1.Correlation of non-crocin components of Gardeniae Fructus with its external properties.
Xiao YE ; Wei-Hong FENG ; Dong ZHANG ; Xiao-Qian LIU ; Yao-Hua LIANG ; Chun LI ; Zhi-Min WANG
China Journal of Chinese Materia Medica 2022;47(15):4098-4109
This study aimed to explore the correlation of the content of 15 non-crocin components of Gardeniae Fructus with its external properties(shape and color). The fruit shape was quantified according to the length/diameter measured by ruler and vernier calliper and the chromaticity values L~*, a~*, b~*, and ΔE~* of all samples were determined by chroma meter. Chromatographic separation was conducted on a Welch Ultimate XB C_(18) column(4.6 mm×250 mm, 5 μm) under gradient elution with acetonitrile solution(A) and 0.1% formic acid aqueous solution(B) as the mobile phase at a flow rate of 1.0 mL·min~(-1). The column temperature was 30 ℃ and the detection wavelength was 238 nm. The high-performance liquid chromatography(HPLC) method was established for simultaneous determination of the content of eight iridoid glycosides, six phenolic acids, and one flavonoid in 21 batches of Gardeniae Fructus samples. The correlation of the content of the 15 components with shapes and chromaticity values in each sample was analyzed by multivariate statistical analysis. According to the circulation situation and traditional experience, 21 batches of Gardeniae Fructus samples were divided into three categories, namely 14 batches of Jiangxi products(small and round, red and yellow), 4 batches of Fujian products(oval, red) and 3 batches of Shuizhizi(Gardenia jasminoides, longest, reddest). The Gardeniae Fructus samples were sequenced as Jiangxi products(1.71) < Fujian products(1.99) < Shuizhizi(2.55) in terms of the length/diameter average, Jiangxi products(17.7) < Fujian products(19.7) ≈ Shuizhizi(19.6) in terms of average value of a~*(red and green), Jiangxi products(24.4) > Fujian products(19.2) ≈ Shuizhizi(19.3) in terms of b~*(yellow and blue), and Jiangxi products(49.8) > Fujian products(48.0) ≈ Shuizhizi(47.8) in terms of L~*(brightness). The total content of the 15 components, 8 iridoid glycosides, 6 phenolic acids, and rutin in Jiangxi products was in the ranges of 65.53-99.64, 52.15-89.16, 6.10-11.83, and 0.145-1.81 mg·g~(-1), respectively. The total amount of the 15 components, 8 iridoid glycosides, 6 phenolic acids, and rutin in Fujian products was in the ranges of 69.33-94.35, 63.52-85.19, 5.39-8.41, and 0.333-0.757 mg·g~(-1), respectively. In Shuizhizi, the total content of the 15 components, 8 iridoid glycosides, 6 phenolic acids, and rutin was in the ranges of 77.35-85.98, 68.69-76.56, 7.30-9.05, and 0.368-0.697 mg·g~(-1), respectively. Pearson correlation analysis revealed that Gardeniae Fructus with leaner and longer fruit shape possessed lower content of total phenolic acids(the sum of the six phenolic acids) and rutin, but the correlation with iridoid glycosides was not high. Additionally, the higher content of total phenolic acids and rutin denoted the yellow coloration of Gardeniae Fructus, and the higher content of cryptochlorogenic acid, chlorogenic acid, and rutin meant the brighter color of Gardeniae Fructus. However, the higher content of geniposide and neochlorogenic acid and the lower content of deacetyl asperulosidic acid methyl ester led to the red coloration of Gardeniae Fructus. The results indicated that the morphological characters of Gardeniae Fructus were closely related to its chemical components. The more round shape and the yellower color reflected the higher content of phenolic acids and flavonoid, and Gardeniae Fructus with redder color had higher content of geniposide. OPLA-DA showed that the length/diameter and the content of six iridoid glycosides(gardoside, shanzhiside, gardenoside, genipin 1-gentiobioside, 6β-hydroxy geniposide, and deacetyl asperulosidic acid methyl ester), two phenolic acids(neochlorogenic acid and cryptochlorogenic acid) and rutin could be used as markers to distinguish three types of samples. This study provided experimental data for the scientific connotation of "quality evaluation through morphological identification" of Gardeniae Fructus.
Chromatography, High Pressure Liquid/methods*
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Drugs, Chinese Herbal/analysis*
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Esters/analysis*
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Flavonoids/analysis*
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Fruit/chemistry*
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Gardenia/chemistry*
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Iridoids/analysis*
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Rutin/analysis*
2.Fingerprinting and multi-indicator quantitative analysis of Mongolian drug Digeda-4 decoction.
Xiang TIAN ; Rui-Xue DING ; Gen-Na BA ; Yu-Xia BAI ; Na-Mu-Ji-la LAXI ; Xiao-Yong RAO ; Xiao-Jian LUO
China Journal of Chinese Materia Medica 2018;43(19):3962-3969
To establish the high performance liquid chromatography (HPLC) fingerprint for Digeda-4 decoction (DGD-4D), determine the contents of aesculetin, geniposide, picroside Ⅰ, picroside Ⅱ and ellagicacid in DGD-4D, and provide the scientific foundation for quality control of DGD-4D. The analysis was performed on Diamonsil(2) C₁₈ (4.6 mm×250 mm,5 μm) column, with methanol-0.1% phosphoric acid aqueous solution as mobile phase for gradient elution. The flow rate was 1.0 mL·min⁻¹; injection size was 10 μL; temperature was maintained at 30 °C, and the detection wavelength was set at 254 nm. The common mode of DGD-4D HPLC fingerprint was established, and the hidden information was analyzed by Chemometrics. Chromatographic peaks for DGD-4D were identified by HPLC and quantitative analysis was conducted for characteristic peaks. There were 17 common peaks in the fingerprints and the similarity of the fingerprints was over 0.9 in all 15 batches. The samples were broadly divided into four kinds by principal component analysis and clustering analysis. Four marker compounds were verified by partial least squares discriminant analysis, and No. 9, 12 and 14 peaks were identified as geniposide, picroside Ⅱ, and picroside Ⅰ respectively. The average recoveries were in the range of 95.91%-97.31%. The HPLC fingerprint method for content determination is reliable, accurate, rapid, simple, and reproducible, and can be used as one of the effective methods to control the quality of DGD-4D.
Chromatography, High Pressure Liquid
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Cinnamates
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Drugs, Chinese Herbal
;
analysis
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standards
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Iridoid Glucosides
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Iridoids
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Methanol
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Principal Component Analysis
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Quality Control
3.Chemical constituents from ethyl acetate-soluble extraction of Valeriana jatamansi.
Sheng LIN ; Peng FU ; Yun-Heng SHEN ; Ji YE ; Zhong-Xiao ZHANG ; Xian-Wen YANG ; Hui-Liang LI ; Run-Hui LIU ; Xi-Ke XU ; Wei-Dong ZHANG
China Journal of Chinese Materia Medica 2018;43(1):100-108
Application of a combination of various chromatographic techniques including column chromatography over silica gel, Sephadex LH-20, macroporous adsorbent resin, and reversed-phase HPLC, led to the isolation of 173 compounds including irdidoids, monoterpenes, sesquiterpenes, triterpenes, lignans, flavonoids, and simple aromatic derivatives from the ethyl acetate-soluble fraction of the whole plants of Valeriana jatamansi(Valerianaceae), and their structures were elucidated by spectroscopic methods including 1D, 2D NMR UV, IR, and MS techniques. Among them, 77 compounds were new. In previous reports, we have described the isolation, structure elucidation, and bioactivities of 68 new and 25 known compounds. As a consequence, we herein reported the isolation and structure elucidation of the remaining 9 new and 71 known compounds, the structure revision of valeriotriate A(8a), as well as cytotoxicity of some compounds.
Acetates
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Chromatography, High Pressure Liquid
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Flavonoids
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analysis
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Iridoids
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analysis
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Lignans
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analysis
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Molecular Structure
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Monoterpenes
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analysis
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Phytochemicals
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analysis
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Plant Extracts
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chemistry
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Sesquiterpenes
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analysis
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Triterpenes
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analysis
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Valerian
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chemistry
4.Pharmacokinetics of loganin, ferulic acid and stilbene glucoside in Bushen Tongluo formula in vivo.
Xiang-dan LIU ; Pan HUANG ; Yue-hua LU ; Ming MA ; Ri-bao ZHOU ; Lin-xiang YUAN ; Xin-jun PENG
China Journal of Chinese Materia Medica 2015;40(12):2428-2434
To study the pharmacokinetics characteristic of loganin, ferulic acid and stilbene glucoside in rat plasma after oral administration of Bushen Tongluo formula. The plasma samples were treated by using liquid-liquid extraction technique, the concentrations were determined by HPLC-UV. Johnson spherigel C18 column (4.6 mm x 250 mm, 5 μm) was adopted and eluted with the of mobile phase of methanol-water containing 0.01% glacial acetic acid in a gradient mode, with the flow rate at 1.0 mL x min(-1), column temperature at 30 degrees C and injection volume of 10 μL. According to the findings, loganin was determined at 235 nm, ferulic acid and stilbene glucoside were determined at 320 nm, with the sample size of 10 μL. The pharmacokinetic parameters of loganin, ferulic acid and stilbene glucoside were calculated by DAS 2. 0 software as follows: C(max) was (0.369 ± 0.042), (0.387 ± 0.071), (0.233 ± 0.044) mg x L(-1); t(max) was (0.226 ± 0.022), (0.282 ± 0.031), (0.233 ± 0.044) h; t(½β) was (6.89 ± 0.20), (10.73 ± 0.11), (6.93 ± 0.09) h; AUC(0-∞) was (1.91 ± 0.36), (3.22 ± 0.52), (1.52 ± 0.33) mg x h x L(-1); AUCO(0-t) was (1.62 ± 0.33), (2.58 ± 0.43), (1.30 ± 0.30) mg x h x L(-1); CL was (20.2 ± 4.0), (1.39 ± 0.23), (31.7 ± 6.9) L x h(-1) x kg(-1), respectively. The results showed that after the oral administration with Bushen Tongluo formula, loganin, ferulic acid and stilbene glucoside showed concentration-time curves in conformity with the two compartment model, with a rapid absorption, loganin and stilbene glucoside was excreted at a moderate speed, and ferulic acid was excreted slowly (but with the highest bioavailability). Bushen Tongluo formula can main maintain plasma concentration with three administrations everyday and so is suitable to be made into common oral preparation.
Administration, Oral
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Animals
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Biological Availability
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Coumaric Acids
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administration & dosage
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blood
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pharmacokinetics
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Drugs, Chinese Herbal
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administration & dosage
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analysis
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pharmacokinetics
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Glucosides
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administration & dosage
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blood
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pharmacokinetics
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Iridoids
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administration & dosage
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blood
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pharmacokinetics
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Male
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Rats
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Rats, Sprague-Dawley
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Stilbenes
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administration & dosage
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blood
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pharmacokinetics
5.A partial pathway- and network-based transformation reveals the synergistic mechanism of JA and UA against cerebral ischemia-reperfusion injury.
Shanshan GUO ; Li GUO ; Yanan YU ; Bing LI ; Yingying ZHANG ; Haixia LI ; Ping WU ; Jie WANG ; Ye YUAN ; Zhong WANG ; Yongyan WANG
Protein & Cell 2014;5(11):873-877
Animals
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Brain
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drug effects
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metabolism
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pathology
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Brain Ischemia
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complications
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Drug Synergism
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Gene Regulatory Networks
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drug effects
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genetics
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Iridoids
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pharmacology
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Linear Models
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Male
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Mice
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Models, Genetic
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Oligonucleotide Array Sequence Analysis
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Reperfusion Injury
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drug therapy
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etiology
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genetics
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Signal Transduction
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drug effects
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genetics
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Transcriptome
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drug effects
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genetics
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Ursodeoxycholic Acid
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pharmacology
6.Content comparison of main chemical compositions in Gardenia jasminoids roasted with ginger juice.
Cun ZHANG ; Yu-Tian LI ; Yong-Qing XIAO ; Ding-Rong YU ; Yin-Lian MA ; Xue-Zhu GU
China Journal of Chinese Materia Medica 2013;38(7):962-965
OBJECTIVETo compare the contents of the main chemical compositions in Gardenia jasminoids before and after being roasted with ginger juice.
METHODFour diterpenoid pigments constituents (C-1, C-2, C-3, crocetin) were determined simultaneously by UPLC on an Agilent Poroshell 120 EC-C18 column at 35 degrees C with the methanol-0.5% formic acid anhydrous in gradient elution as the mobile phrase. The detection wavelength was set at 440 nm and the flow rate was 0.4 mL x min(-1). Two iridoids constituents (G-1, G-2) were determined simultaneously by HPLC on an Agilent TC-C18(2) column at 35 degrees C with acetonitrile-0.5% formic acid anhydrous (18:82) as the mobile phrase. The detection wavelength was set at 238 nm and the flow rate was 1.0 mL x min(-1).
RESULTAfter being processed with ginger juice, the contents of the diterpenoid pigments constituents decreased slightly and the contents of the iridoids constituents increased slightly.
CONCLUSIONThe contents of the main chemical compositions in G. jasminoids roasted with ginger juice increased slightly with some regularity, but there were no significant differences.
Carotenoids ; analysis ; Chemistry, Pharmaceutical ; Chromatography, High Pressure Liquid ; Drugs, Chinese Herbal ; analysis ; Gardenia ; chemistry ; Ginger ; chemistry ; Iridoids ; analysis ; Pharmacology
7.Determination of loganin in Pterocephalus hookeri by HPLC.
De TAN ; Rui GU ; Yi ZHANG ; Xianli MENG ; Xianrong LAI
China Journal of Chinese Materia Medica 2011;36(24):3472-3474
OBJECTIVETo develop an HPLC method for determination of loganin in Pterocephalus hookeri.
METHODThe analysis was performed on a Welchrom C18 column (4.6 mm x 250 mm, 5 microm) with acetonitrile-water (12:88) as the the mobile phase at a flow rate of 1 mL x min(-1) and the detection wavelength was 240 nm.
RESULTThe peak areas and injection amounts of loganin had a good linear relationship at the range of 0.06-1.2 microg. The average recovery was 97.0%, and the RSD was 1.4%.
CONCLUSIONThe method is simple, accurate, and can be used for its quality control.
Chromatography, High Pressure Liquid ; methods ; Iridoids ; analysis ; Medicine, Tibetan Traditional ; Plants, Medicinal ; chemistry
8.Role and mechanism of uncoupling protein 2 on the fatty acid-induced dysfunction of pancreatic alpha cells in vitro.
Jie-ying SU ; Hong-liang LI ; Wen-ying YANG ; Jian-zhong XIAO ; Rui-qin DU ; Xiao-xia SHEN ; Zhe CAI ; Lan ZHANG ; Jun SHU
Chinese Medical Journal 2010;123(17):2416-2423
BACKGROUNDUncoupling protein (UCP) 2 is related to the dysfunction of beta cells induced by fatty acids. However, whether UCP2 has similar effects on alpha cell is still not clear. This study aimed to investigate the effects of UCP2 and its possible mechanisms in lipotoxicity-induced dysfunction of pancreatic alpha cells.
METHODSThe alpha TC1-6 cells were used in this study to evaluate the effects of palmitate and/or UCP2 inhibit factors on the glucagon secretory function, glucagon content, the glucagon mRNA level and the nitrotyrosine level in the supernatant. Meantime, the expression levels of UCP2 and peroxisome proliferator-activated receptor-γ coactivator-1 alpha (PGC-1 alpha) were measured by real-time reverse transcription polymerase chain reaction (RT-PCR) and Western blotting. Furthermore, the possible relationship between UCP2 and insulin signal transduction pathway was analyzed.
RESULTSPalmitate stimulated alpha cell glucagon secretion and the expression of UCP2 and PGC-1 alpha, which could be partially decreased by the inhibition of UCP2. Palmitate increased nitrotyrosine level and suppressed insulin signal transduction pathway in alpha cells. Inhibition of UCP2 influenced the effects of free fatty acid on alpha cells and may relate to glucagon secretion.
CONCLUSIONUCP2 played an important role on alpha cell dysfunction induced by free fatty acid in vitro, which may be related to its effects on oxidative stress and insulin signal transduction pathway.
Animals ; Cells, Cultured ; Glucagon ; secretion ; Glucagon-Secreting Cells ; drug effects ; physiology ; Insulin ; pharmacology ; Insulin Receptor Substrate Proteins ; metabolism ; Ion Channels ; genetics ; physiology ; Iridoid Glycosides ; pharmacology ; Iridoids ; Mice ; Mitochondrial Proteins ; genetics ; physiology ; Oxidative Stress ; Palmitic Acid ; toxicity ; Peroxisome Proliferator-Activated Receptor Gamma Coactivator 1-alpha ; Phosphorylation ; RNA, Messenger ; analysis ; Signal Transduction ; Trans-Activators ; genetics ; physiology ; Transcription Factors ; Tyrosine ; analogs & derivatives ; metabolism ; Uncoupling Protein 2
9.Determination of oleuropein in stem of Syringa oblata from different districts by HPLC.
Xiaohui WEI ; Shuxia ZHANG ; Weifeng ZHAI ; Shujun ZHANG ; Zhengtao WANG
China Journal of Chinese Materia Medica 2009;34(3):304-306
OBJECTIVETo develop an HPLC method for the determination of oleuropein in Syringa oblata.
METHODAn Aigilent ZORBAX SB- C18 column (4.6 mm x 250 mm, 5 microm) was used. The mobile phase was acetonitrile-water (21 : 79). The flow rate was 1.0 mL x min(-1). The detection wavelenghth was set at 232 nm and the column temperature was 30 degrees C.
RESULTThe linear range of oleuropein were from 0.011 62 g x L(-1) to 1.162 g x L(-1). The average recovery was 98.7% with RSD 2.5% (n=9).
CONCLUSIONThe method is reliable, accurate and specific. It can be used for quality control of the stem of Syringa oblata.
Acetonitriles ; chemistry ; Benzoates ; chemistry ; Chromatography, High Pressure Liquid ; methods ; Drugs, Chinese Herbal ; Iridoids ; Pyrans ; analysis ; Syringa ; chemistry ; Vasodilator Agents ; analysis
10.Two iridoid glycoside from roots of Phlomis medicinalis.
Hengyue XUE ; Chunhong ZHANG ; Gangli WANG ; Ruichao LIN ; Ping LI
China Journal of Chinese Materia Medica 2009;34(1):57-59
OBJECTIVETo study the chemical constituents of the roots of Phlomis medicinalis.
METHODThe compounds were isolated and repeatedly purified by macroporous resin, silica gel column chromatography, TLC and PREP-HPLC. Their structures were elucidated by physical and chemical properties and NMR spectra.
RESULTTwo iridoid glucosides were obtained and elucidated as 7-epilamalbide (1), chlorotuberoside (2).
CONCLUSIONCompound 1 was a new compound, compound 2 was isolated from the plant for the first time.
Glucosides ; analysis ; isolation & purification ; Iridoid Glucosides ; Iridoids ; analysis ; isolation & purification ; Magnetic Resonance Spectroscopy ; Phlomis ; chemistry ; Plant Roots ; chemistry

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