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ACN/methanol Mixture (methanol + mixture)
Selected AbstractsAnalyses of alkaloids in different products by NACE-MSELECTROPHORESIS, Issue 22 2007Chen-Wen Chiu Abstract A simple method for the separation and characterization of five nicotine-related alkaloids by NACE employing UV and MS detections is described here for the first time. Several factors, including NACE parameters (compositions of running solution) and MS parameters (such as nature and flow rate of sheath liquid, pressure of nebulization gas, and flow rate of dry gas), were optimized in order to obtain both an adequate CE separation and high MS signals for the alkaloid compounds used in this study. A reliable CE separation of five alkaloids was achieved in 50,mM ammonium formate that was dissolved in an ACN/methanol mixture (50:50, v/v) of pH*,4.0 (apparent pH 4.0). The optimal electrospray MS measurement was carried out in the positive ionization mode using a coaxial sheath liquid composed of isopropyl alcohol and water in the ratio of 80:20 v/v at a flow rate of 180,,L/h. In addition, the proposed NACE method was also applied in the analyses of alkaloids in several products including chewing gums, beverages, and tobaccos. This NACE-MS method was found to provide a better detection ability and separation resolution for the analysis of nicotine alkaloids when compared to other aqueous CE-MS reports. [source] Preparation of novel ZSM-5 zeolite-filled chitosan membranes for pervaporation separation of dimethyl carbonate/methanol mixturesJOURNAL OF APPLIED POLYMER SCIENCE, Issue 3 2007Bingbing Liu Abstract Novel mixed matrix membranes were prepared by incorporating ZSM-5 zeolite into chitosan polymer for the pervaporative separation of dimethyl carbonate (DMC) from methanol. These membranes were characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and X-ray diffraction (XRD) to assess their morphology, intermolecular interactions, and crystallinity. Sorption studies indicated that the degree of swelling for zeolite-filled membranes increased with zeolite content in the membrane increasing and the separation selectivity of DMC/methanol was dominated by solubility selectivity rather than diffusivity selectivity. The characteristics of these membranes for separating DMC/methanol mixtures were investigated by varying zeolite content, feed composition, and operating temperature. The pervaporation separation index (PSI) showed that 5 wt % of ZSM-5 zeolite-filled membrane gave the optimum performance in the PV process. From the temperature-dependent permeation values, the Arrhenius activation parameters were estimated. The resulting lower activation energy values obtained for zeolite-filled membranes contribute to the framework of the zeolite. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007 [source] A TRLFS Study on the Complexation of CmIII and EuIII with 2,6-Bis(5,6-dipropyl-1,2,4-triazin-3-yl)pyridine in Water/Methanol MixtureEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 19 2010Sascha Trumm Abstract The complexation of CmIII and EuIII with 2,6-bis(5,6-dipropyl-1,2,4-triazin-3-yl)pyridine (nPr-BTP) in water/methanol solution is studied. 1:3 complexes [M(nPr-BTP)3]3+ form from the solvated metal ions upon addition of ligand. The conditional stability constants are log,K = 14.4 and log,K = 11.9. For both metal ions the complexation reaction is both enthalpy and entropy driven. ,H is 10.1 kJ/mol more negative than ,H, whereas the entropy difference is small. The difference in ,G between the formation of the CmIII and EuIII complexes is in good agreement with nPr-BTP's selectivity in liquid-liquid extraction. [source] Study of the bio-production of carotenoids by Sporidiobolus salmonicolor (CBS 2636) using pre-treated agro-industrial substratesJOURNAL OF CHEMICAL TECHNOLOGY & BIOTECHNOLOGY, Issue 9 2008Eunice Valduga Abstract BACKGROUND: The increasing industrial demand for carotenoids has aroused interest in their bio-production, and the need to reduce production costs has encouraged the use of low cost industrial substrates, such as agro-industrial residues. Thus the objective of this research was the bio-production of carotenoids by Sporidiobolus salmonicolor using agro-industrial substrates (corn steep liquor and sugarcane molasses), pre-treated with acids (sulphuric and phosphoric). RESULTS: Bio-production was carried out in an orbital shaker using a 10% (v/v) inoculum, incubation at 25 °C, and agitation at 180 rpm for 120 h in a non-illuminated environment. The carotenoids were recovered using liquid N2 combined with dimethylsulphoxide for cell rupture, and an acetone/methanol mixture (7:3 v/v) for extraction. CONCLUSION: The complete second-order design allowed for optimisation of the carotenoid concentration obtained from industrial substrates pre-treated with acids (sulphuric and phosphoric), obtaining a total carotenoid content of 541.5 µg L,1 using 10 g L,1 sugarcane molasses, 5 g L,1 corn steep liquor and 5 g L,1 yeast hydrolysate at 25 °C, with agitation at 180 rpm and an initial pH of 4.0. Copyright © 2008 Society of Chemical Industry [source] Hypericum perforatum,Chemical profiling and quantitative results of St. John's Wort products by an improved high-performance liquid chromatography methodJOURNAL OF PHARMACEUTICAL SCIENCES, Issue 3 2002M. Ganzera Abstract The analysis of flavonoids, naphthodianthrones, and the phloroglucinol derivative hyperforin in H. perforatum is described in this article. In a 35-min HPLC run nine major compounds could be identified and baseline separated in the methanolic plant extracts. For an optimum separation the mobile phase consisted of 10 mM ammonium acetate buffer (pH 5.0) and an acetonitrile/methanol mixture; a Synergi MAX-RP 80 Ĺ column (C-12 material) was used as stationary phase. Detection was performed at 270 nm, and the identity of the compounds was confirmed in an LC-MS experiment. Commercial St. John's Wort products were analyzed and qualitative and quantitative results are discussed. © 2002 Wiley-Liss, Inc. and the American Pharmaceutical Association J Pharm Sci 91:623,630, 2002 [source] Cascade Reactions: Catalytic Synthesis of Functionalized 1,3-Dihydroisobenzofuran and Tetrahydrofuran Derivatives by Sequential Nucleophilic Ring Opening,Heterocyclization, Oxidative Carbonylation of AlkynyloxiranesADVANCED SYNTHESIS & CATALYSIS (PREVIOUSLY: JOURNAL FUER PRAKTISCHE CHEMIE), Issue 14-15 2009Nicola Della Ca' Abstract Differently substituted alkynyloxiranes were efficiently converted into functionalized 1,3-dihydroisobenzofurans and tetrahydrofuran derivatives in fair to good yields by a new cascade reaction, consisting of a sequential nucleophilic ring opening,heterocyclization,oxidative carbonylation process. Reactions were carried out at 80,100,°C and under a 3:1 mixture of carbon monoxide and air (total pressure=32,42,atm at 25,°C) in methanol or acetonitrile/methanol mixtures in the presence of catalytic amounts of palladium diiodide in conjunction with an excess of potassium iodide. The nucleophilic species beginning the cascade process by regioselective attack to the less hindered carbon of the oxirane ring can be methanol itself or iodide anions. [source] Novel Thorium Membrane Sensors with Anionic Response Based on Trioctylphosphine Oxide and Toluate IonophoresELECTROANALYSIS, Issue 19 2008Abstract Two novel potentiometric polymeric membrane sensors for rapid and accurate determination of thorium are described. These are based on the use of trioctylphosphine oxide (TOPO) and thorium toluate (Th-TA) as ionophores dispersed in poly(vinyl chloride) matrix membranes plasticized with nitrophenyloctyl ether. In strong nitric acid medium, Th(IV) nitrate is converted into [Th(NO3)6]2, complex and sensed as anionic divalent ion which exclude most cationic effect. Validation of the assay methods using the quality assurance standards (linearity range, accuracy, precision, within-day variability, between-day-repeatability, lower detection limit and sensitivity) reveals excellent performance characteristics of both sensors. The sensors exhibit near-Nernstian response for 1.0×10,6,1.0×10,1 M Th over the pH range 2.5,4.5. Calibration slopes of ,32.3±0.3 and ,27.2±0.2,mV/decade, precision of ±0.5 and ±0.8% and accuracy of 98.8±0.9 and 97.9±0.7% are obtained with TOPO and Th-TA based sensors, respectively. Negligible interferences are caused by most interfering mono-, di-, tri-, tetra-, penta-, and hexa-valent elements commonly associated with thorium in naturally occurring minerals and ores. High concentrations of Cl,, F,, SO42,, and NO3, ions have no diverse effect. Complete removal of the effect of the interferents in complex matrices is achieved by retention of [Th(NO3)6]2, complex from 5,M nitric acid/methanol mixture (1,:,9,v/v) on a strong anion exchanger, washing out the cationic interferents followed by stripping off thorium anion complex and measurements. Both sensors are used for determining thorium in certified thorium ore samples (20,120,mg Th/kg) and some naturally occurring ores (200,600,mg Th/kg). The results obtained agree fairly well with the certified labeled values or the data obtained using X-ray fluorescence spectrometry [source] Determination of urinary S -phenylmercapturic acid, a specific metabolite of benzene, by liquid chromatography/single quadrupole mass spectrometryRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 9 2005Luciano Maestri A high-performance liquid chromatography/single quadrupole mass spectrometry (LC/MS) method is described for the determination of urinary S -phenylmercapturic acid (S-PMA), a specific metabolite of benzene. Urine samples were spiked with [13C6]S-PMA (used as the internal standard) and acidified; then they were purified by solid-phase extraction (SPE) on C18 cartridges. Analyses were conducted on a reversed-phase column by gradient runs with 1% aqueous acetic acid/methanol mixtures at different proportions as the mobile phase. The detector was used in electrospray negative ion mode (ESI,), the ions m/z 238 for S-PMA and 244 for [13C6]S-PMA being recorded simultaneously. The detection limit (for a signal-to-noise ratio,=,3) was 0.2,,g/L, thus allowing for the measurement of background excretion of S-PMA in the general population. The use of the internal standard allowed us to obtain good precision (CV% values <3%) and a linear calibration curve within the range of interest for monitoring occupational exposure to benzene (up to 500,,g/L). The method was applied to assay the metabolite concentration in a group of 299 workers (68 smokers and 231 non-smokers) occupationally exposed to relatively low levels of benzene (environmental concentration,=,0.4,220,,g/m3, mean 11.4,,g/m3) and 236 non-exposed subjects (134 smokers and 102 non-smokers). The results clearly showed that smoking must be taken into account for the correct interpretation of the results of S-PMA measurements for the assessment of work-related benzene exposure. When only non-smokers were selected, the mean excretion of S-PMA was significantly higher in workers exposed to benzene (1.2,±,0.9,,g/g creatinine) than in the control group (0.7,±,0.6,,g/g creatinine) (p,<,0.001), thus confirming the role of S-PMA as a biomarker of benzene on a group basis, even for relatively low exposure degrees. Copyright © 2005 John Wiley & Sons, Ltd. [source] Preparation of novel ZSM-5 zeolite-filled chitosan membranes for pervaporation separation of dimethyl carbonate/methanol mixturesJOURNAL OF APPLIED POLYMER SCIENCE, Issue 3 2007Bingbing Liu Abstract Novel mixed matrix membranes were prepared by incorporating ZSM-5 zeolite into chitosan polymer for the pervaporative separation of dimethyl carbonate (DMC) from methanol. These membranes were characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and X-ray diffraction (XRD) to assess their morphology, intermolecular interactions, and crystallinity. Sorption studies indicated that the degree of swelling for zeolite-filled membranes increased with zeolite content in the membrane increasing and the separation selectivity of DMC/methanol was dominated by solubility selectivity rather than diffusivity selectivity. The characteristics of these membranes for separating DMC/methanol mixtures were investigated by varying zeolite content, feed composition, and operating temperature. The pervaporation separation index (PSI) showed that 5 wt % of ZSM-5 zeolite-filled membrane gave the optimum performance in the PV process. From the temperature-dependent permeation values, the Arrhenius activation parameters were estimated. The resulting lower activation energy values obtained for zeolite-filled membranes contribute to the framework of the zeolite. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007 [source] Unusual atmospheric pressure chemical ionization conditions for detection of organic peroxidesJOURNAL OF MASS SPECTROMETRY (INCORP BIOLOGICAL MASS SPECTROMETRY), Issue 9 2003David Rondeau Abstract Organic peroxides such as the cumene hydroperoxide I (Mr = 152 u), the di- tert -butyl peroxide II (Mr = 146 u) and the tert -butyl peroxybenzoate III (Mr = 194 u) were analyzed by atmospheric pressure chemical ionization mass spectrometry using a water,methanol mixture as solvent with a low flow-rate of mobile phase and unusual conditions of the source temperature (,50 °C) and probe temperature (70,200 °C). The mass spectra of these compounds show the formation of (i) an [M + H]+ ion (m/z 153) for the hydroperoxide I, (ii) a stable adduct [M + CH3OH2]+ ion (m/z 179) for the dialkyl peroxide II and (iii) several protonated adduct species such as protonated molecules (m/z 195) and different protonated adduct ions (m/z 227, 389 and 421) for the peroxyester III. Tandem mass spectrometric experiments, exact mass measurements and theoretical calculations were performed for characterize these gas-phase ionic species. Using the double-well energy potential model illustrating a gas-phase bimolecular reaction, three important factors are taken into account to propose a qualitative interpretation of peroxide behavior toward the CH3OH2+, i.e. thermochemical parameters () and two kinetic factors such as the capture constant of the initial stable ion,dipole and the magnitude of the rate constant of proton transfer reaction into the loose proton bond cluster. Copyright © 2003 John Wiley & Sons, Ltd. [source] Secondary conformation of short lysine- and leucine-rich peptides assessed by optical spectroscopies: Effect of chain length, concentration, solvent, and timeBIOPOLYMERS, Issue 1 2006Belén Hernández Abstract Solution secondary structures of three synthetic cationic peptides, currently used in antisense oligonucleotide delivery into living cells, have been analyzed by means of circular dichroism (CD) and Raman scattering in different buffers as a function of concentration and time. All three peptides are of minimalist conception, i.e., formed by only two types of amino acids (leucine: L and lysine: K). Two of these peptides contain 15 aminoacids: Nter - KLLKLLLKLLLKLLK (L10K5), Nter -KLKLKLKLKLKLKLK (L7K8), and the third one has only 9 residues: Nter -KLKLKLKLK (L4K5). The conformational behavior of the 15-mers in pure water differs considerably one from another. Although both of them are initially disordered in the 50,350 ,M range, L10K5 gradually undergoes a disordered to , -helix transition for molecular concentrations above 100 ,M. In all other solvents used, L10K5 adopts a stable , -helical conformation. In methanol and methanol/Tris mixture, nonnative , -helices can be induced in both KL-alternating peptides, i.e., L7K8 and L4K5. However, in major cases and with a time delay depending on peptide concentration, , -like structures can be gradually formed in both solutions. In PBS and methanol/PBS mixture, the tendency for L7K8 and L4K5 is to form structures belonging to , -family. A discussion has been undertaken on the effect of counterions as well as their nature in the stabilization of ordered structures in both KL-alternating peptides. © 2005 Wiley Periodicals, Inc. Biopolymers 81: 8,19, 2006 This article was originally published online as an accepted preprint. The "Published Online" date corresponds to the preprint version. You can request a copy of the preprint by emailing the Biopolymers editorial office at biopolymers@wiley.com [source] Synthesis of PEDOT Nanoparticles and Vesicles by Dispersion Polymerization in Alcoholic MediaMACROMOLECULAR RAPID COMMUNICATIONS, Issue 17 2006Muhammad Mumtaz Abstract Summary: The synthesis of PEDOT nanoparticles and vesicles by dispersion polymerization in a methanol/water mixture (3/2, v/v) is reported, using either ammonium persulfate or iron(III) p -toluenesulfonate as oxidants and , -EDOT-PEO as a reactive stabilizer. The influence of the oxidant as well as the , -EDOT-PEO molar mass and concentration on the core-shell particle morphology and conductivity properties have been investigated. PEDOT particles with conductivities up to 1.5,×,10,2 S,·,cm,1 have been obtained in high yield. TEM image of PEDOT vesicles prepared using PEO-based stabilizers of 25,000 g,·,mol,1 in water/methanol mixture (2:3 v/v) at room temperature using ammonium persulfate as an oxidant. [source] Selective preconcentration of volatile mercaptans in small SPE cartridges: Quantitative determination of trace odor-active polyfunctional mercaptans in wineJOURNAL OF SEPARATION SCIENCE, JSS, Issue 21 2009Laura Mateo-Vivaracho Abstract A general procedure for the selective preconcentration and purification of mercaptans has been developed. Mercaptans are strongly retained in a small (20,mg) SPE cartridge containing p- hydroxymercurybenzoate. The cartridge can then be rinsed with relatively high volumes of polar (water/methanol mixtures) and non-polar (pentane or pentane/ether mixtures) rinsing solutions to remove nearly all volatile compounds lacking a thiol functionality. Retained analytes are further eluted with a small volume of an organic solvent containing 1,4-dithioerythritol. Some basic aspects of the strategy, such as the retention of p -hydroxymercurybenzoate in the sorbent and its stability versus different rinsing and eluting systems, have been studied in depth. Light sulfur compounds contained in water or wine, including mercaptans such as methanethiol or thioethers, such as diethyl sulfide, can be quantitatively extracted, although only mercaptans can be quantitatively recovered if a polar rinsing is applied. The strategy has been applied to the GC-MS quantitative determination of some trace polyfunctional mercaptans that are key aromas in wine, such as 2-methyl-3-furanthiol, 2-furfurylthiol, 4-mercapto-4-methyl-2-pentanone, 3-mercaptohexyl acetate or 3-mercaptohexanol. The developed method reaches detection limits in the ng/L range and has a satisfactory analytical behavior, being quite simple and fast. [source] | |||||||||||||