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991.
Partial least squares model and design of experiments toward the analysis of the metabolome of Jatropha gossypifolia leaves: Extraction and chromatographic fingerprint optimization 下载免费PDF全文
Fausto Carnevale Neto Rafael Teixeira Freire Patrícia Cardoso Renato Lajarim Carneiro Vanderlan Da Silva Bolzani Ian Castro‐Gamboa 《Journal of separation science》2016,39(6):1023-1030
A major challenge in metabolomic studies is how to extract and analyze an entire metabolome. So far, no single method was able to clearly complete this task in an efficient and reproducible way. In this work we proposed a sequential strategy for the extraction and chromatographic separation of metabolites from leaves Jatropha gossypifolia using a design of experiments and partial least square model. The effect of 14 different solvents on extraction process was evaluated and an optimized separation condition on liquid chromatography was estimated considering mobile phase composition and analysis time. The initial conditions of extraction using methanol and separation in 30 min between 5 and 100% water/methanol (1:1 v/v) with 0.1% of acetic acid, 20 μL sample volume, 3.0 mL min?1 flow rate and 25°C column temperature led to 107 chromatographic peaks. After the optimization strategy using i‐propanol/chloroform (1:1 v/v) for extraction, linear gradient elution of 60 min between 5 and 100% water/(acetonitrile/methanol 68:32 v/v with 0.1% of acetic acid), 30 μL sample volume, 2.0 mL min?1 flow rate, and 30°C column temperature, we detected 140 chromatographic peaks, 30.84% more peaks compared to initial method. This is a reliable strategy using a limited number of experiments for metabolomics protocols. 相似文献
992.
MALDI‐MS of flavonoids: a systematic investigation of ionization and in‐source dissociation mechanisms 下载免费PDF全文
Matrix assisted laser desorption ionization (MALDI) is a technique widely employed in the analysis of proteins and peptides, and nowadays it has also been applied to small molecules. There is little significant information regarding the in‐source dissociation processes on MALDI for natural products. Twenty‐six flavonoids (flavanones, flavones and flavonols) were analyzed by MALDI using different methods (with different matrices) and without matrix to comprehend the in‐source reactions and establish good analysis methods for these compounds. Depending on the class, structure and the laser intensity applied, methoxylated flavonoid aglycones can eliminate methyl radicals (˙CH3) in the source, such as flavonols, but lithium 2,4‐dihydroxybenzoate matrix suppresses the ˙CH3 eliminations and retro‐Diels–Alder cleavages in the source. All of the flavonoid O‐glycosides evaluated herein eliminated the sugar in source, even in the presence of the matrix, and its product radical ions ([M‐H‐sugar]?˙) were observed in the negative mode. The flavone C‐glycosides suffered intense dissociation, which was reduced by the addition of a matrix and the application of low laser intensity, mainly in the negative mode. Depending on the hydroxyl substituents, the [M‐H‐H]?˙ ion was observed with variable relative intensity in the spectra. Copyright © 2015 John Wiley & Sons, Ltd. 相似文献
993.
Synthesis of New Chlorin e6 Trimethyl and Protoporphyrin IX Dimethyl Ester Derivatives and Their Photophysical and Electrochemical Characterizations 下载免费PDF全文
Dr. José C. J. M. D. S. Menezes Prof. M. Amparo F. Faustino Prof. Kleber T. de Oliveira Dr. Marciana P. Uliana Prof. Vitor F. Ferreira Dr. Steffen Hackbarth Prof. Beate Röder Dr. Thiago Teixeira Tasso Dr. Taniyuki Furuyama Prof. Nagao Kobayashi Prof. Artur M. S. Silva Prof. M. Graça P. M. S. Neves Prof. José A. S. Cavaleiro 《Chemistry (Weinheim an der Bergstrasse, Germany)》2014,20(42):13644-13655
In view of increasing demands for efficient photosensitizers for photodynamic therapy (PDT), we herein report the synthesis and photophysical characterizations of new chlorin e6 trimethyl ester and protoporphyrin IX dimethyl ester dyads as free bases and ZnII complexes. The synthesis of these molecules linked at the β‐pyrrolic positions to pyrano[3,2‐c]coumarin, pyrano[3,2‐c]quinolinone, and pyrano[3,2‐c]naphthoquinone moieties was performed by using the domino Knoevenagel hetero Diels–Alder reaction. The α‐methylenechromanes, α‐methylenequinoline, and ortho‐quinone methides were generated in situ from a Knoevenagel reaction of 4‐hydroxycoumarin, 4‐hydroxy‐6‐methylcoumarin, 4‐hydroxy‐N‐methylquinolinone, and 2‐hydroxy‐1,4‐naphthoquinone, respectively, with paraformaldehyde in dioxane. All the dyads as free bases and as ZnII complexes were obtained in high yields. All new compounds were fully characterized by 1D and 2D NMR techniques, UV/Vis spectroscopy, and HRMS. Their photophysical properties were evaluated by measuring the fluorescence quantum yield, the singlet oxygen quantum yield by luminescence detection, and also the triplet lifetimes were correlated by flash photolysis and intersystem crossing (ISC) rates. The fluorescence lifetimes were measured by a time‐correlated single photon count (TCSPC) method, fluorescence decay associated spectra (FDAS), and anisotropy measurements. Magnetic circular dichroism (MCD) and circular dichroism (CD) spectra were recorded for one ZnII complex in order to obtain information, respectively, on the electronic and conformational states, and interpretation of these spectra was enhanced by molecular orbital (MO) calculations. Electrochemical studies of the ZnII complexes were also carried out to gain insights into their behavior for such applications. 相似文献
994.
M-TIMES SECANT-LIKE MULTI-PROJCTION METHOD FOR SPARSE MINIMIZATION PROBLEM@林正华
@宋岱才
@赵立芹~~ 相似文献
995.
指出了当前流行的差示扫描量热法DSC单峰法测样品纯度所基于的假定有一些不确切的地方,并用计算机动态摸拟了DSC实验过程,结果证实了本文的论断。 相似文献
996.
MAO Mingfei LUO Jianguang REN Li CHEN Zhequan LIU Zhifang College of Materials South China University of Technology Guangzhou China Department of Chemical Engineering Nanhua University Hengyang China 《Chinese Journal of Reactive Polymers》2002,(1)
1. INTRODUCTION Poly (diphenyl oxide) (DPO) resins are a series of heat-resisting thermosetting resins. In 1960s, the West House Company applied them to make H class insulting materials and got an extensive use successfully [1]. But due to the three main… 相似文献
997.
Integrated "ICT chromophore-receptor" systems show ion-induced shifts in their electronic absorption spectra. The wavelength of observation can be used to reversibly configure the system to any of the four logic operations permissible with a single input (YES, NOT, PASS 1, PASS 0), under conditions of ion input and transmittance output. We demonstrate these with dyes integrated into Tsien's calcium receptor, 1-2. Applying multiple ion inputs to 1-2 also allows us to perform two- or three-input OR or NOR operations. The weak fluorescence output of 1 also shows YES or NOT logic depending on how it is configured by excitation and emission wavelengths. Integrated "receptor(1)-ICT chromophore-receptor(2)" systems 3-5 selectively target two ions into the receptor terminals. The ion-induced transmittance output of 3-5 can also be configured via wavelength to illustrate several logic types including, most importantly, XOR. The opposite effects of the two ions on the energy of the chromophore excited state is responsible for this behaviour. INHIBIT and REVERSE IMPLICATION are two of the other logic types seen here. Integration of XOR logic with a preceding OR operation can be arranged by using three ion inputs. The fluorescence output of these systems can be configured via wavelength to display INHIBIT or NOR logic under two-input conditions. The superposition or multiplicity of logic gate configurations is an unusual consequence of the ability to simultaneously observe multiple wavelengths. 相似文献
998.
HOU Ying SHI Zhan YANG Ming LI Guang-hua FENG Shou-hua State key Laboratory of Inorganic Synthesis Preparative Chemistry College of Chemistry Jilin University Changchun P. R. China 《高等学校化学研究》2005,21(4):406-410
IntroductionThe syntheses of metal-organic coordination poly-mers have been attracting increasing attention owing tothe potential applications of their functional materials incatalysis,non-linear optics,magnetism sensors andmolecular recognition[1—7].Coordination polymers crys-tallized from polyaromatic acids and metal-ions are ofgreat interest for their polymeric structures and porousproperties[8—12].Their network topologies based on mo-lecular building blocks are usually controlled and mod… 相似文献
999.
João P.C. Tomé Dong-Gyu Cho Maria G.P.M.S. Neves Artur M.S. Silva 《Tetrahedron letters》2006,47(18):3131-3134
Sapphyrins participate in Diels-Alder reactions with pentacene affording novel barrelene-fused sapphyrins. The new compounds were synthesized using traditional heating and microwave irradiation conditions. The experiments carried out under microwave irradiation proved cleaner, affording only the monoadduct and in higher yields. 相似文献
1000.
Ncoglycoproteins of human serum albumin (HSA) modified with some kind of carbohydrates were synthesized. Their molecular weight and purification were determined by HPSEC and SDS-PAGE, respectively. The binding properties of these conjugates to hepatic steHate cells (HSCs) were evaluated by confocai fluorescence microscopy. The bioactivity revealed that compound 4a (HSA modified with glucose) showed high bindiug affinity. 相似文献