Home About us Contact
|
Home About us Contact | ||
|
|
||
Sodium Acetate (sodium + acetate)
Kinds of Sodium Acetate Terms modified by Sodium Acetate Selected AbstractsSodium acetate enhances hydrogen peroxide production in Weissella cibariaLETTERS IN APPLIED MICROBIOLOGY, Issue 1 2009A. Endo Abstract Aims:, To investigate hydrogen peroxide production by lactic acid bacteria (LAB) and to determine the key factors involved. Methods and Results:, Six strains of Weissella cibaria produced large amounts (2·2,3·2 mmol l,1) of hydrogen peroxide in GYP broth supplemented with sodium acetate, but very low accumulations in glucose yeast peptone broth without sodium acetate. Increased production of hydrogen peroxide was also recorded when strains of W. cibaria were cultured in the presence of potassium acetate, sodium isocitrate and sodium citrate. Oxidases and peroxidases were not detected, or were present at low levels in W. cibaria. However, strong nicotinamide adenine dinucleotide (NADH) oxidase activity was recorded, suggesting that the enzyme plays a key role in production of hydrogen peroxide by W. cibaria. Conclusions:,Weissella cibaria produces large quantities of hydrogen peroxide in aerated cultures, in a process that is dependent on the presence of acetate in the culture medium. NADH oxidase is likely the key enzyme in this process. Significance and Impact of the Study:, This is the first study showing that sodium acetate, normally present in culture media of LAB, is a key factor for hydrogen peroxide production by W. cibaria. The exact mechanisms involved are not known. [source] Optimisation of the headspace-solid phase microextraction for organomercury and organotin compound determination in sediment and biotaJOURNAL OF SEPARATION SCIENCE, JSS, Issue 4 2008Alejandra Delgado Abstract Headspace solid-phase microextraction was optimised for the simultaneous preconcentration of methylmercury (MeHg+), monobutyltin, dibutyltin, tributyltin, monophenyltin (MPhT), diphenyltin (DPhT), and triphenyltin (TPhT) from sediments and biota. Extraction time (3,24 min), extraction temperature (20,90°C), desorption time (1,10.4 min), desorption temperature (152,260°C), and sample volume (5,22 mL) were simultaneously optimised, while variables such as fibre type (30 ,m polydimethylsiloxane, PDMS), pH (acetic acid/sodium acetate, HOAc/NaOAc, 2 mol/L, pH , 4.8), the concentration of the derivatisation agent (sodium tetraethylborate, NaBEt4, 0.1% m/v), and the ionic strength (fixed by the buffer solution) were kept constant. The variables were optimised according to the experiments proposed by the MultiSimplex program and the responses were considered in order to establish the optimum conditions. The repeatability (relative standard deviation, RSD, 5,20.6%) and limits of detection (LODs, 0.05,0.97 ng/g) of the overall method were also estimated. The lowest precisions were obtained for DPhT and TPhT. The optimised preconcentration method was applied to the determination of MeHg+, butyl- and phenyltins in certified reference materials (IAEA-405 MeHg+ in estuarine sediment, BCR-646 butyl- and phenyltins in marine sediment, BCR-463 MeHg+ in tuna fish, DOLT-2 MeHg+ in dogfish liver, and BCR-477 butyltins in mussel tissue) by GC with microwave-induced plasma/atomic-emission detection. [source] Combined use of chiral ionic liquid and cyclodextrin for MEKC: Part I. Simultaneous enantioseparation of anionic profensELECTROPHORESIS, Issue 16 2009Bin Wang Abstract The enantiomers of five profen drugs were simultaneously separated by MEKC with the combined use of 2,3,6-tri- O -methyl-,-cyclodextrin and chiral cationic ionic liquid, N -undecenoxy-carbonyl- L -leucinol bromide, which formed micelles in aqueous buffers. Enantioseparations of these profen drugs were optimized by varying the chain length and concentration of the IL surfactant using a standard recipe containing 35,mM 2,3,6-tri- O -methyl-,-cyclodextrin, 5,mM sodium acetate at pH 5.0. The batch-to-batch reproducibility of N -undecenoxy-carbonyl- L -leucinol bromide was tested and found to have no significant impact in terms of enantiomeric resolution, efficiency, and migration time. Finally, this method was successfully applied for the quantitative determination of ibuprofen in pharmaceutical tablets. [source] Hydrido-Osmium(II), -Osmium(IV) and-Osmium(VI) Complexes with Functionalized Phosphanes as Ligands,EUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 35 2009Birgit Richter Abstract Reaction of five-coordinate [OsHCl(CO)(PiPr3)2] (1) with the chelating phosphane iPr2PCH2CO2Me gave six-coordinate [OsHCl(CO)(PiPr3){,2(P,O)- iPr2PCH2C(=O)OMe}] (2), which upon treatment with CO and O2 afforded the 1:1 adducts [OsHCl(CO)(L)(PiPr3){,(P)- iPr2PCH2CO2Me}] (3, 4) by partial opening of the chelate ring. The vinyl complex [OsCl(CH=CHPh)(CO)(PiPr3){,2(P,O)- iPr2PCH2C(=O)OMe}] (5) was obtained from 2 and PhC,CH by insertion of the alkyne into the Os,H bond. Reaction of 2 with sodium acetate led to metathesis of the anionic ligands and formation of [OsH(,2 -O2CCH3)(CO)(PiPr3){,(P)- iPr2PCH2CO2Me}] (6). Osmium(VI) compounds [OsH6(PiPr2R)2] with R = CH2CH2OMe (12), CH2CO2Me (13) and CH2CO2Et (14), and [OsH6(PiPr3){,(P)- iPr2PCH2CH2NMe2}] (16) were prepared from osmium(IV) precursors and shown to rapidly react with O2 and primary alcohols. Exploratory studies revealed that the catalytic activity of the hexahydrido complexes in the hydrogen transfer reaction from 2-propanol to cyclohexanone and acetophenone depends on the type of the functionalized phosphane and is best for R = CH2CH2OMe. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2009) [source] Heterocyclic synthesis containing bridgehead nitrogen atom: Synthesis of 3-[(2H)-2-oxobenzo[b]pyran-3-yl]- s -triazolo[3,4- b]-1,3,4-thiadiazine and thiazole derivativesHETEROATOM CHEMISTRY, Issue 2 2003M. A. Raslan The reaction of 2H-2-oxobenzo[b]pyran-3-hydrazide (2) with carbon disulfide in basic DMF afforded potassium thiocarbamate 3, which readily underwent heterocyclization upon its reaction with hydrazine and/or phenacyl bromide to yield 1,2,4-tiazole (4) and thiazole 7 derivatives, respectively. Condensation of 4 with substituted phenacyl bromide and/or chloranil gave 1,2,4-triazole[3,4-b]thiadiazine (5a,b) and 3,10-bis-[2H-2-oxobenzo[b]pyran-3-yl]-6,13-dichloro-bis-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazino[5,,6,-b:5,,6,-e]cyclohexa-1,4-diene (6), respectively. Cyclization of thiosemicarbazide 10 by refluxing it in sodium hydroxide and/or phosphoryl chloride afforded triazole 13 and thiadiazole 15 derivatives, respectively. Also, 10 reacted with phenacyl bromide in the presence of anhydrous sodium acetate to give the oxothiazolidine derivative 17. The structure of the synthesized compounds were confirmed by elemental analyses, IR, 1H NMR, and mass spectra. © 2003 Wiley Periodicals, Inc. Heteroatom Chem 14:114,120, 2003; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/hc.10109 [source] Microwave-assisted depolymerization of poly(ethylene terephthalate) [PET] at atmospheric pressureADVANCES IN POLYMER TECHNOLOGY, Issue 4 2006Mir Mohammad Alavi Nikje Abstract Microwave-assisted hydroglycolysis of poly(ethylene terephthalate) using an excess of methanol, ethanol, 1-butanol, 1-pentanol, and 1-hexanol in the presence of different simple basic catalysts, namely, potassium hydroxide, sodium hydroxide, sodium acetate, and zinc acetate, is reported. Reactions were performed at short times without any side reactions, namely, oxidation of ethylene glycol. The products terephthalic acid and ethylene glycol were obtained in their pure form with sufficiently high yields with potassium hydroxide. The purified product was characterized by IR and nuclear magnetic resonance spectroscopy. The process of hydroglycolysis reported here is economically viable since yields of recycled products are high, and it has potential for further improvement to produce useful products. This process is of economic interest because much of the raw materials can be recovered and used for virgin PET resin synthesis. © 2007 Wiley Periodicals, Inc. Adv Polym Techn 25:242,246, 2006; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/adv.20080 [source] Different combinations of salts affect the growth and bacteriocin production by Lactobacillus salivarius CRL 1328JOURNAL OF CHEMICAL TECHNOLOGY & BIOTECHNOLOGY, Issue 1 2010María Silvina Juárez Tomás Abstract BACKGROUND: The culture medium for optimal growth of vaginal Lactobacillus salivarius CRL 1328 is different from that for optimal bacteriocin production. To simultaneously obtain high amount of biomass and bacteriocin of this microorganism, the effects of different basal culture media and salts on both responses were evaluated. The study was performed by using a complete factorial experimental design 26, with central points. Sixty-four different growth media, which resulted from the combinations of two basal culture media and two concentrations of five salts (ammonium citrate, sodium acetate, MgSO4, MnSO4, and K2HPO4) were assayed. RESULTS: Only the addition of MnSO4 to each culture medium significantly stimulated the growth of L. salivarius. The presence of sodium acetate or MgSO4 stimulated the bacteriocin production, while MnSO4 and K2HPO4 exerted an inhibitory effect. However, the simultaneous addition of MnSO4 and sodium acetate to both basal culture media allowed high bacteriocin levels to be reached, attenuating the inhibitory effect of Mn2+. CONCLUSIONS: The application of a complete experimental design contributed to simultaneous optimization of the biomass and bacteriocin production of L. salivarius CRL 1328. The results obtained are potentially applicable to the technological production of probiotic bacteria and antagonistic substance to be included in a probiotic pharmaceutical product. Copyright © 2009 Society of Chemical Industry [source] Synthesis, characterization and studies of new 3-benzyl-4H -1,2,4-triazole-5-thiol and thiazolo[3,2- b][1,2,4]triazole-5(6H)-one heterocyclesJOURNAL OF HETEROCYCLIC CHEMISTRY, Issue 3 2008Abdelwareth A. O. Sarhan 3-Benzyl-4-phenyl-1,2,4-triazole-5-thiol (1) was synthesized and used as starting material for preparation of 1,2,4-triazole bearing substituted thiosemicarbazides moiety (4a-d) in high yields. The thiosemicarbazides 4a-d were cyclized in basic medium to give two triazole rings linked by thiomethylene group (5a-d), while cyclization of thiosemicarbazides 4a-d with chloroacetyl chloride in the presence of CHCl3 and K2CO3 afforded the thiazolidinone derivatives 6a-d. The reaction of thiosemicarbazides 4a-c with phenacyl bromide in the presence of EtOH and fused CH3COONa gave the corresponding thiazoline ring systems 7a-c. Condensation of the 3-benzyl-1,2,4-triazole-5(1H)-thiol (1) with chloroacetic acid and aromatic aldehydes (8a- g) in boiling acetic acid/acetic anhydride mixture in the presence of fused sodium acetate gave one single isomer only, which might be 9a-g or 10a-g. Upon application of Micheal addition reaction on compounds 9a-e with cyclic secondary amines such as piperidine or morpholine the 2-benzyl-6-(,-amino-aryl/methyl)-1,3-thiazolo[3,2- b][1,2,4]-triazol-5-ols (11a-j) were obtained in good yields The structure of all new compounds were determined using both spectral and elemental analyses. [source] Studies with enamines: Reactivity of N,N -dimethyl- N -[(E)-2-(4-nitrophenyl)-1-ethenyl]amine towards nitrilimine and aromatic diazonium saltsJOURNAL OF HETEROCYCLIC CHEMISTRY, Issue 3 2007Hamad M. Al-Matar In the presence of triethylamine, cycloaddition reaction of enamine 1 with hydrazonoyl halides 2 followed by dimethylamine elimination was achieved, yielding the corresponding 1,3,4-trisubstituted pyrazoles 4. Coupling of enamine 1 with aromatic diazonium salts afforded 2-(arylhydrazono)-2-(4-nitrophenyl)acetaldehyde 9 in good yield. Refluxing the phenyl hydrazone 9a with chloroacetone in ethanol in the presence of triethylamine afforded 1,3,5-trisubstituted pyrazole 12a, formed via intermediate 11a. Reaction of 9a with hydroxylamine hydrochloride in ethanol in the presence of anhydrous sodium acetate yielded oxime 13a which was irradiated in a microwave oven in the presence of acetic acid to afford a mixture of 15a and 16a. [source] Ring transformations of heterocyclic compounds.JOURNAL OF HETEROCYCLIC CHEMISTRY, Issue 2 2002The synthesis of pyrido[1,2- a]indolium perchlorates 8,11 from 2,4,6-triarylpyrylium perchlorates 1 and 2-methyl-3H -indoles 6,9 in the presence of a basic condensing agent (anhydrous sodium acetate, piperidine acetate, triethylamine/acetic acid, triethylamine) in ethanol by a 2,4-[C3+C2N] pyrylium ring transformation is reported. Spectroscopic data of the transformation products and their mode of formation are discussed. [source] Determination of BAPTA-AM, the acetoxymethyl tetraester of BAPTA, in rat plasma by liquid chromatography tandem mass spectrometryJOURNAL OF MASS SPECTROMETRY (INCORP BIOLOGICAL MASS SPECTROMETRY), Issue 12 2006Feng Zheng Abstract BAPTA-AM is the acetoxymethylester of the calcium chelator BAPTA and has demonstrated efficacy in several animal models of cerebral ischemia. This paper describes the development of a method for the determination of BAPTA-AM in rat plasma by liquid chromatography/tandem mass spectrometry. Owing to multiple ester groups in the structure of BAPTA-AM, [M + Na]+ was chosen as the analytical ion for quantification of BAPTA-AM. During the analytical method development, a high percentage of organic solvent and the addition of an amount of sodium acetate and formic acid in the mobile phase were found to favor the sensitivity and reproducibility of [M + Na]+. Poor fragmentation was usually observed in the MS/MS spectra of sodium adduct ions. However, abundant and reproducible fragment ions were observed for the BAPTA-AM sodium adduct ion, and therefore the traditional selective reaction-monitoring mode was used to further improve the sensitivity of MS detection. Because of the lability of the ester bond, a combination of fluoride and hydrochloric acid was applied to minimize the enzymatic hydrolysis, and acetonitrile was chosen to avoid the chemical hydrolysis or solvolysis during the sample collection and preparation procedure. On the basis of these studies, a rapid, sensitive and reproducible method for the determination of BAPTA-AM in rat plasma, using LC/ESI-MS/MS and a simple protein precipitation procedure, was developed and validated. Also, the present method was successfully applied to the determination of BAPTA-AM plasma concentrations for pharmacokinetic studies in rats. Copyright © 2006 John Wiley & Sons, Ltd. [source] Alterations in Brain Glucose Utilization Accompanying Elevations in Blood Ethanol and Acetate Concentrations in the RatALCOHOLISM, Issue 2 2010Robert J. Pawlosky Background:, Previous studies in humans have shown that alcohol consumption decreased the rate of brain glucose utilization. We investigated whether the major metabolite of ethanol, acetate, could account for this observation by providing an alternate to glucose as an energy substrate for brain and the metabolic consequences of that shift. Methods:, Rats were infused with solutions of sodium acetate, ethanol, or saline containing 13C-2-glucose as a tracer elevating the blood ethanol (BEC) and blood acetate (BAcC) concentrations. After an hour, blood was sampled and the brains of animals were removed by freeze blowing. Tissue samples were analyzed for the intermediates of glucose metabolism, Krebs' cycle, acyl-coenzyme A (CoA) compounds, and amino acids. Results:, Mean peak BEC and BAcC were approximately 25 and 0.8 mM, respectively, in ethanol-infused animals. Peak blood BAcC increased to 12 mM in acetate-infused animals. Both ethanol and acetate infused animals had a lower uptake of 13C-glucose into the brain compared to controls and the concentration of brain 13C-glucose-6-phosphate varied inversely with the BAcC. There were higher concentrations of brain malonyl-CoA and somewhat lower levels of free Mg2+ in ethanol-treated animals compared to saline controls. In acetate-infused animals the concentrations of brain lactate, ,-ketoglutarate, and fumarate were higher. Moreover, the free cytosolic [NAD+]/[NADH] was lower, the free mitochondrial [NAD+]/[NADH] and [CoQ]/[CoQH2] were oxidized and the ,G, of ATP lowered by acetate infusion from ,61.4 kJ to ,59.9 kJ/mol. Conclusions:, Animals with elevated levels of blood ethanol or acetate had decreased 13C-glucose uptake into the brain. In acetate-infused animals elevated BAcC were associated with a decrease in 13C-glucose phosphorylation. The co-ordinate decrease in free cytosolic NAD, oxidation of mitochondrial NAD and Q couples and the decrease in ,G, of ATP was similar to administration of uncoupling agents indicating that the metabolism of acetate in brain caused the mitochondrial voltage dependent pore to form. [source] Cotinine as a biomarker of tobacco exposure: Development of a HPLC method and comparison of matricesJOURNAL OF SEPARATION SCIENCE, JSS, Issue 4-5 2010Guilherme Oliveira Petersen Abstract Tobacco dependence reaches one-third of the world population, and is the second leading cause of death around the world. Cotinine, a major metabolite of nicotine, is the most appropriate parameter to evaluate tobacco exposure and smoking status due to its higher stability and half-life when compared to nicotine. The procedure involves liquid,liquid extraction, separation on a RP column (Zorbax® XDB C8), isocratic pump (0.5,mL/min of water,methanol,sodium acetate (0.1,M),ACN (50:15:25:10, v/v/v/v), 1.0,mL of citric acid (0.034,M) and 5.0,mL of triethylamine for each liter) and HPLC-UV detection (261,nm). The analytical procedure proved to be sensitive, selective, precise, accurate and linear (r>0.99) in the range of 5,500.0,ng/mL for cotinine. 2-Phenylimidazole was used as the internal standard. The LOD was 0.18,ng/mL and the LOQ was 5.0,ng/mL. All samples from smoking volunteers were collected simultaneously to establish a comparison between serum, plasma, and urine. The urinary cotinine levels were normalized by the creatinine and urine density. A significant correlation was found (p<0.01) between all matrices. Results indicate that the urine normalization by creatinine or density is unnecessary. This method is considered reliable for determining cotinine in serum and plasma of smokers and in environmental tobacco smoke exposure. [source] Sodium acetate enhances hydrogen peroxide production in Weissella cibariaLETTERS IN APPLIED MICROBIOLOGY, Issue 1 2009A. Endo Abstract Aims:, To investigate hydrogen peroxide production by lactic acid bacteria (LAB) and to determine the key factors involved. Methods and Results:, Six strains of Weissella cibaria produced large amounts (2·2,3·2 mmol l,1) of hydrogen peroxide in GYP broth supplemented with sodium acetate, but very low accumulations in glucose yeast peptone broth without sodium acetate. Increased production of hydrogen peroxide was also recorded when strains of W. cibaria were cultured in the presence of potassium acetate, sodium isocitrate and sodium citrate. Oxidases and peroxidases were not detected, or were present at low levels in W. cibaria. However, strong nicotinamide adenine dinucleotide (NADH) oxidase activity was recorded, suggesting that the enzyme plays a key role in production of hydrogen peroxide by W. cibaria. Conclusions:,Weissella cibaria produces large quantities of hydrogen peroxide in aerated cultures, in a process that is dependent on the presence of acetate in the culture medium. NADH oxidase is likely the key enzyme in this process. Significance and Impact of the Study:, This is the first study showing that sodium acetate, normally present in culture media of LAB, is a key factor for hydrogen peroxide production by W. cibaria. The exact mechanisms involved are not known. [source] Preliminary evidence for in vitro methylation of tributyltin in a marine sedimentAPPLIED ORGANOMETALLIC CHEMISTRY, Issue 11 2001Alfred J. Vella Abstract Recent reports from our laboratory on the occurrence of methylbutyltins in marine sediments and seawater suggest that these compounds are formed in the environment by the methylation of both tributyltin (TBT) and thatof its degradation products, i.e. dibutyltin and monobutyltin, to give MenBu(4,n)Sn for which n,=,1, 2 and 3 respectively. We investigated the possibility of inducing methylation of TBT in seawater,sediment mixtures in experiments carried out in vitro using environmental materials collected from a yacht marina in Msida, Malta. Three water,sediment mixtures, which were shown to contain TBT, dibutyltin and monobutyltin but no other organotins, were spiked with tributyltin chloride (90,mg in 100,ml sea-water/100,ml sediment); to one mixture was added sodium acetate and to another methanol, to act as possible additional carbon sources, and all mixtures were allowed to stand at 25,°C in stoppered clear-glass bottles in diffused light for a maximum of 315 days. Speciation and quantification of organotins was performed using aqueous phase boroethylation with simultaneous solvent extraction followed by gas chromatography with flame photometric detection. The atmosphere inside the bottles quickly became reducing with abundant presence of H2S, and after an induction period of about 112 days, and only in the reaction mixture containing methanol, methyltributyltin (MeBu3Sn) was observed in both sediment (maximum concentration 0.87 µgSn g,1) and overlying water (maximum concentration 6.0 µgSn l,1). The minimum conversion yield of TBT into MeBu3Sn was estimated to be 0.3%. MeBu3Sn has a significantly lower affinity for sediment than TBT and, therefore, is more mobile in the marine environment, possibly also migrating into the atmosphere to generate a hitherto unsuspected flux of organotin into that phase. Copyright © 2001 John Wiley & Sons, Ltd. [source] Mixed-chalcogenide double-butterfly complex [{(CO)6Fe2SSe}2{,-C(H),C(H)}]ACTA CRYSTALLOGRAPHICA SECTION C, Issue 4 2000Kaliyamoorthy Panneerselvam Bubbling acetylene gas slowly through a methanol solution of [(CO)6Fe2{,-SSe}] containing sodium acetate for 48,h at room temperature yields the double-butterfly complex ,-[ethane-1,1,2,2-tetra(selenido/sulfido)]bis[hexacarbonyldiiron(Fe,Fe)], [Fe4(C2H2S2Se2)(CO)12]. The molecular structure was established by single-crystal X-ray diffraction techniques. The structure consists of two Fe2SSe butterfly units linked to each other through a bridging HC,CH group. The molecule has twofold symmetry and the two Fe atoms have distorted octahedral geometries. [source] Effect of seeding sludge type and hydrodynamic shear force on the aerobic sludge granulation in sequencing batch airlift reactorsASIA-PACIFIC JOURNAL OF CHEMICAL ENGINEERING, Issue 5 2009K. Y. Koh Abstract Two sequencing batch airlift reactors (SBARs) were operated simultaneously for two separate runs. In the first run, two different types of seeding sludge were cultivated in two separate reactors under the same superficial air velocity (SAV). In the second run, the same seeding sludge was cultivated in both reactors but under different SAV, i.e. 1.2 and 3.6 cm s,1. Both runs were carried out for a period of about 20 days, during which the chemical oxygen demand (COD) removal efficiency and morphology of sludge were examined. Batch tests using sodium acetate as the main carbon source were conducted to investigate the COD removal efficiency, and the morphologies of sludge were examined under light microscopy. Results showed that the COD removal efficiency improved with cultivation time. Morphological study showed that all cultivated sludge lost their filamentous species after a few days of cultivation, leaving behind communities of loosely packed pellet-like groups. Although the SAV recommended by other researchers was applied to the SBAR, granulation did not take place at the end of both experimental runs. It was suspected that the failure for aerobic sludge to granulate under the selected operating strategies and reactor configuration was partly due to the intrinsic traits of the sludge microbial community. Copyright © 2009 Curtin University of Technology and John Wiley & Sons, Ltd. [source] Crystallization and preliminary X-ray characterization of a thermostable pectate lyase from Thermotoga maritimaACTA CRYSTALLOGRAPHICA SECTION D, Issue 4 2002Michael A. McDonough Pectate lyase is an enzyme involved in the degradation of the pectate portion of the primary plant cell wall. A recombinant pectate lyase from Thermotoga maritima where three of the four cysteine residues have been mutated (C132I, C156N, C194L) has been crystallized. Crystals of the same morphology and trigonal space group R3 with similar unit-cell parameters were obtained under two different conditions. The first, 0.3,M (NH4)H2PO4 pH 4.2, gave crystals with a maximum size of 0.4 × 0.2 × 0.2,mm in one week that diffracted to a resolution of 1.87,Å and had unit-cell parameters a = b = 80.6, c = 148.8,Å. The second, 0.1,M sodium acetate, 6%(w/v) PEG 4000 pH 6.5, gave the same size crystals in two weeks that diffracted to a resolution of 2.1,Å and had unit-cell parameters a = b = 80.0, c = 150.1,Å. [source] Crystallization and preliminary X-ray analysis of the archaeosine tRNA-guanine transglycosylase from Pyrococcus horikoshiiACTA CRYSTALLOGRAPHICA SECTION D, Issue 11 2001Ryuichiro Ishitani The archaeosine tRNA-guanine transglycosylase from the hyperthermophilic archaeon Pyrococcus horikoshii was crystallized and preliminary X-ray characterization was performed. Single crystals were grown by the hanging-drop vapour-diffusion method, using sodium/potassium phosphate and sodium acetate as precipitants. The space group is P41212 or P43212, with unit-cell parameters a = b = 99.28,(14), c = 363.74,(56),Å. The cryocooled crystals diffracted X-rays beyond 2.2,Å resolution using synchrotron radiation from station BL44XU at SPring-8 (Harima). Selenomethionine-substituted protein crystals were prepared in order to solve the structure by the MAD phasing method. [source] Cloning, purification, crystallization and preliminary X-ray crystallographic analysis of SET/TAF-I,,N from Homo sapiensACTA CRYSTALLOGRAPHICA SECTION F (ELECTRONIC), Issue 8 2010Zhen Xu The histone chaperone SET encoded by the SET gene, which is also known as template-activating factor I, (TAF-I,), is a multifunctional molecule that is involved in many biological phenomena such as histone binding, nucleosome assembly, chromatin remodelling, replication, transcription and apoptosis. A truncated SET/TAF-I,,N protein that lacked the first 22 residues of the N-terminus but contained the C-terminal acidic domain and an additional His6 tag at the C-terminus was overexpressed in Escherichia coli and crystallized by the hanging-drop vapour-diffusion method using sodium acetate as precipitant at 283,K. The crystals diffracted to 2.7,Å resolution and belonged to space group P43212. [source] Crystallization and preliminary X-ray diffraction studies of hyperthermophilic archaeal Rieske-type ferredoxin (ARF) from Sulfolobus solfataricus P1ACTA CRYSTALLOGRAPHICA SECTION F (ELECTRONIC), Issue 7 2010Asako Kounosu The hyperthermophilic archaeal Rieske-type [2Fe,2S] ferredoxin (ARF) from Sulfolobus solfataricus P1 contains a low-potential Rieske-type [2Fe,2S] cluster that has served as a tractable model for ligand-substitution studies on this protein family. Recombinant ARF harbouring a pET30a vector-derived N-terminal extension region plus a hexahistidine tag has been heterologously overproduced in Escherichia coli, purified and crystallized by the hanging-drop vapour-diffusion method using 0.05,M sodium acetate, 0.05,M HEPES, 2,M ammonium sulfate pH 5.5. The crystals diffracted to 1.85,Å resolution and belonged to the tetragonal space group P43212, with unit-cell parameters a = 60.72, c = 83.31,Å. The asymmetric unit contains one protein molecule. [source] Crystallization and preliminary X-ray diffraction analysis of the complex of Kunitz-type tamarind trypsin inhibitor and porcine pancreatic trypsinACTA CRYSTALLOGRAPHICA SECTION F (ELECTRONIC), Issue 11 2009Sakshi Tomar The complex of Tamarindus indica Kunitz-type trypsin inhibitor and porcine trypsin has been crystallized by the sitting-drop vapour-diffusion method using ammonium acetate as precipitant and sodium acetate as buffer. The homogeneity of complex formation was checked by size-exclusion chromatography and further confirmed by reducing SDS,PAGE. The crystals diffracted to 2.0,Å resolution and belonged to the tetragonal space group P41, with unit-cell parameters a = b = 57.1, c = 120.1,Å. Preliminary X-ray diffraction analysis indicated the presence of one unit of inhibitor,trypsin complex per asymmetric unit, with a solvent content of 45%. [source] Determination of secnidazole in human plasma by high-performance liquid chromatography with UV detection and its application to the bioequivalence studiesBIOMEDICAL CHROMATOGRAPHY, Issue 3 2007Xiaoyu Li Abstract A simple, accurate, precise and sensitive HPLC-UV method was developed for the determination of secnidazole in human plasma. Secnidazole and tinidazole (IS) were extracted from 0.2 mL of human plasma by ethyl acetate. Secnidazole was then separated by HPLC on a Diamond C18 column and quantified by ultraviolet detection at 319 nm. The mobile phase consisted of acetonitrile,aqueous 5 mm sodium acetate (30:70, v/v) containing of 0.1% acetic acid adjusted to pH 4.0, and the flow rate was 1.0 mL/min. The low limit of quantification was 0.1 µg/mL. The method was linear over the concentration range 0.1,25.0 µg/mL (R2 = 1.000). The recovery of secnidazole from human plasma ranged from 76.5 to 89.1%. Inter- and intra-assay precision ranged from 3.3 to 10.7%. Secnidazole in plasma was stable when stored at ambient temperature for 8 h, at ,20°C for 2 weeks and at ,20°C for three freeze,thaw cycles. The developed method was successfully applied to the pharmacokinetic and bioequivalence studies between test and reference secnidazole tablets following a single 500 mg oral dosage to 20 healthy volunteers of both genders. Pharmacokinetics parameters Tmax, Cmax, AUC0,t, AUC0,,, T1/2 were determined of both preparations. The analysis of variance (ANOVA) did not show any significant difference between the two preparations and 90% confidence intervals fell within the acceptable range for bioequivalence. It was concluded that the two secnidazole preparations are bioequivalence and may be used interchangeably. Copyright © 2007 John Wiley & Sons, Ltd. [source] The effect of carbon source on microbial community structure and Cr(VI) reduction rateBIOTECHNOLOGY & BIOENGINEERING, Issue 3 2010Athanasia G. Tekerlekopoulou Abstract In the present work, the effect of the carbon source on microbial community structure in batch cultures derived from industrial sludge and hexavalent chromium reduction was studied. Experiments in aerobic batch reactors were carried out by amending industrial sludge with two different carbon sources: sodium acetate and sucrose. In each of the experiments performed, four different initial Cr(VI) concentrations of: 6, 13, 30 and 115,mg/L were tested. The change of carbon source in the batch reactor from sodium acetate to sucrose led to a 1.3,2.1 fold increase in chromium reduction rate and to a 5- to 9.5-fold increase in biomass. Analysis of the microbial structure in the batch reactor showed that the dominant communities were bacterial species (Acinetobacter lwoffii, Defluvibacter lusatiensis, Pseudoxanthomonas japonensis, Mesorhizium chacoense, and Flavobacterium suncheonense) when sodium acetate was used as carbon source and fungal strains (Trichoderma viride and Pichia jadinii), when sodium acetate was replaced by sucrose. These results indicate that the carbon source is a key parameter for microbial dynamics and enhanced chromium reduction and should be taken into account for efficient bioreactor design. Biotechnol. Bioeng. 2010;107: 478,487. © 2010 Wiley Periodicals, Inc. [source] Impact of freezing on pH of buffered solutions and consequences for monoclonal antibody aggregationBIOTECHNOLOGY PROGRESS, Issue 3 2010Parag Kolhe Abstract Freezing of biologic drug substance at large scale is an important unit operation that enables manufacturing flexibility and increased use-period for the material. Stability of the biologic in frozen solutions is associated with a number of issues including potentially destabilizing pH changes. The pH changes arise from temperature-associated change in the pKas, solubility limitations, eutectic crystallization, and cryoconcentration. The pH changes for most of the common protein formulation buffers in the frozen state have not been systematically measured. Sodium phosphate buffer, a well-studied system, shows the greatest change in pH when going from +25 to ,30°C. Among the other buffers, histidine hydrochloride, sodium acetate, histidine acetate, citrate, and succinate, less than 1 pH unit change (increase) was observed over the temperature range from +25 to ,30°C, whereas Tris-hydrochloride had an ,1.2 pH unit increase. In general, a steady increase in pH was observed for all these buffers once cooled below 0°C. A formulated IgG2 monoclonal antibody in histidine buffer with added trehalose showed the same pH behavior as the buffer itself. This antibody in various formulations was subject to freeze/thaw cycling representing a wide process (phase transition) time range, reflective of practical situations. Measurement of soluble aggregates after repeated freeze,thaw cycles shows that the change in pH was not a factor for aggregate formation in this case, which instead is governed by the presence or absence of noncrystallizing cryoprotective excipients. In the absence of a cryoprotectant, longer phase transition times lead to higher aggregation. © 2009 American Institute of Chemical Engineers Biotechnol. Prog., 2010 [source] Overexpression, purification, crystallization and preliminary structural studies of p -coumaric acid decarboxylase from Lactobacillus plantarumACTA CRYSTALLOGRAPHICA SECTION F (ELECTRONIC), Issue 4 2007Blanca De Las Rivas The substrate-inducible p -coumaric acid decarboxylase (PDC) from Lactobacillus plantarum has been overexpressed in Escherichia coli, purified and confirmed to possess decarboxylase activity. The recombinant His6 -tagged enzyme was crystallized using the hanging-drop vapour-diffusion method from a solution containing 20%(w/v) PEG 4000, 12%(w/v) 2-propanol, 0.2,M sodium acetate, 0.1,M Tris,HCl pH 8.0 with 0.1,M barium chloride as an additive. Diffraction data were collected in-house to 2.04,Å resolution. Crystals belonged to the tetragonal space group P43, with unit-cell parameters a = b = 43.15, c = 231.86,Å. The estimated Matthews coefficient was 2.36,Å3,Da,1, corresponding to 48% solvent content, which is consistent with the presence of two protein molecules in the asymmetric unit. The structure of PDC has been determined by the molecular-replacement method. Currently, the structure of PDC complexed with substrate analogues is in progress, with the aim of elucidating the structural basis of the catalytic mechanism. [source] Expression, purification and crystallization of a novel nonstructural protein VP9 from white spot syndrome virusACTA CRYSTALLOGRAPHICA SECTION F (ELECTRONIC), Issue 8 2006Yang Liu The nonstructural protein VP9 from white spot syndrome virus (WSSV) has been identified and expressed in Escherichia coli. To facilitate purification, a cleavable His6 tag was introduced at the N-terminus. The native protein was purified and crystallized by vapour diffusion against mother liquor containing 2,M sodium acetate, 100,mM MES pH 6.3, 25,mM cadmium sulfate and 3% glycerol. Crystals were obtained within 7,d and diffracted to 2.2,Å; they belonged to space group P212121, with unit-cell parameters a = 74.13, b = 78.21, c = 78.98,Å and four molecules in the asymmetric unit. The selenomethionine-labelled protein produced isomorphous crystals that diffracted to approximately 3.3,Å. [source] Effects of cadmium on formation of the ventral body wall in chick embryos and their prevention by zinc pretreatmentBIRTH DEFECTS RESEARCH, Issue 2 2001Jennifer Thompson Background Cadmium (Cd) is an established experimental teratogen whose effects can be reversed by pretreatment with zinc. Mesodermal development is a frequently reported target for Cd teratogenicity. The aim of this study was to examine the mechanisms of Cd induced body wall defects in chick embryos. Methods Chick embryos in shell-less culture were treated with 50 ,l of cadmium acetate (8.9 × 10,5 M Cd2+) at 60-hr incubation (H.-H. stages 16,17). Controls received equimolar sodium acetate. Other embryos were treated with various concentrations of zinc acetate and then with Cd or NaAc 1 hrs later. Development was evaluated 48 hrs later. Resin-embedded 1-,m sections were examined at earlier stages. Results Cd caused embryolethality (35%), ventral body wall defect with malpositioned lower limbs (40%), and weight reduction in survivors. After 4-hr treatment with Cd, breakdown of junctions between peridermal cells with rounding up and desquamation occurred. Shape changes were also seen in the basal layer of the ectoderm. At 4 hr, cell death was evident in lateral plate mesoderm, somites, and neuroepithelium; the lateral plate mesoderm began to grow dorsally, carrying the attached limb buds with it. Zn pretreatment protected against the lethal, teratogenic, and growth-retarding effects of Cd, as well as ectodermal changes and cell death. Conclusions Cd disrupts peridermal cell adhesion and induces cell death in the mesoderm. This may result in abnormal growth of lateral plate mesoderm and in a body wall defect. Zn pretreatment prevents both the gross teratogenic effects and the cellular changes, most likely by competition with Cd. Teratology 64:87,97, 2001. © 2001 Wiley-Liss, Inc. [source] The Pheromone Production of Female Plodia interpunctella Is Inhibited by Tyraminergic AntagonistsCHEMISTRY & BIODIVERSITY, Issue 11 2004Akinori Hirashima Several compounds were found to suppress the calling behavior and in vitro pheromone biosynthesis of the Indian meal moth, Plodia interpunctella. The compounds were screened by means of a calling-behavior bioassay with female P. interpunctella. Five derivatives with activities in the nanomolar range were identified, in order of decreasing pheromonostatic activity: 4-hydroxybenzaldehyde semicarbazone (42) >5-(4-methoxyphenyl)-1,3-oxazole (38) >5-[4-(tert -butyl)phenyl]-1,3-oxazole (40) >5-(3-methoxyphenyl)-1,3-oxazole (35) >5-(4-cyanophenyl)-1,3-oxazole (36). These compounds also showed in vitro inhibitory activity in intracellular de novo pheromone biosynthesis, as determined with isolated pheromone-gland preparations that incorporated [1- 14C]sodium acetate in the presence of the so-called pheromone-biosynthesis-activating neuropeptide (PBAN). The non-additive effect of the inhibitor with antagonist (yohimbine) for the tyramine (TA) receptor suggests that it could be a tyraminergic antagonist. Three-dimensional (3D) computer models were built from a set of compounds. Among the common-featured models generated by the program Catalyst/HipHop, aromatic-ring (AR) and H-bond-acceptor-lipophilic (HBAl) features were considered to be essential for inhibitory activity in the calling behavior and in vitro pheromone biosynthesis. Active compounds, including yohimbine, mapped well onto all the AR and HBAl features of the hypothesis. Less-active compounds were shown to be unable to achieve an energetically favorable conformation, consistent with our 3D common-feature pharmacophore models. The present hypothesis demonstrates that calling behavior and PBAN-stimulated incorporation of radioactivity are inhibited by tyraminergic antagonists. [source] Synthesis of some new fused coumarin derivativesCHINESE JOURNAL OF CHEMISTRY, Issue 4 2000El-Deen Ibrahim Mohey Abstract 2-Hydrazino-4-hydroxy-5H -[1]-benzopyrano-[4,3-d]-pyrimidin-5-one (3) was prepared via condensation of 2 with hydrazine hydrate. Treatment of 3 with methylene chloride, ethyl chloroformate, ethyl chloroacetate and benzaldehyde yielded the corresponding 2 - ( substituted ) hydrazino - 4 -hydro-xy-5H -[1]-benzopyrano-[4,3-d]-pyrimidin-5-one (4, 5, 6, and 10), followed by cyclization of 4, 5 and 6 with dimethyl formamide and fused sodium acetate under reflux, while compound 10 was cyclized with bromine and sodium acetate in acetic acid. Compound 3 reacted with ,-(toloyl) acrylic acid, ethyl ,-cyano- p -methoxycinnamate, diethyl malonate and acetyl chloride affording the corresponding 2-(substituted) hydrazino-4-hydroxy-5H -[1]-benzopyrano-[4,3-d]-pyrimidin-5-one (12, 13, 14, 15 and 16). [source] | ||||||||||||||||||||||||||||||||||