1.Study on HPLC fingerprints of Senecio scandens and S. scandens.
Xuejing YANG ; Aizhen XIONG ; Li YANG ; Changhong WANG ; Zhengtao WANG
China Journal of Chinese Materia Medica 2011;36(6):725-728
OBJECTIVETo develop an HPLC method for fingerprint study of both Senecio scandens and S. scandens.
METHODFingerprints of the two Senecio herbs were compared. And the concentrations of main peaks in them were semi-quantified as chlorogenic acid or hyperoside. Chromatography was performed on a Shiseido Capcell Pak MG II C18 (4.6 mm x 250 mm, 5 microm) column using a gradient elution of acetonitrile-water containing 0.2% acetic acid. And detection wavelength was 360 nm.
RESULTSignificant difference was found in the fingerprint of the two herbs. Eleven peaks were picked out for the evaluation of S. scandens and S. scandens, respectively. They were identified to be either organic acid compounds or flavones by HPLC-UV and LC-ESI-MS analysis. And semi-quantification of them showed the concentrations of organic acid compounds and flavones in S. scandens were 2.29- and 15.56- folds of those in S. scandens, respectively.
CONCLUSIONThe developed HPLC method is suitable for the fingerprint study for both of S. scandens and S. scandens. It is robust and producible enough to be used for the quality evaluation on S. scandens.
Chlorogenic Acid ; analysis ; Chromatography, High Pressure Liquid ; methods ; Quercetin ; analogs & derivatives ; analysis ; Senecio ; chemistry
2.Degradation kinetics of chlorogenic acid, cryptochlorogenic acid, and neochlorogenic acid at neutral and alkaline pH values.
Peng ZHU ; Xiao-lei MIAO ; Yong CHEN
Acta Pharmaceutica Sinica 2016;51(1):122-126
The degradation kinetics of chlorogenic acid (5-CQA), cryptochlorogenic acid (4-CQA), and neochlorogenic acid (3-CQA) in aqueous solution at 37 degrees C and different pH values (7.05, 7.96, 9.25) were investigated in the present work. The results indicated that 3-, 4- and 5-CQA tended to remain stable in acidic pH circumstance, and unstable in neutral and alkaline pH circumstance. With the increase of the alkalinity, the degradation of 3-, 4- and 5-CQA was increased leading to a less amount of total CQA and was satisfactorily described by the Weibull equation. Meanwhile, caffeic acid was not detected after the degradation of CQA. Moreover, the degradation of 3-CQA and 5-CQA tended to be converted to 4-CQA, and the degradation of 4-CQA tended to be converted to 3-CQA rather than 5-CQA. The comparison of the degradation kinetics parameters of 3-, 4- and 5-CQA at neutral and alkaline pH values showed that the orders of the rate constant (k) values were 4-CQA > 3-CQA > 5-CQA, while the orders of the degradation half life (t½) values were 4-CQA < 3-CQA < 5-CQA, indicating the orders of the stabilities of 3-, 4- and 5-CQA at 37 degrees C and neutral and alkaline pH values were 4-CQA < 3-CQA < 5-CQA.
Caffeic Acids
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Chlorogenic Acid
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analogs & derivatives
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chemistry
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Hydrogen-Ion Concentration
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Kinetics
3.Establishment of HPLC fingerprint and comparison of active ingredients between varieties of chrysanthemum in Hubei province.
Yin LIU ; Wen-Ling GONG ; Wu-Zhou BAO ; Lan-Ping GUO ; Yang XU ; Yi-Mei LIU ; Da-Hui LIU
China Journal of Chinese Materia Medica 2019;44(17):3711-3717
In this paper,the fingerprint of different varieties of chrysanthemum were established with " Similarity Evaluation System for Chromatographic Fingerprint of Chinese Materia Medica" and the content of chlorogenic acid,galuteolin and 3,5-O-dicaffeoylquinic acid in 29 batches of different varieties of chrysanthemum in Futianhe town,Huangtugang town and Wuhan city were compared. At the same time,similarity evaluation and common peak clustering analysis were carried out. There were 11 common peaks in the fingerprints of 29 batches of different varieties of chrysanthemum,and the similarity ranged from 0. 802 to 0. 975. Hangju and Gongju were divided into one group by cluster analysis,and Huangju into another category. The established fingerprint method provides a basis for the identification of chrysanthemum cultivars. The content of 29 batches of chlorogenic acid was between 4. 092 and 11. 723 mg·g-1,luteolin was between 1. 010 and 11. 713 mg·g-1,and 3,5-O-dicaffeoylquinic acid was between 8. 828 and 33. 435 mg·g-1,both reach the pharmacopoeia standard,but the effective components of different varieties of chrysanthemum were quite different. Based on the contents of three active ingredients and the diversity of fingerprint peaks,the quality of the characteristic germplasm resource of local Fubaijuin Macheng is superior,and the protection of local characteristic germplasm resource should be strengthened in production.
Chlorogenic Acid
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analogs & derivatives
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analysis
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Chromatography, High Pressure Liquid
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Chrysanthemum
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chemistry
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Luteolin
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analysis
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Phytochemicals
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analysis
4.Chemical constitutents from pre-formulation of lonicerae japonicae flos in shuanghuanglian lyophilized powder for injection.
China Journal of Chinese Materia Medica 2011;36(12):1613-1619
OBJECTIVETo research the chemical constitutents for the pre-formulation of Lonicerae Japonicae Flos (the dried buds of Lonicera japonica) in Shuanghuanglian lyophilized powder for injection and provide substance foundation for the adverse reaction of Shuanghuanglian lyophilized powder for injection.
METHODThe chemical constituents were isolated by column chromatography and preparative HPLC. All structures were characterized by the spectroscopic methods including ESI-MS, 1H-NMR, 13C-NMR, and compared with data in the literature.
RESULTTwenty compounds were isolated and identified as sophoraricoside(1), luteolin-7-O-beta-D-glucopyranoside(2), rutin(3), quercetin(4), 3,5-O-dicaffeoyl quinic acid methyl ester(5), 4,5-O-dicaffeoyl quinic acid methyl ester(6), 3,4-O-dicaffeoyl quinic acid methyl ester(7), 4,5-dicaffeoyl quinic acid(8), 3,4-dicaffeoyl quinic acid(9), chlorogenic acid(10), epi-vogeloside (11), sweroside(12), vogeloside(13), secoxyloganin(14), macranthoidin A(15), macranthoidin B(16), loniceroside A(17), loniceroside B(18), loniceroside C(19), dipsacoside B(20).
CONCLUSIONCompound 1 was identified in genus Lonicera for the first time and compounds 1-20 were isolated from the pre-formulation for the first time.
Chlorogenic Acid ; chemistry ; Drugs, Chinese Herbal ; chemistry ; Flowers ; chemistry ; Freeze Drying ; Lonicera ; chemistry ; Oleanolic Acid ; analogs & derivatives ; chemistry ; Quinic Acid ; analogs & derivatives ; chemistry ; Rutin ; chemistry ; Saponins ; chemistry
5.Quantitative analysis of seven phenolic acids in eight Yinqiao Jiedu serial preparations by quantitative analysis of multi-components with single-marker.
Jun-jun WANG ; Li ZHANG ; Qing GUO ; Jun-ping KOU ; Bo-yang YU ; Dan-hua GU
Acta Pharmaceutica Sinica 2015;50(4):480-485
The study aims to develop a unified method to determine seven phenolic acids (neochlorogenic acid, chlorogenic acid, 4-caffeoylquinic acid, caffeic acid, isochlorogenic acid B, isochlorogenic acid A and isochlorogenic acid C) contained in honeysuckle flower that is the monarch drug of all the eight Yinqiao Jiedu serial preparations using quantitative analysis of multi-components by single-marker (QAMS). Firstly, chlorogenic acid was used as a reference to get the average relative correction factors (RCFs) of the other phenolic acids in ratios to the reference; columns and instruments from different companies were used to validate the durability of the achieved RCFs in different levels of standard solutions; and honeysuckle flower extract was used as the reference substance to fix the positions of chromatographic peaks. Secondly, the contents of seven phenolic acids in eight different Yinqiao Jiedu serial preparations samples were calculated based on the RCFs durability. Finally, the quantitative results were compared between QAMS and the external standard (ES) method. The results have showed that the durability of the achieved RCFs is good (RSD during 0.80% - 2.56%), and there are no differences between the quantitative results of QAMS and ES (the relative average deviation < 0.93%). So it can be successfully used to the quantitative control of honeysuckle flower principally prescribed in Yinqiao Jiedu serial preparations.
Caffeic Acids
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analysis
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Chlorogenic Acid
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analogs & derivatives
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analysis
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Chromatography, High Pressure Liquid
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Drugs, Chinese Herbal
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analysis
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Flowers
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chemistry
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Hydroxybenzoates
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analysis
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Lonicera
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chemistry
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Quinic Acid
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analogs & derivatives
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analysis
6.Comparative study on four major active compounds of Sanvitalia procumbens and Chrysanthemum morifolium cv 'Hangju' and 'Gongju'.
Liang WANG ; Tao WANG ; Qiao-Sheng GUO ; Yong HUANG ; Hao-Kun XU
China Journal of Chinese Materia Medica 2013;38(20):3442-3445
The contents of chlorogenic acid, 3,5-O-caffeoylquinic acid, galuteolin and quercitrin in Sanvitalia procumbens and Chrysanthemum morifolium cv. 'Hangju' and 'Gongju' were determined by RP-HPLC. The main active ingredient of S. procumbens was similar to C. morifolium cv. 'Hangju' and 'Gongju'. The content varied significantly. The contents of chlorogenic acid, quercitrin and galuteolin in S. procumbens were 7.46, 46.58, 26.01 mg x g(-1), respectively, and they were the highest among the samples. The content of 3,5-O-caffeoylquinic acid in C. morifolium cv. 'Hangju' was 14.70 mg x g(-1), it was the highest among the samples. The data of the study provide a basis for further research and development of S. procumbens.
Asteraceae
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chemistry
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Chlorogenic Acid
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analogs & derivatives
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analysis
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Chromatography, High Pressure Liquid
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Chrysanthemum
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chemistry
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Drugs, Chinese Herbal
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analysis
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Quinic Acid
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analogs & derivatives
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analysis
7.Quinic acid esters from herba of Siphonostegia chinensis.
Hong-liang JIANG ; Li-zhen XU ; Xue-dong YANG ; Da ZHANG ; Shi-lin YANG ; Zhong-mei ZOU
China Journal of Chinese Materia Medica 2002;27(12):923-926
OBJECTIVETo study the bioactive constituents, quinic acid esters, from Siphonostegia chinensis.
METHODThe compounds were extracted with solvents, isolated by various column chromatography and identified by spectroscopic methods.
RESULTThree quinic acid esters were isolated and identified as 3,4-di-O-caffeoylquinic acid(I), macranthoin F(II), and methyl ester of 3, 4,5-tri-O-caffeoylquinic acid (III).
CONCLUSIONAll compounds were isolated from Siphonostegia for the first time.
Chlorogenic Acid ; analogs & derivatives ; chemistry ; isolation & purification ; Plants, Medicinal ; chemistry ; Quality Control ; Saponins ; chemistry ; isolation & purification ; Scrophulariaceae ; chemistry
8.Simultaneous determination of rutin, isoquercitrin and chlorogenic acid in Farfarae Flos by HPLC.
Di WU ; Zhengtao WANG ; Mian ZHANG
China Journal of Chinese Materia Medica 2010;35(20):2722-2725
OBJECTIVETo develop an HPLC method for simultaneous determination of rutin, isoquercitrin and chlorogenic acid in Farfarae Flos.
METHODThe analysis was carried out on a Phenomenex Synergi POLAR-RP 80A column (4.6 mm x 250 mm, 4 microm) with gradient elution using methanol-acetonitrile-water (adjusted to pH 2.5 with formic acid) as mobile phase. The flow rate was 1.2 mL x min(-1) and the detection wavelength was at 255 nm.
RESULTThe calibration curves were linear over the range of 0.2-2 000 microg x L(-1) for rutin and isoquercitrin, 10-2 000 microg x L(-1) for chlorogenic acid, respectively. The average recoveries were 99.5% for rutin, 100.1% for isoquercitrin and 99.4% for chlorogenic acid, respectively, with RSD not more than 3.0%.
CONCLUSIONThe described method is reliable and could be used for the quality control of Farfarae Flos.
Calibration ; Chlorogenic Acid ; analysis ; Chromatography, High Pressure Liquid ; methods ; Quercetin ; analogs & derivatives ; analysis ; Rutin ; analysis ; Tussilago ; chemistry
9.Simultaneous determination of five organic acids in Kudiezi injection by HPLC.
Rui LIU ; Lu SUN ; Wen ZHAO ; Yu-Bo LI ; Yan-Jun ZHANG
China Journal of Chinese Materia Medica 2013;38(19):3287-3290
The aim was to develop a high performance liquid chromatography method for simultaneous determination of five organic acids in Kudiezi injection. The Diamonsil C18 column (4.6 mm x 200 mm, 5 microm) was adopted with acetonitrile and water as the mobile phase at a gradient mode program. The flow rate was 1.0 mL min-1 , detection wavelength was 325 nm, and column temperature was 35 degree C. The linear range of monocaffeyltartaric acid, chlorogenic acid, caffeic acid, ferulic acid, and chicoric acid were 0. 64-81.60 (r =0. 999 9),0.09-11. 10 (r =0.999 8) ,0.09-11.30 (r =0. 999 8),0.10-12.80 (r =0.999 9),0.43-55. 50 mg L-1 (r = 0.999 8) , respectively. The average recoveries were 101.8% ,100. 9% ,99. 24% ,99. 83% ,101.9%, respectively, with RSD of less than 2.0%. The developed HPLC method was simple, sensitive and accurate with good repeatability. This work provided helpful information for comprehensive quality control of Kudiezi injection. [Key words] Kudiezi injection; organic acids; content determination; HPLC
Caffeic Acids
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analysis
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Chlorogenic Acid
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analysis
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Chromatography, High Pressure Liquid
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methods
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Coumaric Acids
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analysis
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Drugs, Chinese Herbal
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chemistry
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Quinic Acid
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analogs & derivatives
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analysis
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Succinates
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analysis
10.Chemical comparison of different Farfarae Flos by NMR-based metabolomic approaches.
Zheng-zheng ZHANG ; Hai-juan ZHI ; Xue-mei QIN ; Zhen-yu LI
Acta Pharmaceutica Sinica 2015;50(5):599-604
1H NMR-based metabolomic approach combined with multivariate statistical analysis was used to evaluate the quality of 21 Farfarae Flos (FF) samples from different growth regions. Principal component analysis showed that wild and cultivated FF could be separated clearly, suggesting a big chemical difference existed between them. Supervised PLS-DA analysis indicated that the wild samples showed higher levels of secondary metabolites, such as bauer-7-ene-3β, 16α-diol, chlorogenic acid, rutin, 7-(3'-ethylcrotonoyloxy)-1α-(2'-methyl-butyryloxy)-3, 14-dehydro-Z-notonipetranone (EMDNT), tussilagone, β-sitosterol and sitosterone. This is consistent with traditional experience that the quality of wild samples are better than that of cultivated ones. The content of pyrrolizidine alkaloids senkirkine also differed greatly among samples from different habitats. The Pearson correlation analysis showed that senkirkine is positively correlated with 4, 5-O-dicaffeoylquinic acid, 3,5-O-dicaffeoylquinic acid, 3,4-O-dicaffeoylquinic acid, rutin, kampferol analogues, to a statistically significant extent. The correlation between the toxic compounds and the bioactive components in FF should be further studied.
Chlorogenic Acid
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Drugs, Chinese Herbal
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chemistry
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Flowers
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chemistry
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Magnetic Resonance Imaging
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Magnetic Resonance Spectroscopy
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Metabolomics
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Quinic Acid
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analogs & derivatives
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Rutin
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Sitosterols
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Tussilago
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chemistry