 280, 330 nm.
RESULTThe linear ranges were 50-400 mg x L(-1) for harpagide, 1-40 mg x L(-1) for harpagoside, 1-20 mg x L(-1) for cinnamic acid, 0.5-4.5 mg x L(-1) for acteoside,1-60 mg x L(-1) for angoroside C, respectively. The average recoveries of the five constituents were 100.8% (RSD 0.62%), 101.7% (RSD 0.32%), 98.8% (RSD 0.48%), 99.9% (RSD 1.4%), 99.2% (RSD 1.1%), respectively.
CONCLUSIONThrough the validation, the method was proved to be sensitive, accurate, repeatable, and can be used for quality control of the roots of S. ningpoensis.
Chromatography, High Pressure Liquid ; methods ; Cinnamates ; analysis ; Coumaric Acids ; analysis ; Glucosides ; analysis ; Glycosides ; analysis ; Iridoid Glycosides ; Phenols ; analysis ; Pyrans ; analysis ; Scrophularia ; chemistry ; Trisaccharides ; analysis
4.Determination of tenacissoside H in Marsdeniae tenacissimae by HPLC-ELSD.
Huali LI ; Yan LU ; Jiayun HU ; Daofeng CHEN
China Journal of Chinese Materia Medica 2010;35(16):2083-2086
In order to improve the quality standard of Marsdenia tenacissima, a quantitative determination method of tenacissoside H was developed using high performance liquid chromatography. The method was carried out on a YMC ODS-H80 (4.6 mm x 250 mm, 4 microm) column eluted with a mixture of acetonitrile and water (50:50) as the mobile phase. The flow rate was 0.8 mL x min(-1) and the column temperature was 35 degrees C. An evaporative light scattering detector (ELSD) was used with the temperature of drift tube set at 60 degrees C and the gas flow rate of nitrogen set at 1.5 mL x min(-1). The calibration curve was linear in the range from 0.5625 to 36.00 microg (r = 0.9998). The average recovery and RSD were 99.41% and 1.8%, respectively. The contents of tenacissoside H in the 11 samples from different habitats varied from 0.201% to 0.862%. The method established in this paper is specific and reliable to control and evaluate the quality of M. tenacissima.
Chromatography, High Pressure Liquid
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Glycosides
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analysis
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Marsdenia
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chemistry
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Reproducibility of Results
5.Determination of tortoside A in Ilicis pubescentis by RP-HPLC.
Shuli LI ; Yuan ZHOU ; Pengfei TU
China Journal of Chinese Materia Medica 2011;36(22):3146-3148
OBJECTIVETo establish a RP-HPLC method for the determination of tortoside A in Ilex pubences.
METHODKromasil-C18 (4.6 mm x 250 mm, 5 microm) column was used in HPLC with mobile phase acetonitrite-0.1% H3PO4 (17:83), the column temperature was 30 degrees C, the flow rate was 1 mL x min(-1), the detection wavelength was set at 210 nm, and inject volume was 10 microL RESULT: Tortoside A was well separated under the established conditions, the liner range of tortoside A was 26.05-521.00 microg (r = 0.999 9, n = 6), and the average recovery was 98.42%.
CONCLUSIONIt was the first time to establish the RP-HPLC method with accuracy, good reproducibility for determining the content of tortoside A in I. Pubescentis.
Chromatography, High Pressure Liquid ; methods ; Glycosides ; analysis ; Ilex ; chemistry
6.Fingerprint analysis of Zhimu-Huangbai herb pair and simultaneous determination of its alkaloids, xanthone glycosides and steroidal saponins by HPLC-DAD-ELSD.
Feng ZHANG ; Qi YANG ; Lian-Na SUN ; Shou-Hong GAO ; Xia TAO ; Wan-Sheng CHEN
Chinese Journal of Natural Medicines (English Ed.) 2014;12(7):525-534
AIM:
To develop and validate a high performance liquid chromatography (HPLC) coupled with diode array and evaporative light scattering detectors (DAD-ELSD) method for the quantitative determination and fingerprint analysis of ten active constituents in three chemical classes (namely, xanthone glycosides, steroidal saponins, and alkaloids) in Zhimu-Huangbai herb pair (ZB).
METHOD:
Chromatographic separation was performed on a Diamonsil C18 column (4.6 mm × 250 mm, 5 μm, Dikma) by gradient elution using acetic acid in acetonitrile solution at a flow rate of 1.0 mL·min(-1) at 260 nm. The drift tube temperature of ELSD was set to 60 °C and nebulizer gas pressure was 4.0 Bar. Method validation was performed to assure its linearity, limits of detection and quantification, precision, repeatability, stability, and accuracy.
RESULTS:
The HPLC-DAD-ELSD method allowed the quantification of ten compounds (phellodendrine, jatrorrhizine, palmatine, berberine, neomangiferin, mangiferin, timosaponin E-I, timosaponin B-II, timosaponin B, and timosaponin A-III), and was successfully applied to fingerprint analysis for ten batches of ZB samples.
CONCLUSION
This was the first time to apply the combination of DAD and ELSD for the simultaneous determination of ten active ingredients in ZB. The results showed that the combination of quantitative analysis for marker ingredients and chemical fingerprint for the TCM herb pair provides a potentially powerful, widely introduced, and internationally accepted strategy for assessment of complex TCM formulas.
Alkaloids
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analysis
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Chromatography, High Pressure Liquid
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instrumentation
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methods
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Drugs, Chinese Herbal
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analysis
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Glycosides
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analysis
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Xanthones
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analysis
7.Further chemical investigation of leaves of Aquilaria Sinensis.
Fang XIA ; Jian SUN ; Yong JIANG ; Peng-Fei TU
China Journal of Chinese Materia Medica 2013;38(19):3299-3303
To comprehensively utilize the rich resource of Aquilaria sinensis,the ethanol extract of the leaves of A. sinensis was further chemically investigated, which led to the isolation of 12 compounds. By means of 'H- , "C-NMR, and ESI-MS data, and through comparison with those reported in literatures,their structures were identified as iriflophenone 2-(O-a-L)-rhamnoside(1) ,4'-hydroxy-5 methoxyflavone-7-O-glucoxyloside (2) ,7,3',5'-tri-O-methyltricetin(3) ,7-O-beta-D-glucopyranoside of 5-O-methylapigenin(4) ,2-phenyl-ethyl-D-glucopyranoside( 5), salidroside, (6) , benzyl alcohol O-beta-D-glucopyranoside (7) , 2, 6-dimethoxy-4-hydroxyphenol-1-O-beta-D-glucopyranoside(8) ,vanilloloside(9) , ( + ) -syringaresinol( 10) ,beta-tocopherol( 11) and stigmast-5-ene-3beta,7alpha-diol( 12). Among them, compounds 2,3,5-9,11 and 12 were isolated from this genus for the first time. This research hopefully provides valuable data for the further utilization and development of the leaves of A. sinensis.
Glucosides
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analysis
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Glycosides
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analysis
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Phenols
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analysis
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Plant Extracts
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chemistry
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Plant Leaves
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chemistry
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Saponins
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analysis
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Thymelaeaceae
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chemistry
8.Study on superposition law of drug bitterness based on tongue taste evaluation and electronic tongue evaluation.
Xue-Lin LI ; Yao ZHANG ; Peng-Ju CHEN ; Jun-Han SHI ; Jing YAO ; Qing-Xiao WANG ; Xin-Jing GUI ; Lu ZHANG ; Ke-Han WANG ; Jing MA ; Yan-Li WANG ; Rui-Xin LIU
China Journal of Chinese Materia Medica 2019;44(23):5134-5142
Traditional Chinese medicine( TCM) decoction contains complex bitterness. In this paper,the simple mixing of TCM monomer bitter substances is used as the entry point to study the law of bitterness superposition. With berberine hydrochloride( alkaloids),geniposide( terpenoids),and arbutin( glycosides) as mother liquor,sophoridine( alkaloids),gentiopicroside( terpenoids),and puerarin( glycosides) as additive substances,these different additive substances were mixed with different mother liquor according to concentration gradients to form different liquid mixtures. The bitterness of the additive solution and the mixtures was evaluated by traditional human taste panel method( THTPM) and electronic tongue; the bitterness-concentration fitting model of the additive solution and the liquid mixtures was established by Weibull and logarithmic curves. By comparing and analyzing the bitterness-concentration model and the bitterness difference( ΔI_0/ΔI_e) of the additive solution and the mixture,the influence of mother liquor on the bitterness of the mixture was investigated. The results showed that both the additive solution bitterness model and the liquid mixture bitterness model were consistent with the Weibull model and the logarithmic model( THTPM: R~2≥0. 887 0,P<0. 01; electronic tongue test:R~2≥0. 753 2,P<0. 05). The fitting degree of the Weibull model was generally higher than that of the logarithmic model; the bitterness difference( ΔI_0) was monotonously decreasing; the fitting equation of tongue bitterness and electronic tongue bitterness: R~2≥0. 874 2,P<0. 01. In this article,through the superposition of different kinds of TCM bitter substances,THTPM and electronic tongue test was combined. It was found that the bitterness after superposition was still in Weibull or logarithmic relationship with the concentration of additive substances; THTPM showed that the effect of bitter mother liquor on the bitterness of the mixture decreased with the increase of the concentration of the additive; the bitterness of the electronic tongue was obviously related to the bitterness of THTPM. However,further verification is needed later by optimizing the concentration gradient and expanding the sample size.
Alkaloids/analysis*
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Electronic Nose
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Glycosides/analysis*
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Humans
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Medicine, Chinese Traditional
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Taste
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Terpenes/analysis*
9.UPLC and HPLC analysis on contents of astilbin and engeletin in dong medicine "sunl gaems" of Guizhou origin by QAMS.
Hong-zhi DU ; Xi-cheng HE ; Heng NONG ; Li-sha DONG ; Hu-biao CHEN ; Juan CAI ; Ming LI
China Journal of Chinese Materia Medica 2015;40(15):3115-3120
This study aimed to simultaneously determine the contents of astilbin and engeletin in dong medicine "sunl gaems" of Guizhou origin by quantitative analysis of multi-components by single marker (QAMS), with astilbin as the internal standard substance. On UPLC and HPLC chromatograms, different models of instruments were used to investigate relative correction factors (RCF), in order to discuss the interoperability of RCFs established in different chromatographic systems. The engeletin content was calculated based on the established RCFs and compared by the one point external standard method and the external standard working curve method, in order to verify the accuracy of QAMS. According to the result, in different chromatograms, the ratios between RCF and retention time of engeletin and astilbin had a good reproducibility, with RSD between 2.0% and 1.8%, both were less than 3%. The relative differences among results of QAMS, the external standard working curve method of dong medicine "sunl gaems" ranged between 1.6% and 3.9%, with RSD between 2.02%-0.80% in line with relevant requirements and Pearson correlation coefficient at 0.9998 (P <0.01). The findings showed that QAMS was an accurate, reliable and highly reproducible method to determine the contents of astilbin and engeletin in dong medicine "sunl gaems" of Guizhou origin and so could be used to control the inherent quality of the herb.
Chromatography, High Pressure Liquid
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methods
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Drugs, Chinese Herbal
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analysis
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Flavonols
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analysis
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Glycosides
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analysis
10.A new antioxidant flavonoid glycoside from flowers of Hosta plantaginea.
Qing-Guang ZHOU ; Li YANG ; Jun-Wei HE ; Guo-Yue ZHONG
China Journal of Chinese Materia Medica 2019;44(15):3312-3315
Phytochemical investigation of the flowers of Hosta plantaginea led to isolate of one new flavonoid glycoside,plantanone C( 1) by silica gel,Sephadex LH-20,and RP-HPLC column chromatographies. Its structure was extensively determined on basis of HR-ESI-MS and NMR spectroscopic data. Compound 1 exhibited moderate antioxidant activity against DPPH radical scavenging activity,with an IC50 value of 240. 2 μmol·L~(-1).
Antioxidants
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analysis
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isolation & purification
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Flavonoids
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analysis
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isolation & purification
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Flowers
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chemistry
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Glycosides
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analysis
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isolation & purification
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Hosta
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chemistry