1.Analysis of chemical constituents in ethyl acetate extract of Taxilli Herba by UPLC-Q-Exactive-MS and screening of potential xanthine oxidase inhibitors.
Yuan LIANG ; Li LI ; Yi CAI ; Li-Ba XU ; Feng-Feng XIE ; Da-Long LIANG ; Fu-Lai CHEN
China Journal of Chinese Materia Medica 2022;47(4):972-979
The present study analyzed and identified the chemical constituents from ethyl acetate(EA) extract of Taxilli Herba with UPLC-Q-Exactive-MS and screened active xanthine oxidase(XO) inhibitors with HPLC. The analysis was performed on an Hypersil GOLD C_(18) reversed-phase column(2.1 mm×50 mm, 1.9 μm), with the mobile phase of water containing 1% formic acid(A) and methanol(B) under gradient elution, the flow rate of 0.3 mL·min~(-1), and the injection volume of 5 μL. ESI source was used for MS and the compounds were collected in positive and negative ion modes. Xcalibur 4.1 was used to analyze the retention time, accurate relative molecular weight, and fragmentation of the compounds. The inhibitory activity of some known compounds on XO was screened by HPLC. Thirty chemical constituents were identified, including phenolic acids and flavonoids by experimental data combined with information of standards, data reported previously, and databases, such as MzCloud and ChemSpider. The activities of 10 chemical components were screened. Gallic acid and naringenin chalcone had strong inhibitory activities on XO with IC_(50) of 57 μg·mL~(-1) and 108 μg·mL~(-1). UPLC-Q-Exactive-MS allows the accurate, rapid, and comprehensive identification of main chemical constituents from Taxilli Herba. Gallic acid and naringenin chalcone may be the active components of XO inhibitors.
Acetates
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Chromatography, High Pressure Liquid
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Drugs, Chinese Herbal/chemistry*
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Tandem Mass Spectrometry
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Xanthine Oxidase
2.Chemical constituents from ethyl acetate extraction of Prunus mume.
Can-Can WANG ; Wei ZHANG ; De-Ling WU ; Feng-Qing XU ; Jin-Song LIU ; Jin-Wei QIAO
China Journal of Chinese Materia Medica 2020;45(2):347-351
Eight compounds were isolated from the ethyl acetate extraction of Prunus mume by column chromatography. On the basis of physicochemical properties and spectrum analysis, these compounds were identified as isoquercitrin-6″-O-benzoate(1), pinoresinol(2), naringin(3), ethyl-β-D-glucopyranoside(4), astragalin(5), quercetin(6), hypericin(7), and rutin(8). Among them, compound 1 was a new natural product, and compounds 2-5 were isolated from this plant for the first time. In vitro study, compounds 1, 3, 5-8 could significantly increase the cell survival ratio.
Acetates
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Phytochemicals/analysis*
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Plant Extracts/chemistry*
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Prunus/chemistry*
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Solvents
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
;
Flavonoids
;
analysis
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Iridoids
;
analysis
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Lignans
;
analysis
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Molecular Structure
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Monoterpenes
;
analysis
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Phytochemicals
;
analysis
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Plant Extracts
;
chemistry
;
Sesquiterpenes
;
analysis
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Triterpenes
;
analysis
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Valerian
;
chemistry
4.An oriental melon 9-lipoxygenase gene CmLOX09 response to stresses, hormones, and signal substances.
Li-Jun JU ; Chong ZHANG ; Jing-Jing LIAO ; Yue-Peng LI ; Hong-Yan QI
Journal of Zhejiang University. Science. B 2018;19(8):596-609
In plants, lipoxygenases (LOXs) play a crucial role in biotic and abiotic stresses. In our previous study, five 13-LOX genes of oriental melon were regulated by abiotic stress but it is unclear whether the 9-LOX is involved in biotic and abiotic stresses. The promoter analysis revealed that CmLOX09 (type of 9-LOX) has hormone elements, signal substances, and stress elements. We analyzed the expression of CmLOX09 and its downstream genes-CmHPL and CmAOS-in the leaves of four-leaf stage seedlings of the oriental melon cultivar "Yumeiren" under wound, hormone, and signal substances. CmLOX09, CmHPL, and CmAOS were all induced by wounding. CmLOX09 was induced by auxin (indole acetic acid, IAA) and gibberellins (GA3); however, CmHPL and CmAOS showed differential responses to IAA and GA3. CmLOX09, CmHPL, and CmAOS were all induced by hydrogen peroxide (H2O2) and methyl jasmonate (MeJA), while being inhibited by abscisic acid (ABA) and salicylic acid (SA). CmLOX09, CmHPL, and CmAOS were all induced by the powdery mildew pathogen Podosphaera xanthii. The content of 2-hexynol and 2-hexenal in leaves after MeJA treatment was significantly higher than that in the control. After infection with P. xanthii, the diseased leaves of the oriental melon were divided into four levels-levels 1, 2, 3, and 4. The content of jasmonic acid (JA) in the leaves of levels 1 and 3 was significantly higher than that in the level 0 leaves. In summary, the results suggested that CmLOX09 might play a positive role in the response to MeJA through the hydroperoxide lyase (HPL) pathway to produce C6 alcohols and aldehydes, and in the response to P. xanthii through the allene oxide synthase (AOS) pathway to form JA.
Abscisic Acid
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Acetates/chemistry*
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Aldehyde-Lyases/metabolism*
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Aldehydes/chemistry*
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Cucurbitaceae/genetics*
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Cyclopentanes/chemistry*
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Cytochrome P-450 Enzyme System/metabolism*
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Gene Expression Profiling
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Gene Expression Regulation, Plant
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Hormones/metabolism*
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Hydrogen Peroxide/metabolism*
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Intramolecular Oxidoreductases/metabolism*
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Lipoxygenase/metabolism*
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Oxylipins/chemistry*
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Plant Leaves/genetics*
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Plant Proteins/metabolism*
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Promoter Regions, Genetic
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Salicylic Acid/chemistry*
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Seedlings/metabolism*
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Signal Transduction
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Stress, Physiological
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Transgenes
5.Anti-inflammatory and membrane stabilizing properties of methyl jasmonate in rats.
Solomon UMUKORO ; Akinyinka Oladipo ALABI ; Anthony Taghogho EDUVIERE ; Abayomi Mayowa AJAYI ; Oluwafemi Gabriel OLUWOLE
Chinese Journal of Natural Medicines (English Ed.) 2017;15(3):202-209
The present investigation was carried out to evaluate anti-inflammatory and membrane stabilizing properties of methyl jasmonate (MJ) in experimental rat models of acute and chronic inflammation. The effects of MJ on acute inflammation were assessed using carrageenan-induced rat's paw edema model. The granuloma air pouch model was employed to evaluate the effects of MJ on chronic inflammation produced by carrageenan in rats. The number of white blood cells (WBC) in pouch exudates was estimated using light microscopy. The levels of biomarkers of oxidative stress, such as malondialdehyde (MDA), glutathione (GSH) and activity of antioxidant enzymes in the exudates, were determined using spectrophotometry. The membrane stabilizing property of MJ was assessed based on inhibition of hemolysis of rat red blood cells (RBC) exposed to hypotonic medium. Our results indicated that MJ (25-100 mg·kg, i.p.) produced significant anti-inflammatory activity in carrageenan-induced paw edema in rats (P < 0.05). MJ reduced the volume of pouch exudates and the number of WBC in carrageenan-induced granulomatous inflammation. It also exhibited potent antioxidant and membrane stabilizing activities. In conclusion, these findings suggest the therapeutic potentials of methyl jasmonate in disease conditions associated with inflammation and its anti-inflammatory activity may be related to its antioxidant and membrane stabilizing activities.
Acetates
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administration & dosage
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Animals
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Anti-Inflammatory Agents
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administration & dosage
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Cell Membrane
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chemistry
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drug effects
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immunology
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Cyclopentanes
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administration & dosage
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Disease Models, Animal
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Edema
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drug therapy
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immunology
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Erythrocytes
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chemistry
;
drug effects
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Glutathione
;
immunology
;
Humans
;
Male
;
Malondialdehyde
;
immunology
;
Oxylipins
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administration & dosage
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Plant Extracts
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administration & dosage
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Rats
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Rats, Wistar
6.Synergistic Anti-bacterial Effects of Phellinus baumii Ethyl Acetate Extracts and beta-Lactam Antimicrobial Agents Against Methicillin-Resistant Staphylococcus aureus.
Seung Bok HONG ; Man Hee RHEE ; Bong Sik YUN ; Young Hoon LIM ; Hyung Geun SONG ; Kyeong Seob SHIN
Annals of Laboratory Medicine 2016;36(2):111-116
BACKGROUND: The development of new drugs or alternative therapies effective against methicillin-resistant Staphylococcus aureus (MRSA) is of great importance, and various natural anti-MRSA products are good candidates for combination therapies. We evaluated the antibacterial activities of a Phellinus baumii ethyl acetate extract (PBEAE) and its synergistic effects with beta-lactams against MRSA. METHODS: The broth microdilution method was used to determine the minimal inhibitory concentration (MIC) and minimal bactericidal concentration (MBC) of the PBEAE. The PBEAE synergistic effects were determined by evaluating the MICs of anti-staphylococcal antibiotic mixtures, with or without PBEAE. Anti-MRSA synergistic bactericidal effects of the PBEAE and beta-lactams were assessed by time-killing assay. An ELISA was used to determine the effect of the PBEAE on penicillin binding protein (PBP)2a production. RESULTS: The MICs and MBCs of PBEAE against MRSA were 256-512 and 1,024-2,048 microg/mL, respectively. The PBEAE significantly reduced MICs of all beta-lactams tested, including oxacillin, cefazolin, cefepime, and penicillin. However, the PBEAE had little or no effect on the activity of non-beta-lactams. Time-killing assays showed that the synergistic effects of two beta-lactams (oxacillin and cefazolin) with the PBEAE were bactericidal in nature (Deltalog10 colony forming unit/mL at 24 hr: 2.34-2.87 and 2.10-3.04, respectively). The PBEAE induced a dose-dependent decrease in PBP2a production by MRSA, suggesting that the inhibition of PBP2a production was a major synergistic mechanism between the beta-lactams and the PBEAE. CONCLUSIONS: PBEAE can enhance the efficacy of beta-lactams for combined therapy in patients infected with MRSA.
Acetates/chemistry
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Agaricales/*chemistry/metabolism
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Anti-Infective Agents/chemistry/*pharmacology
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Drug Synergism
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Enzyme-Linked Immunosorbent Assay
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Methicillin-Resistant Staphylococcus aureus/*drug effects/metabolism
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Microbial Sensitivity Tests
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Penicillin-Binding Proteins/analysis/metabolism
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Plant Extracts/chemistry/*pharmacology
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beta-Lactams/*pharmacology
7.Effect of glyceryl triacetate on properties of PLA/PBAT blends.
Nan YANG ; Xiyuan WANG ; Yunxuan WENG ; Yujuan JIN ; Min ZHANG
Chinese Journal of Biotechnology 2016;32(6):839-847
Poly lactic acid (PLA)/Poly (butyleneadipate-co-terephthalate)(PBAT) and glyceryl triacetate (GTA) blend were prepared by torque rheometer, and the effect of GTA on thermodynamical performance, mechanical properties and microstructure of PLA/PBAT composites were studied using differential scanning calorimeter(DSC), dynamic mechanical analysis(DMA), universal testing machine, impact testing machine and scanning electron microscope(SEM). After adding GTA, Tg values of the two phases gradually became closer, blends cold crystallization temperature and melting temperature decreased. When with 3 phr GTA, the dispersed phase particle size of PLA/PBAT blend decreased. Mechanics performance test showed that the elongation at break and impact strength of the PLA/PBAT blend was greatly increased with 3 phr GTA, and the elongation at break increased 2.6 times, improved from 17.7% to 64.1%.
Acetates
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chemistry
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Calorimetry, Differential Scanning
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Crystallization
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Lactic Acid
;
Polyesters
;
chemistry
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Polymers
;
Temperature
8.HPLC-based activity profiling of anti-hepatocellular carcinoma constituents from the Tibetan medicine, Caragana tibetica.
Ping SONG ; Qiang WANG ; Jing-Nan LV ; Chan XU ; Qin-Xiong LIN ; Xin-Hua MA ; Mi HUANG ; Xin-Zhou YANG
Journal of Huazhong University of Science and Technology (Medical Sciences) 2015;35(3):450-455
During the screening of a traditional Chinese folk herb library against HepG2 and Hep3B cell lines, the EtOAc extract from the Tibetan medicine, Caragana tibetica (CT-EtOAc) exhibited potential anti-hepatocellular carcinoma (anti-HCC) activity. HPLC-based activity profiling was performed for targeted identification of anti-HCC activity from CT-EtOAc by MS-directed purification method. CT-EtOAc was separated by time-based fractionation for further anti-HCC bioassay by a semipreparative HPLC column (150 mm × 10 mm i.d., 5 μm) with a single injection of 5 mg. Bioassay-guided and ESIMS-directed large scale purification was performed with a single injection of 400 mg of CT-EtOAc by peak-based fractionation. A 1.4-mm heavy wall micro NMR tube with z-gradient was used to measure one and two dimensional NMR spectra for the minor or trace amounts of components of the extract. Two active compounds could be elucidated as naringenin chalcone (CT-1) and 3-hydroxy-8, 9-dimethoxypterocarpan (CT-2) relevant to anti-HCC effects for the EtOAc extract of C. tibetica rapidly and unambiguously by this protocol.
Acetates
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pharmacology
;
Antineoplastic Agents
;
chemistry
;
pharmacology
;
Caragana
;
chemistry
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Carcinoma, Hepatocellular
;
drug therapy
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Cell Line, Tumor
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Chalcones
;
pharmacology
;
Chromatography, High Pressure Liquid
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Hep G2 Cells
;
Humans
;
Liver Neoplasms
;
drug therapy
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Medicine, Tibetan Traditional
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Plant Extracts
;
chemistry
;
pharmacology
;
Plant Roots
;
chemistry
9.Screening of homoacetogen mixed culture converting H2/CO2 to acetate.
Kan LUO ; Bo FU ; Lijuan ZHANG ; Hongbo LIU ; He LIU
Chinese Journal of Biotechnology 2014;30(12):1901-1911
Homoacetogens are a group of microorganisms with application potential to produce chemicals and biofuels by the bioconversion of synthesis gas. In this study, we collected waste activated sludge samples to screen homoacetogens by Hungate anaerobic technique, and studied the effect of pH on acetate and alcohol production from H2/CO2 gas. The mixed culture contained Clostridium ljungdahlii, Lysinibacillus fusiformis and Bacillus cereus. Acetate concentration achieved 31.69 mmol/L when the initial pH was 7. The mixed culture containing homoacetogen could converting H2/CO2 to acetate, which provides an efficient microbial resource for the bioconversion of synthesis gas.
Acetates
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chemistry
;
Bacteria
;
classification
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Biofuels
;
Carbon Dioxide
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Hydrogen
;
Sewage
;
microbiology
10.Determination of the content of residual solvents in Haikesu 2 by head-space gas chromatography.
Xuan XIAO ; Dong LIU ; Ke-Min WANG ; Jia-Zhi CHEN ; Shu ZHANG
Acta Academiae Medicinae Sinicae 2014;36(6):602-605
OBJECTIVETo determine ethylacetate and petroleum ether(60-90 ℃)in Haikesu 2,which is one of the raw materials of artificial musk,using the head-space gas chromatography.
METHODSThe determination was performed on HP-5(30 m×0.53 mm,5 Μm)capillary column with an hydrogen flame ionization detector. The solvent was dimethyl sulfoxide and the internal standard was methanol. The injector temperature and the detector temperature were controlled at 180 ℃ and 250 ℃,respectively. The carrier gas was nitrogen. The containers of head-space injector were preheated at 90 ℃ for 15 minutes. The column temperature was programmed raised,which achieved baseline separation of the components.
RESULTSThe results showed a good linear relationship for ethylacetate and petroleum ether(60-90 ℃)in their linearity range;and the limit of detection was 0.7 and 0.3 Μg/ml,respectively. The good precision and good average recoveries were satisfactory.
CONCLUSIONThe head-space gas chromatography is simple,rapid,and precise technique for the measurement of residual solvents in Haikesu 2.
Acetates ; analysis ; Chromatography, Gas ; Drugs, Chinese Herbal ; chemistry ; Fatty Acids, Monounsaturated ; chemistry ; Flame Ionization ; Solvents ; analysis

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