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71.
A method for the analytical determination of sotolon [4,5-dimethyl-3-hydroxy-2(5H)-furanone], maltol [3-hydroxy-2-methyl-4H-pyran-4-one] and free furaneol [2,5-dimethyl-4-hydroxy-3(2H)-furanone] in wine has been developed. The analytes are extracted from 50 ml of wine in a solid-phase extraction cartridge filled with 800 mg of LiChrolut EN resins. Interferences are removed with 15 ml of a pentane-dichloromethane (20:1) solution, and analytes are recovered with 6 ml of dichloromethane. The extract is concentrated up to 0.1 ml and analyzed by GC-ion trap MS. Maltol and sotolon were determined by selected ion storage of ions in the m/z ranges 120-153 and 79-95, using the ions m/z 126 and 83 for quantitation, respectively. Furaneol was determined by non-resonant fragmentation of the m/z 128 mother ion and subsequent analysis of the m/z 81 ion. The detection limits of the method are in all cases between 0.5 and 1 microg l(-1), well below the olfactory thresholds of the compounds. The precision of the method is in the 4-5% range for levels in wine around 20 microg l(-1). Linearity holds at least up to 400 microg l(-1), and is satisfactory in all cases. The recoveries of maltol and sotolon are constant (70 and 64%, respectively) and do not depend on the type of wine. On the contrary, in the case of furaneol, red wines show constant and high recoveries (97%), while the recoveries on white wines range between 30 and 80%. Different experiments showed that this behavior is probably due to the existence of complexes formed between furaneol and sulphur dioxide or catechols. Sensory experiments confirmed that the complexed forms found in white wines are not perceived by orthonasal olfaction, and that the furaneol determined by the method can be considered as the free and odor-active fraction. 相似文献
72.
Cellulose-based hydrogel materials were prepared and modified with tannic acid and l-methionine using ionic liquid as the solvent. The gels were prepared to develop a sustained release medium for selenourea (SeU). The drug delivery characteristics of selenourea-loaded cellulose (CSeU), selenourea-loaded tannic acid-modified cellulose (CTSeU), and selenourea-loaded L-methionine-modified cellulose (CMSeU) were investigated in aqueous media and simulated gastric fluid (SGF) media. This modified gel beads have been characterized using field emission scanning electron microscope, X-ray energy-dispersive spectroscopy, Fourier transform infrared spectroscopy, thermogravimetry–differential thermal analysis and swelling properties and compared with those of the unmodified ones. We also investigated the inhibitory effects of SeU released from these gels on the activity of mushroom tyrosinase. Out of all the gel materials, CTSeU showed maximum SeU release both in water and SGF media. However, tyrosinase inhibitory action in PBS medium was comparable for all the three gel materials. 相似文献
73.
《Arabian Journal of Chemistry》2020,13(8):6568-6579
In this work, the sol–gel technique was used to prepare a new organic–inorganic hybrid from Epoxidized Natural Rubber (ENR-50) and Titanium dioxide (TiO2) by blending different content of titania precursors (10, 30, and 50 wt%) with an ENR-50 matrix. A wide range of analyses was conducted to understand the nature of this hybrid and also to evaluate its potential uses in applications required high refractive index such as micro optical and optoelectronic devices. Results indicated that the ring-opening reaction of epoxide groups in ENR-50 increased with the increase of titania content in the hybrid resulting a strong bonding between titania and ENR-50 through TiOC bond, which was observed in FTIR spectrum at 1027–1028 cm−1. It is also observed a slight decrease in the intensity of the amorphous peak along with a new crystalline peak appeared at 2θ = 23 and 27° due to the crystalline nature of titania. The hybrids showed three thermal degradation steps in the range of temperature 76 to 769 °C due to the existence of the Ti moieties with the mixture of polymer chains, which in turn shifted the Tg at 24.3, 26.9 and 28.1 °C for the hybrid at 10, 30, and 50 wt% TiO2 compared to the Tg of ENR-50 at −18.4 °C respectively. The morphology of the ENR-50 showed clear changes during of the synthesis of ENR-50/TiO2 hybrids, these changes were proven by SEM, TEM, and AFM analyses. Uv–Vis results showed that the higher wavelength peak at 293 nm has shifted to 296, 298 and 300 nm for the hybrid at 10, 30, and 50 wt% TiO2 respectively due to the strong interaction between titania precursors and ENR-50 matrix. Furthermore, the hybrids showed good optical transparency in the visible light range. 相似文献
74.
Yoshihiko Ito Yoshinori Inubushi Toru Sugaya Takeo Saegusa 《Journal of organometallic chemistry》1977,137(1):1-9
Reaction of carboxamides with Cu2O in the presence of t-butyl isocyanide gave new chelated copper(I) complexes, which probably are formed by the insertion of t-butyl isocyanide into the coppernitrogen bond of copper(I) amide isonitrile complexes, which were initially produced from the carboxamides and Cu2Ot-butyl isocyanide complex. The same chelated copper(I) complexes were prepared more readily by the reaction of the corresponding N-trimethylsilyl-carboxamides with Cu2Ot-butyl isocyanide complex. Reactions of the copper(I) complexes thus obtained with alkylating agents, such as alkyl halides, alkyl tosylates and triethyloxonium tetrafluoroborate, also were described. 相似文献
75.
Jiang He Florian Rauch Dr. Alexandra Friedrich Dr. Daniel Sieh Dr. Tatjana Ribbeck Dr. Ivo Krummenacher Prof. Dr. Holger Braunschweig Prof. Dr. Maik Finze Prof. Dr. Todd B. Marder 《Chemistry (Weinheim an der Bergstrasse, Germany)》2019,25(60):13777-13784
N-heterocyclic olefins (NHOs), relatives of N-heterocyclic carbenes (NHCs), exhibit high nucleophilicity and soft Lewis basic character. To investigate their π-electron donating ability, NHOs were attached to triarylborane π-acceptors (A) giving donor (D)–π–A compounds 1 – 3 . In addition, an enamine π-donor analogue ( 4 ) was synthesized for comparison. UV–visible absorption studies show a larger red shift for the NHO-containing boranes than for the enamine analogue, a relative of cyclic (alkyl)(amino) carbenes (CAACs). Solvent-dependent emission studies indicate that 1 – 4 have moderate intramolecular charge-transfer (ICT) behavior. Electrochemical investigations reveal that the NHO-containing boranes have extremely low reversible oxidation potentials (e.g., for 3 , =−0.40 V vs. ferrocene/ferrocenium, Fc/Fc+, in THF). Time-dependent (TD) DFT calculations show that the HOMOs of 1 – 3 are much more destabilized than that of the enamine-containing 4 , which confirms the stronger donating ability of NHOs. 相似文献
76.
Purification of plasmid DNA vectors by aqueous two-phase extraction and hydrophobic interaction chromatography 总被引:4,自引:0,他引:4
The current study explores the possibility of using a polyethyleneglycol(PEG)-ammonium sulphate aqueous two-phase system (ATPS) as an early step in a process for the purification of a model 6.1 kbp plasmid DNA (pDNA) vector. Neutralised alkaline lysates were fed directly to ATPS. Conditions were selected to direct pDNA towards the salt-rich bottom phase, so that this stream could be subsequently processed by hydrophobic interaction chromatography (HIC). Screening of the best conditions for ATPS extraction was performed using three PEG molecular weights (300, 400 and 600) and varying the tie-line length, phase volume ratio and lysate load. For a 20% (w/w) lysate load, the best results were obtained with PEG 600 using the shortest tie-line (38.16%, w/w). By further manipulating the system composition along this tie-line in order to obtain a top/bottom phase volume ratio of 9.3 (35%, w/w PEG 600, 6%, w/w NH4)2 SO4), it was possible to recover 100% of pDNA in the bottom phase with a three-fold increase in concentration. Further increase in the lysate load up to 40% (w/w) with this system resulted in a eight-fold increase in pDNA concentration, but with a yield loss of 15%. The ATPS extraction was integrated with HIC and the overall process compared with a previously defined process that uses sequential precipitations with iso-propanol and ammonium sulphate prior to HIC. Although the final yield is lower in the ATPS-based process the purity grade of the final pDNA product is higher. This shows that it is possible to substitute the time-consuming two-step precipitation procedure by a simple ATPS extraction. 相似文献
77.
Zgoła-Grześkowiak A Grześkowiak T Zembrzuska J Frańska M Frański R Lukaszewski Z 《Journal of chromatography. A》2005,1068(2):327-333
In the current study a method of isotachophoretic separation of selected carboxylic acids was developed. The method was used for the determination of carboxylated oligo(ethylene glycol)s and their degradation products in biodegradation tests of PEG 250 DA [a mixture of dicarboxylated oligo(ethylene glycol)s]. Two tests were performed in the studies: the Organization for Economic Cooperation and Development (OECD) screening test and the river water die-away test. Both the biodegradation tests proved relatively fast biodegradation of the studied compounds. In the OECD screening test the biodegradation was faster than in the river water die-away test which can be ascribed to a higher concentration of bacteria in the biodegradation liquor. The minimal sample pretreatment and relatively low cost of analysis by the isotachophoretic method used here make it a good alternative to existing methods of carboxylic acids analysis. 相似文献
78.
A novel zirconia-based hybrid organic-inorganic sol-gel coating was developed for capillary microextraction (CME) (in-tube SPME). High degree of chemical inertness inherent in zirconia makes it very difficult to covalently bind a suitable organic ligand to its surface. In the present work, this problem was addressed from a sol-gel chemistry point of view. Principles of sol-gel chemistry were employed to chemically bind a hydroxy-terminated silicone polymer (polydimethyldiphenylsiloxane, PDMDPS) to a sol-gel zirconia network in the course of its evolution from a highly reactive alkoxide precursor undergoing controlled hydrolytic polycondensation reactions. A fused silica capillary was filled with a properly designed sol solution to allow for the sol-gel reactions to take place within the capillary for a predetermined period of time (typically 15-30 min). In the course of this process, a layer of the evolving hybrid organic-inorganic sol-gel polymer got chemically anchored to the silanol groups on the capillary inner walls via condensation reaction. At the end of this in-capillary residence time, the unbonded part of the sol solution was expelled from the capillary under helium pressure, leaving behind a chemically bonded sol-gel zirconia-PDMDPS coating on the inner walls. Polycyclic aromatic hydrocarbons, ketones, and aldehydes were efficiently extracted and preconcentrated from dilute aqueous samples using sol-gel zirconia-PDMDPS coated capillaries followed by thermal desorption and GC analysis of the extracted solutes. The newly developed sol-gel hybrid zirconia coatings demonstrated excellent pH stability, and retained the extraction characteristics intact even after continuous rinsing with a 0.1 M NaOH solution for 24 h. To our knowledge, this is the first report on the use of a sol-gel zirconia-based hybrid organic-inorganic coating as an extraction medium in solid phase microextraction (SPME). 相似文献
79.
《Arabian Journal of Chemistry》2020,13(1):1198-1228
Vanadate and vanadium compounds exist in many environmental, biological and clinical matrices, and despite the need only limited progress has been made on the analysis of vanadium compounds. The vanadium coordination chemistry of different oxidation states is known, and the result of the characterization and speciation analysis depends on the subsequent chemistry and the methods of analysis. Many studies have used a range of methods for the characterization and determination of metal ions in a variety of materials. One successful technique is high performance liquid chromatography (HPLC) that has been used mainly for measuring total vanadium level and metal speciation. Some cases have been reported where complexes of different oxidation states of vanadium have been separated by HPLC. Specifically reversed phase (RP) HPLC has frequently been used for the measurement of vanadium. Other HPLC methods such as normal phase, anion-exchange, cation-exchange, size exclusion and other RP-HPLC modes such as, ion-pair and micellar have been used to separate selected vanadium compounds. We will present a review that summarizes and critically analyzes the reported methods for analysis of vanadium salts and vanadium compounds in different sample matrices. We will compare various HPLC methods and modes including sample preparation, chelating reagents, mobile phase and detection methods. The comparison will allow us to identify the best analytical HPLC method and mode for measuring vanadium levels and what information such methods provide with regard to speciation and quantitation of the vanadium compounds. 相似文献
80.
《Arabian Journal of Chemistry》2022,15(3):103646
One of the most common problems in wounds is delayed healing and complications such as infection. Therefore, the need for novel materials accelerates the healing of wounds especially abdominal wounds after surgery besides high efficiency and safety is mandatory. The rate of wound healing, anti-inflammatory and biocompatibility of Zn-Al LDH (Zn-Al layer double hydroxide) alone and loaded with Curcumin (Zn-Al LDH/Curcumin) was screened via in-vivo assays through intramuscular implantation in rat abdominal wall with intact peritoneum cavity. The implanted drugs were formed through Curcumin loaded into LDH of Zn-Al with drug release of 56.78 ± 1.51% within 24 h. The synthesized nanocomposite was characterized by (TGA/DTA) thermal analysis, (XRD) X-ray diffraction, (FESEM) Field emission scanning electron microscopy, (HRTEM) high resolution transmission electron microscope, energy dispersive X-ray (EDX) and low-temperature N2 adsorption, pore volume and average pore size distribution. The integrity of blood circulation, inflammatory signs, wound healing rate, capacity of tissue integration, antigenicity and composite biocompatibility, auto fluorescence ability of collagen bundles and the tensile strength of the muscle were assessed histopathologically after 7 and 30 days’ post-implantation. Excellent wound healing ability was achieved with shortest length between the wound gap edges and higher tensile strength of the muscle. Besides emit florescence very well followed by good healing and tensile muscles strength in Curcumin while very low strength with scar formation in Zn-Al LDH/Curcumin in both acute and chronic wound. No signs of inflammation in Curcumin & Zn-Al LDH. No vessels obstruction or bleeding observed in both Zn-Al LDH and Curcumin more than Zn-Al LDH/Curcumin and control which examined through candling. Good healing & infiltrated immune cells in same groups through histopathological examination. This work supports the anti-inflammatory, wound healing and biocompatibility of both LDH and Curcumin with living matter, increasing their biomedical applications in this era with safety and increasing efficacy with prolonged drug release. 相似文献