Total synthesis of 1-(Z)-atractylodinol

The total synthesis of 1-(Z)-atractylodinol, a natural polyacetylenic alcohol with several biological activities, has been achieved using a newly developed telluride synthon and a novel use for the Negishi type coupling reaction employing vinyl tellurides.     

Standard enthalpy of solution and formation of cesium chromate. Derived thermodynamic properties of the aqueous chromate,bichromate, and dichromate ions,alkali metal and alkaline earth chromates,and lead chromate

Calorimetric measurements of the enthalpy of solution of cesium chromate gave ΔH_soln = (7622 ± 24) cal_th mol^?1 for a dilution of Cs₂CrO₄·21128H₂O. This result, along with the enthalpy of dilution gave the standard enthalpy of solution, ΔH_soln^o = (7512 ± 31) cal_th mol^?1, whence the standard enthalpy of formation, ΔH_f⁰(Cs₂CrO₄, c, 298.15 K), was calculated to be ?(341.78 ± 0.46) kcal_th mol^?1. Recomputed thermodynamic data for the formation of the other alkali metal chromates have been tabulated. From their solubilities and enthalpies of solution, the standard entropies, S⁰(298 K), of BaCrO₄ and PbCrO₄ were estimated to be (38.9 ± 0.9) and (43.7 ± 1.2) cal_th K^?1 mol^?1, respectively. There is evidence that ΔH_f⁰(SrCrO₄, c, 298.15 K) may be in error. Thermochemical, solubility, and equilibrium data, have been combined to update the thermodynamic properties of the aqueous chromate (CrO₄^2?), bichromate (HCrO₄^?), and dichromate (Cr₂O₇^2?) ions. The new values at 298.15 K are as follows:

     

3.

Characterization of Sol-gel bioencapsulates for ester hydrolysis and synthesis     

Cleide M. F. Soares  Heizir F. de Castro  Juliana E. Itako  Flavio F. De Moraes  Gisella M. Zanin 《Applied biochemistry and biotechnology》2005,123(1-3):845-859

Candida rugosa lipase was entrapped in silica sol-gel particles prepared by hydrolysis of methyltrimethoxysilane and assayed by p-nitrophenyl palmitate hydrolysis, as a function of pH and temperature, giving pH optima of 7.8 (free enzyme) and 5.0–8.0 (immobilized enzyme). The optimum temperature for the immobilized enzyme (50–55°C) was 19°C higher than for the free enzyme. Thermal, operational, and storage stability were determined with n-butanol and bytyric acid, giving at 45°C a half-life 2.7 times greater for the immobilized enzyme; storage time was 21 d at room temperature. For ester synthesis, the optimum temperature was 47°C, and high esterification conversions were obtained under repeated batch cycles (half-life of 138 h).     

4.

A new polyphenol modified electrode containing an anchored ruthenium complex and its use in electrocatalytic oxidation of organic substrates     

Juliana R. Steter  José O.S. PontólioM.I.C.F. Costa  J.R. Romero 《Polyhedron》2007

This work describes the preparation of a new modified electrode containing a ruthenium complex (cis-aquadimethylbipyridyltriphenylphosphineruthenium II), bonded to a stable polyphenol film. This modified electrode promotes the fast electrocatalytic oxidation of safrol (5-allyl-benzo[1,3]dioxole) and isosafrol (5-propenyl-benzo[1,3]dioxole), giving two interesting products benzo[1,3]dioxole-5-carbaldehyde (piperonal) and 3-benzo[1,3]dioxol-5-yl-propenal respectively, with good yields. The electrode preparation can be carried out at a potential range which does not interfere on the anchored electroactive ruthenium complex, but it allows for the phenol oxidation to occur and therefore polymerize forming the polyphenol film. The catalytic character of this modified electrode is showed by its high turnover numbers. The procedure to isolate the products is very simple.     

5.

Incomplete Swallowing and Retracted Tongue Maneuvers for Electromyographic Signal Normalization of the Extrinsic Muscles of the Larynx     

Patricia Maria Mendes Balata  Hilton J. Silva  Gerlane Karla O. Nascimento  Klyvia Juliana R. Moraes  Leandro A. Pernambuco  Maria Clara R. Freitas  Leilane M. Lima  Renata S. Braga  Síntia R. Souza  Silvia Regina A. Moraes 《Journal of voice》2012,26(6):813.e1-813.e7

     

6.

Replacing Synthetic with Microbial Surfactants as Collectors in the Treatment of Aqueous Effluent Produced by Acid Mine Drainage,Using the Dissolved Air Flotation Technique     

Carlyle T. B. Menezes  Erilson C. Barros  Raquel D. Rufino  Juliana M. Luna  Leonie A. Sarubbo 《Applied biochemistry and biotechnology》2011,163(4):540-546

Dissolved air flotation (DAF) is a well-established separation process employing micro bubbles as a carrier phase. The application of this technique in the treatment of acid mine drainage, using three yeast biosurfactants as alternative collectors, is hereby analyzed. Batch studies were carried out in a 50-cm high acrylic column with an external diameter of 2.5 cm. High percentages (above 94%) of heavy metals Fe(III) and Mn(II) were removed by the biosurfactants isolated from Candida lipolytica and Candida sphaerica and the values were found to be similar to those obtained with the use of the synthetic sodium oleate surfactant. The DAF operation with both surfactant and biosurfactants, achieved acceptable turbidity values, in accordance with Brazilian standard limits. The best ones were obtained by the biosurfactant from C. lipolytica, which reached 4.8 NTU. The results obtained with a laboratory synthetic effluent were also satisfactory. The biosurfactants removed almost the same percentages of iron, while the removal percentages of manganese were slightly higher compared with those obtained in the acid mine drainage effluent. They showed that the use of low-cost biosurfactants as collectors in the DAF process is a promising technology for the mining industries.     

7.

Characterization of nanochannel delivery membrane systems for the sustained release of resveratrol and atorvastatin: new perspectives on promoting heart health     

Juliana Sih  Shyam S. Bansal  Stefano Filipini  Silvia Ferrati  Kunal Raghuwansi  Erika Zabre  Eugenia Nicolov  Daniel Fine  Mauro Ferrari  Ganesh Palapattu  Alessandro Grattoni 《Analytical and bioanalytical chemistry》2013,405(5):1547-1557

Novel drug delivery systems capable of continuous sustained release of therapeutics have been studied extensively for use in the prevention and management of chronic diseases. The use of these systems holds promise as a means to achieve higher patient compliance while improving therapeutic index and reducing systemic toxicity. In this work, an implantable nanochannel drug delivery system (nDS) is characterized and evaluated for the long-term sustained release of atorvastatin (ATS) and trans-resveratrol (t-RES), compounds with a proven role in managing atherogenic dyslipidemia and promoting cardioprotection. The primary mediators of drug release in the nDS are nanofluidic membranes with hundreds of thousands of nanochannels (up to 100,000/mm²) that attain zero-order release kinetics by exploiting nanoconfinement and molecule-to-surface interactions that dominate diffusive transport at the nanoscale. These membranes were characterized using gas flow analysis, acetone diffusion, and scanning and transmission electron microscopy (SEM, TEM). The surface properties of the dielectric materials lining the nanochannels, SiO₂ and low-stress silicon nitride, were further investigated using surface charge analysis. Continuous, sustained in vitro release for both ATS and t-RES was established for durations exceeding 1 month. Finally, the influence of the membranes on cell viability was assessed using human microvascular endothelial cells. Morphology changes and adhesion to the surface were analyzed using SEM, while an MTT proliferation assay was used to determine the cell viability. The nanochannel delivery approach, here demonstrated in vitro, not only possesses all requirements for large-scale high-yield industrial fabrication, but also presents the key components for a rapid clinical translation as an implantable delivery system for the sustained administration of cardioprotectants.     

8.

Assessment of dispersive liquid–liquid microextraction for the simultaneous extraction,preconcentration, and derivatization of Hg2+ and CH3Hg+ for further determination by GC–MS     

Bruno M. Soares  Ederson R. Pereira  Juliana V. Maciel  Augusto A. Vieira  Fabio A. Duarte 《Journal of separation science》2013,36(20):3411-3418

This work reports the development of a dispersive liquid – liquid microextraction method for the simultaneous extraction, preconcentration, and derivatization of Hg²⁺ and CH₃Hg⁺ species from water samples for further determination by GC – MS. Some parameters of the proposed method, such as volume and type of disperser and extraction solvent, and Na[B(C₆H₅)₄] concentration were investigated using response surface methodology. Suitable recoveries were obtained using 80 μL C₂Cl₄ (as extraction solvent), 1000 μL ethanol (as disperser solvent), and 300 μL 2.1 mmol/L Na[B(C₆H₅)₄] (as derivatizing agent). Accuracy was evaluated in terms of recovery and ranged from 87 to 99% with RSD values <7%. In addition, a certified reference material of water (NIST 1641d) was analyzed and agreed with the certified value about 107% (for Hg²⁺), with RSD values <8.5%. LODs were 0.3 and 0.2 μg/L, with enrichment factors of 112 and 115 for Hg²⁺ and CH₃Hg⁺, respectively. The optimized method was applied for the determination of Hg²⁺ and CH₃Hg⁺ in tap, well, and lake water samples.     

9.

From Levulinic Acid to Biheterocycles: Synthesis of 1-[(5-Hydroxy-5-trifluoromethyl-3-substituted-4,5-dihydro-1H-pyrazol-1-yl)-3-(5-trifluoromethyl-1H-pyrazol-3-yl)propan-1-ones     

Alex F. C. Flores  Juliana L. Malavolta  Leandro M. Frigo  Morgana Doneda  Darlene C. Flores 《合成通讯》2013,43(10):1198-1204

We develop an efficient method to synthesize novel propionyl-spaced bisheterocyclic compounds. It entails cyclocondensation of 3-(5-trifluoromethyl-1H-pyrazol-3-yl)propanoyl hydrazide obtained from levulinic acid, with 1,1,1-trifluoro-4-methoxy-3-alken-2-ones proceeding regiospecifically to 1-[(5-trifluoromethyl-5-hydroxy-3-substituted-4,5-dihydro-1H-pyrazol-1-yl)-3-(5-trifluoromethyl-1H-pyrazol-3-yl)propan-1-one derivatives.     

10.

Depletion of the xynB2 Gene Upregulates β-Xylosidase Expression in C. crescentus     

Juliana Moço Corrêa  Moara Rodrigues Mingori  Rinaldo Ferreira Gandra  Eduardo Alexandre Loth  Flávio Augusto Vicente Seixas  Rita de Cássia Garcia Simão 《Applied biochemistry and biotechnology》2014,172(2):1085-1097

     

1 [2] [3] [4] [5] [6] [7] [8] [9] [10] [11] 下一页 » 末  页»

	$\text{S}{}^0\text{/}\text{cal}{}_{\mathrm{th}}\text{K}{}^{\mathrm{?1}}\text{mol}{}^{\mathrm{?1}}$	$\text{ΔH}{}_{\mathrm{f}}{}^0\text{/kcal}{}_{\mathrm{th}}\text{mol}{}^{\mathrm{?1}}$	$\text{ΔG}{}_{\mathrm{f}}{}^0\text{/kcal}{}_{\mathrm{th}}\text{mol}{}^{\mathrm{?1}}$
CrO42?(aq)	(13.8 ± 0.5)	?(210.93 ± 0.45)	?(174.8 ± 0.5)
HCrO4?(aq)	(46.6 ± 1.8)	?(210.0 ± 0.7)	?(183.7 ± 0.5)
Cr2O72?(aq)	(67.4 ± 3.9)	?(356.5 ± 1.5)	?(312.8 ± 1.0)

Characterization of Sol-gel bioencapsulates for ester hydrolysis and synthesis

Candida rugosa lipase was entrapped in silica sol-gel particles prepared by hydrolysis of methyltrimethoxysilane and assayed by p-nitrophenyl palmitate hydrolysis, as a function of pH and temperature, giving pH optima of 7.8 (free enzyme) and 5.0–8.0 (immobilized enzyme). The optimum temperature for the immobilized enzyme (50–55°C) was 19°C higher than for the free enzyme. Thermal, operational, and storage stability were determined with n-butanol and bytyric acid, giving at 45°C a half-life 2.7 times greater for the immobilized enzyme; storage time was 21 d at room temperature. For ester synthesis, the optimum temperature was 47°C, and high esterification conversions were obtained under repeated batch cycles (half-life of 138 h).     

A new polyphenol modified electrode containing an anchored ruthenium complex and its use in electrocatalytic oxidation of organic substrates

This work describes the preparation of a new modified electrode containing a ruthenium complex (cis-aquadimethylbipyridyltriphenylphosphineruthenium II), bonded to a stable polyphenol film. This modified electrode promotes the fast electrocatalytic oxidation of safrol (5-allyl-benzo[1,3]dioxole) and isosafrol (5-propenyl-benzo[1,3]dioxole), giving two interesting products benzo[1,3]dioxole-5-carbaldehyde (piperonal) and 3-benzo[1,3]dioxol-5-yl-propenal respectively, with good yields. The electrode preparation can be carried out at a potential range which does not interfere on the anchored electroactive ruthenium complex, but it allows for the phenol oxidation to occur and therefore polymerize forming the polyphenol film. The catalytic character of this modified electrode is showed by its high turnover numbers. The procedure to isolate the products is very simple.     

Replacing Synthetic with Microbial Surfactants as Collectors in the Treatment of Aqueous Effluent Produced by Acid Mine Drainage,Using the Dissolved Air Flotation Technique

Dissolved air flotation (DAF) is a well-established separation process employing micro bubbles as a carrier phase. The application of this technique in the treatment of acid mine drainage, using three yeast biosurfactants as alternative collectors, is hereby analyzed. Batch studies were carried out in a 50-cm high acrylic column with an external diameter of 2.5 cm. High percentages (above 94%) of heavy metals Fe(III) and Mn(II) were removed by the biosurfactants isolated from Candida lipolytica and Candida sphaerica and the values were found to be similar to those obtained with the use of the synthetic sodium oleate surfactant. The DAF operation with both surfactant and biosurfactants, achieved acceptable turbidity values, in accordance with Brazilian standard limits. The best ones were obtained by the biosurfactant from C. lipolytica, which reached 4.8 NTU. The results obtained with a laboratory synthetic effluent were also satisfactory. The biosurfactants removed almost the same percentages of iron, while the removal percentages of manganese were slightly higher compared with those obtained in the acid mine drainage effluent. They showed that the use of low-cost biosurfactants as collectors in the DAF process is a promising technology for the mining industries.     

Characterization of nanochannel delivery membrane systems for the sustained release of resveratrol and atorvastatin: new perspectives on promoting heart health

Novel drug delivery systems capable of continuous sustained release of therapeutics have been studied extensively for use in the prevention and management of chronic diseases. The use of these systems holds promise as a means to achieve higher patient compliance while improving therapeutic index and reducing systemic toxicity. In this work, an implantable nanochannel drug delivery system (nDS) is characterized and evaluated for the long-term sustained release of atorvastatin (ATS) and trans-resveratrol (t-RES), compounds with a proven role in managing atherogenic dyslipidemia and promoting cardioprotection. The primary mediators of drug release in the nDS are nanofluidic membranes with hundreds of thousands of nanochannels (up to 100,000/mm²) that attain zero-order release kinetics by exploiting nanoconfinement and molecule-to-surface interactions that dominate diffusive transport at the nanoscale. These membranes were characterized using gas flow analysis, acetone diffusion, and scanning and transmission electron microscopy (SEM, TEM). The surface properties of the dielectric materials lining the nanochannels, SiO₂ and low-stress silicon nitride, were further investigated using surface charge analysis. Continuous, sustained in vitro release for both ATS and t-RES was established for durations exceeding 1 month. Finally, the influence of the membranes on cell viability was assessed using human microvascular endothelial cells. Morphology changes and adhesion to the surface were analyzed using SEM, while an MTT proliferation assay was used to determine the cell viability. The nanochannel delivery approach, here demonstrated in vitro, not only possesses all requirements for large-scale high-yield industrial fabrication, but also presents the key components for a rapid clinical translation as an implantable delivery system for the sustained administration of cardioprotectants.     

Assessment of dispersive liquid–liquid microextraction for the simultaneous extraction,preconcentration, and derivatization of Hg2+ and CH3Hg+ for further determination by GC–MS

This work reports the development of a dispersive liquid – liquid microextraction method for the simultaneous extraction, preconcentration, and derivatization of Hg²⁺ and CH₃Hg⁺ species from water samples for further determination by GC – MS. Some parameters of the proposed method, such as volume and type of disperser and extraction solvent, and Na[B(C₆H₅)₄] concentration were investigated using response surface methodology. Suitable recoveries were obtained using 80 μL C₂Cl₄ (as extraction solvent), 1000 μL ethanol (as disperser solvent), and 300 μL 2.1 mmol/L Na[B(C₆H₅)₄] (as derivatizing agent). Accuracy was evaluated in terms of recovery and ranged from 87 to 99% with RSD values <7%. In addition, a certified reference material of water (NIST 1641d) was analyzed and agreed with the certified value about 107% (for Hg²⁺), with RSD values <8.5%. LODs were 0.3 and 0.2 μg/L, with enrichment factors of 112 and 115 for Hg²⁺ and CH₃Hg⁺, respectively. The optimized method was applied for the determination of Hg²⁺ and CH₃Hg⁺ in tap, well, and lake water samples.     

From Levulinic Acid to Biheterocycles: Synthesis of 1-[(5-Hydroxy-5-trifluoromethyl-3-substituted-4,5-dihydro-1H-pyrazol-1-yl)-3-(5-trifluoromethyl-1H-pyrazol-3-yl)propan-1-ones

We develop an efficient method to synthesize novel propionyl-spaced bisheterocyclic compounds. It entails cyclocondensation of 3-(5-trifluoromethyl-1H-pyrazol-3-yl)propanoyl hydrazide obtained from levulinic acid, with 1,1,1-trifluoro-4-methoxy-3-alken-2-ones proceeding regiospecifically to 1-[(5-trifluoromethyl-5-hydroxy-3-substituted-4,5-dihydro-1H-pyrazol-1-yl)-3-(5-trifluoromethyl-1H-pyrazol-3-yl)propan-1-one derivatives.