New Acetylcholinesterase‐Inhibitory Pregnane Glycosides of Cynanchum atratum Roots

Three new pregnane glycosides, cynatroside A ( 1 ), cynatroside B ( 2 ), and cynatroside C ( 3 ), isolated from the roots of Cynanchum atratum (Asclepiadaceae), were characterized as 7β‐{[O‐α‐L ‐cymaropyranosyl‐(1→4)‐O‐β‐D ‐digitoxopyranosyl‐(1→4)‐β‐D ‐oleandropyranosyl]oxy}‐3,4,4a,4b,5,6,7,8,10,10a‐decahydro‐6α‐hydroxy‐4b‐ methyl‐2‐(2‐methyl‐3‐furyl)phenanthren‐1(2H)‐one ( 1 ), 7β‐{[O‐β‐D ‐cymaropyranosyl‐(1→4)‐O‐α‐L ‐diginopyranosyl‐(1→4)‐β‐D ‐cymaropyranosyl]oxy}‐3,4,4a,4b,5,6,7,8,10,10a‐decahydro‐2,6α‐dihydroxy‐4b‐methyl‐2‐(2‐methyl‐3‐furyl)phenanthren‐1(2H)‐one ( 2 ), and 7β‐{[O‐α‐L ‐cymaropyranosyl‐(1→4)‐O‐β‐D ‐digitoxopyranosyl‐(1→4)‐β‐L ‐cymaropyranosyl]oxy}‐3,4,4a,4b,5,6,7,8,10,10a‐decahydro‐2,6α‐dihydroxy‐4b‐methyl‐2‐(2‐methyl‐3‐furyl)phenanthren‐1(2H)‐one ( 3 ), respectively. In addition, ten known constituents were identified, i.e., cynascyroside D ( 4 ), glaucoside C ( 5 ), glaucoside D ( 6 ), atratoside A ( 7 ), 2,4‐dihydroxyacetophenone ( 8 ), 4‐hydroxyacetophenone ( 9 ), syringic acid ( 10 ), azelaic acid ( 11 ), suberic acid ( 12 ), and succinic acid ( 13 ). Among these compounds, 1 – 4 significantly inhibit acetylcholinesterase activity.     

Insertion Reactions of Carbon Disulfide into Mg‐C and Mg‐N Bonds: Syntheses and Structural Determinations of Mg(S2CY)2(THF)n(Y=NEt2, NiPr2, iPr,Ph) and BrMg(S2CZ)(THF)3(Z=Ph,iPr)

The insertion reaction of CS₂ with Mg(NR₂)₂ (R= Et, ⁱPr), MgR′₂ (R′= Et, Ph) and R″MgBr (R″= ⁱPr, Ph) respectively lead solid products, Mg(S₂CNR₂)₂(THF)_n ( 1 : R= Et, n=2; 2 : R= ⁱPr, n=1), Mg(S₂C′R)₂(THF)₂ ( 3 : ′R= Et, 4 : ′R= Ph), BrMg(S₂C″R) (THF)₃ ( 5 : ″R= ⁱPr, 6 : ″R= Ph) in which the inserted carbon disulfides act as terminal chelating ligands. These compounds were characterized with ¹H, ¹³C NMR, IR spectroscopy, mass spectrometry, elemental analyses, and X‐ray crystallography.     

Control of Enzymatic Degradation of Microbial Polyesters by Plasma Modification

The rate of enzymatic degradation of surface‐modified microbial polyesters, poly[(R)‐3‐hydroxybutyrate] and poly[(R)‐3‐hydroxybutyrate‐co‐3‐hydroxyvalerate], was studied. The plasma treatments were carried out in a CF₃H or O₂ environment. It was found that the CF₃H plasma‐treated polyesters exhibited significant retardation of enzymatic erosion because of the surface fluorocarbon groups induced by CF₃H plasma. These surface fluorocarbon groups act as retardants on enzymatic degradation due to increased hydrophobicity and of the inactivity of enzymes. However, the increased surface hydrophilicity of polyesters induced by O₂ plasma results in no significant acceleration of the enzymatic erosion, which may be due to the thin modified layer.

Weight loss profiles of P(3HB) film exposed to CF₃H plasma as a function of plasma exposure time.     

Influence of elastomeric core–shell impact modifiers on mechanical properties of cellulose diacetate resin

Cellulose diacetate (CDA) plasticized with triacetine was blended by melting extrusion with two different kind of elastomeric core–shell impact modifiers: methyl methacrylate (MMA, shell) grafted onto styrene–butadiene–rubber (SBR, core) (MSBR) and MMA (shell) grafted onto butyl acrylate rubber (BAR, core) (MBAR). The different CDA/MSBR and CDA/MBAR blends were characterized by mechanical properties and morphological observation with various impact modifier contents. The highest impact strength was observed in the case of the blend with 5 wt% of MSBR and 3 wt% of MBAR, respectively. The tensile strength and Young’s modulus of CDA blends were decreased with increasing both MSBR and MBAR. According to SEM observation, MBAR was dispersed more effectively in CDA matrix than that of MSBR, thus indicating improved impact strength.     

Analysis of Overlapped and Noisy Hydrogen/Deuterium Exchange Mass Spectra

Noisy and overlapped mass spectrometry data hinder the sequence coverage that can be obtained from hydrogen deuterium exchange analysis, and places a limit on the complexity of the samples that can be studied by this technique. Advances in instrumentation have addressed these limits, but as the complexity of the biological samples under investigation increases, these problems are re-encountered. Here we describe the use of binomial distribution fitting with asymmetric linear squares regression for calculating the accurate deuterium content for mass envelopes of low signal or that contain significant overlap. The approach is demonstrated with a test data set of HIV Env gp140 wherein inclusion of the new analysis regime resulted in obtaining exchange data for 42 additional peptides, improving the sequence coverage by 11 %. At the same time, the precision of deuterium uptake measurements was improved for nearly every peptide examined. The improved processing algorithms also provide an efficient method for deconvolution of bimodal mass envelopes and EX1 kinetic signatures. All these functions and visualization tools have been implemented in the new version of the freely available software, HX-Express v2.

Electrochemical properties of PEO/PMMA blend-based polymer electrolytes using imidazolium salt-supported silica as a filler

In this study, the composite polymer electrolytes (CPEs) were prepared by solution casting technique. The CPEs consisted of PEO/PMMA blend as a host matrix doped with LiClO₄. Propylene carbonate (PC) was used as plasticizer and a small amount of imidazolium salt-supported amorphous silica (IS-AS) as a filler was prepared by the sol–gel method. At room temperature, the highest conductivity was obtained for the composition having PEO–PMMA–LiClO₄–PC–4wt. % IS-AS with a value of 1.15 × 10^?4 S/cm. In particular, the CPE using the IS-AS filler showed a higher conductivity than any other sample (fumed silica, amorphous silica). Studies of differential scanning calorimetry and scanning electron microscopy indicated that the ionic conductivity increase was due to an expansion in the amorphous phase which enhances the flexibility of polymeric chains and the homogeneous structure of CPEs. It was found that the ionic conductivity and interfacial resistance stability of CPEs was significantly improved by the addition of IS-AS. In other words, the resistance stability and maximum ambient ionic conductivity of CPEs containing IS-AS filler were better than CPEs containing any other filler.     

Production from ilmenite of TiO2-supported catalysts for selective catalytic reduction of NO with NH3

Economic production of titanium dioxide (yield >98 %) from ilmenite has been achieved by use of a modified sulfate reduction process. A series of samples were prepared by varying the concentration of titanium dioxide nuclei (0.2, 0.3, and 0.6 %) and further impregnation with antimony and vanadia. The structural and acidic properties of the samples were comprehensively studied by X-ray diffraction (XRD), transmission electron microscopy, BJH pore size distribution, and temperature-programmed desorption of NH₃. The XRD results revealed the presence of intense peaks from anatase titanium dioxide. Enhancement of surface area was observed for second-time filtered samples, possibly because of loss of iron from the bulk. As a result, formation of additional micropores was apparent from N₂ adsorption and desorption isotherms. Among all the antimony and vanadia-doped samples, the first-time filtered sample with the low concentration of nuclei (0.2 %) had the highest catalytic activity at low temperatures, owing to its larger pore size and abundant acidic species.     

Glucose Oxidase/Cellulose–Carbon Nanotube Composite Paper as a Biocompatible Bioelectrode for Biofuel Cells

Biofuel cells are devices for generating electrical energy directly from chemical energy of renewable biomass using biocatalysts such as enzymes. Efficient electrical communication between redox enzymes and electrodes is essential for enzymatic biofuel cells. Carbon nanotubes (CNTs) have been recognized as ideal electrode materials because of their high electrical conductivity, large surface area, and inertness. Electrodes consisting entirely of CNTs, which are known as CNT paper, have high surface areas but are typically weak in mechanical strength. In this study, cellulose (CL)–CNT composite paper was fabricated as electrodes for enzymatic biofuel cells. This composite electrode was prepared by vacuum filtration of CNTs followed by reconstitution of cellulose dissolved in ionic liquid, 1-ethyl-3-methylimidazolium acetate. Glucose oxidase (GOx), which is a redox enzyme capable of oxidizing glucose as a renewable fuel using oxygen, was immobilized on the CL–CNT composite paper. Cyclic voltammograms revealed that the GOx/CL–CNT paper electrode showed a pair of well-defined peaks, which agreed well with that of FAD/FADH_2, the redox center of GOx. This result clearly shows that the direct electron transfer (DET) between the GOx and the composite electrode was achieved. However, this DET was dependent on the type of CNTs. It was also found that the GOx immobilized on the composite electrode retained catalytic activity for the oxidation of glucose.     

Pretreatment for Simultaneous Production of Total Lipids and Fermentable Sugars from Marine Alga, Chlorella sp.

The goal of this study was to determine the optimal pretreatment process for the extraction of lipids and reducing sugars to facilitate the simultaneous production of biodiesel and bioethanol from the marine microalga Chorella sp. With a single pretreatment process, the optimal ultrasonication pretreatment process was 10 min at 47 KHz, and extraction yields of 6.5 and 7.1 (percentage, w/w) of the lipids and reducing sugars, respectively, were obtained. The optimal microwave pretreatment process was 10 min at 2,450 MHz, and extraction yields of 6.6 and 7.0 (percentage, w/w) of the lipids and reducing sugars, respectively, were obtained. Lastly, the optimal high-pressure homogenization pretreatment process was two cycles at a pressure of 20,000 psi, and extraction yields of 12.5 and 12.8 (percentage, w/w) of the lipids and reducing sugars, respectively, were obtained. However, because the single pretreatment processes did not markedly improve the extraction yields compared to the results of previous studies, a combination of two pretreatment processes was applied. The yields of lipids and reducing sugars from the combined application of the high-pressure homogenization process and the microwave process were 24.4 and 24.9 % (w/w), respectively, which was up to three times greater than the yields obtained using the single pretreatment processes. Furthermore, the oleic acid content, which is a fatty acid suitable for biodiesel production, was 23.39 % of the fatty acids (w/w). The contents of glucose and xylose, which are among the fermentable sugars useful for bioethanol production, were 77.5 and 13.3 % (w/w) of the fermentable sugars, respectively, suggesting the possibility of simultaneously producing biodiesel and bioethanol. Based on the results of this study, the combined application of the high-pressure homogenization and microwave pretreatment processes is the optimal method to increase the extraction yields of lipids and reducing sugars that are essential for the simultaneous production of biodiesel and bioethanol.