scholarly journals Magnetic Combined Cross-Linked Enzyme Aggregates of Ketoreductase and Alcohol Dehydrogenase: An Efficient and Stable Biocatalyst for Asymmetric Synthesis of (R)-3-Quinuclidinol with Regeneration of Coenzymes In Situ

Catalysts ◽  
2018 ◽  
Vol 8 (8) ◽  
pp. 334 ◽  
Author(s):  
Yuhan Chen ◽  
Qihua Jiang ◽  
Lili Sun ◽  
Qiang Li ◽  
Liping Zhou ◽  
...  

Enzymes are biocatalysts. In this study, a novel biocatalyst consisting of magnetic combined cross-linked enzyme aggregates (combi-CLEAs) of 3-quinuclidinone reductase (QNR) and glucose dehydrogenase (GDH) for enantioselective synthesis of (R)-3-quinuclidinolwith regeneration of cofactors in situ was developed. The magnetic combi-CLEAs were fabricated with the use of ammonium sulfate as a precipitant and glutaraldehyde as a cross-linker for direct immobilization of QNR and GDH from E. coli BL(21) cell lysates onto amino-functionalized Fe3O4 nanoparticles. The physicochemical properties of the magnetic combi-CLEAs were characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) and magnetic measurements. Field emission scanning electron microscope (FE-SEM) images revealed a spherical structure with numerous pores which facilitate the movement of the substrates and coenzymes. Moreover, the magnetic combi-CLEAs exhibited improved operational and thermal stability, enhanced catalytic performance for transformation of 3-quinuclidinone (33 g/L) into (R)-3-quinuclidinol in 100% conversion yield and 100% enantiomeric excess (ee) after 3 h of reaction. The activity of the biocatalysts was preserved about 80% after 70 days storage and retained more than 40% of its initial activity after ten cycles. These results demonstrated that the magnetic combi-CLEAs, as cost-effective and environmentally friendly biocatalysts, were suitable for application in synthesis of (R)-3-quinuclidinol essential for the production of solifenacin and aclidinium with better performance than those currently available.

2017 ◽  
Vol 727 ◽  
pp. 327-334
Author(s):  
Yan Wang ◽  
Jun Wang ◽  
Xiao Fei Zhang ◽  
Ya Qing Liu

La-Nd co-doped barium hexaferrites, Ba0.7(LamNdn)0.3Fe12O19 (D-BaM), were successfully prepared by sol-gel method. PANI / D-BaM composites were synthesized by in-situ polymerization in solution. The structure, morphology and properties of samples have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), vibrating sample magnetometer (VSM), four-probe conductivity tester and vector network analyzer. The XRD patterns showed that the crystal structure of all the samples exist as M-type phases. The SEM images revealed that the particles presented a hexagonal platelet-like morphology. The magnetic properties could be improved by substitutions of La and Nd ions. The saturation magnetization (Ms) and coercive force (Hc) increased with the change of La / Nd ratio to the maximum at La / Nd = 3:1. The doped particles have also been embedded in conductive PANI to prepare electromagnetic materials, and the conductivity kept on the order of 10-2. The microwave absorbing properties of composites at 30 MHz-6 GHz improved obviously, the peak value of reflection loss could reach-7.5 dB.


2018 ◽  
Vol 32 (8) ◽  
pp. 1078-1091 ◽  
Author(s):  
Sibel Erol Dağ ◽  
Pınar Acar Bozkurt ◽  
Fatma Eroğlu ◽  
Meltem Çelik

A series of polystyrene (PS)/unmodified Na-montmorillonite (Na-MMT) composites were prepared via in situ radical polymerization. The prepared composites were characterized using various techniques. The presence of various functional groups in the unmodified Na-MMT and PS/unmodified Na-MMT composite was confirmed by Fourier transform infrared spectroscopy. Morphology and particle size of prepared composites was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). According to the XRD and TEM results, the interlayer spacing of MMT layers was expanded. SEM images showed a spongy and porous-shaped morphology of composites. TEM revealed the Na-MMT intercalated in PS matrix. The thermal stability of PS/unmodified Na-MMT composites was significantly improved as compared to PS, which is confirmed using thermogravimetric analysis (TGA). The TGA curves indicated that the decomposition temperature of composites is higher at 24–51°C depending on the composition of the mixture than that of pure PS. The differential scanning calorimetry (DSC) results showed that the glass transition temperature of composites was higher as compared to PS. The moisture retention, water uptake, Brunauer–Emmett–Teller specific surface area, and specific pore volume of composites were also investigated. Water resistance of the composites can be greatly improved.


Minerals ◽  
2020 ◽  
Vol 10 (4) ◽  
pp. 342 ◽  
Author(s):  
Magdalena Andrunik ◽  
Magdalena Wołowiec ◽  
Daniel Wojnarski ◽  
Sylwia Zelek-Pogudz ◽  
Tomasz Bajda

Heavy metal contamination in soils has become one of the most critical environmental issues. The most efficient in-situ remediation technique is chemical immobilization that uses cost-effective soil amendments such as phosphate compounds to decrease Pb, Cd and Zn accessibility in the contaminated soils. The present study examined the effectiveness of KH2PO4 in immobilizing Pb, Cd and Zn in three samples of contaminated soils collected from ZGH “Bolesław” (Mining and Smelting Plant “Bolesław”). Effectiveness was evaluated using the following methods: a toxicity characteristic leaching procedure (TCLP)-based experiment, sequential extraction, X-ray diffraction analyses (XRD), and scanning electron microscopy–energy dispersive spectroscopy (SEM–EDS). The most efficient percentage reduction of total leachable metal concentration assessed by TCLP was observed for lead (50%–80%), and the least reduction was observed for zinc (1%–17%). The most effective immobilization of stable compounds assessed by sequential extraction was noted for lead, while the weakest immobilization was noted for cadmium. New insoluble mineral phases were identified by SEM-EDS analysis. Cd, Zn, and Pb formed new stable mineral substances with phosphates. The predominant crystal forms were dripstones and groups of needles, which were easily formed by dissolved carbon rock surfaces containing zinc ions. The alkaline nature of the soil and a large number of carbonates mainly influenced the formation of new structures.


Catalysts ◽  
2019 ◽  
Vol 9 (2) ◽  
pp. 155 ◽  
Author(s):  
Zhenheng Diao ◽  
Lushi Cheng ◽  
Xu Hou ◽  
Di Rong ◽  
Yanli Lu ◽  
...  

Hierarchical HZSM-5 membranes were prepared on the inner wall of stainless steel tubes, using amphiphilic organosilane (TPOAC) and mesitylene (TMB) as a meso-porogen and a swelling agent, respectively. The mesoporosity of the HZSM-5 membranes were tailored via formulating the TPOAC/Tetraethylorthosilicate (TPOAC/TEOS) ratio and TMB/TPOAC ratio, in synthesis gel, and the prepared membranes were systematically characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), N2 adsorption–desorption, N2 permeation, inductively coupled plasma (ICP), in situ fourier transform infrared (FT-IR), ammonia temperature-programmed desorption (NH3-TPD), etc. It was found that the increase of the TPOAC/TEOS ratio promoted a specific surface area and diffusivity of the HZSM-5 membranes, as well as decreased acidity; the increase of the TMB/TPOAC ratios led to an enlargement of the mesopore size and diffusivity of the membranes, but with constant acid properties. The catalytic performance of the prepared HZSM-5 membranes was tested using the catalytic cracking of supercritical n-dodecane (500 °C, 4 MPa) as a model reaction. The hierarchical membrane with the TPOAC/TEOS ratio of 0.1 and TMB/TPOAC ratio of 2, exhibited superior catalytic performances with the highest activity of up to 13% improvement and the lowest deactivation rate (nearly a half), compared with the microporous HZSM-5 membrane, due to the benefits of suitable acidity, together with enhanced diffusivity of n-dodecane and cracking products.


1994 ◽  
Vol 9 (2) ◽  
pp. 372-376 ◽  
Author(s):  
T. Harada ◽  
T. Kuji

In the process of crystallization of amorphous melt-spun Nd15Fe77Bx (x = 6–14) alloys, it was found that the crystallization behavior strongly depended upon the boron content even in the same equilibrium three-phase coexistence range. The Nd2Fe14B phase was crystallized directly from the amorphous state in the amorphous Nd-Fe-B materials with relatively lower boron content (Nd15Fe77B6 and Nd15Fe77B8 alloys). In contrast, the metastable body-centered-cubic (bcc) α-iron phase crystallized from the amorphous state prior to the crystallization of the Nd2Fe14B phase in the amorphous Nd-Fe-B materials with relatively higher boron content (Nd15Fe77B10, Nd15Fe77B12, and Nd15Fe77B14 alloys). The existence of the metastable bcc α-iron phase in the amorphous matrix was confirmed by TEM studies, magnetic measurements, and in situ observation by x-ray diffraction. The formation of the metastable phase stabilized the amorphous state, increasing the crystallization temperature of the Nd2Fe14B phase.


2013 ◽  
Vol 1547 ◽  
pp. 135-140 ◽  
Author(s):  
Yarilyn Cedeño-Mattei ◽  
Myrna Reyes ◽  
Oscar Perales-Pérez ◽  
Félix R. Román

ABSTRACTThe present work focuses on the development of a reproducible and cost-effective size-controlled synthesis route for nanoscale MgO and the preliminary assessment of its bactericide capacity as a function of crystal size. Nanoscale MgO was produced through the thermal decomposition of Mg-carbonate hydrate precursor (hydromagnesite) synthesized in aqueous phase. The exclusive formation of the MgO phase, with an average crystallite size between 7 and 13 ± 1 nm, was evidenced by X-Ray Diffraction and HRTEM analyses. Fourier Transform – Infrared spectroscopy confirmed the evolution of the precursor into the desired MgO structure. The bactericidal tests were conducted by measuring the optical density at 600 nm of E. coli in presence of MgO nanoparticles of specific sizes. MgO nanocrystals with average crystallite sizes of 13nm inhibited bacterial growth up to 35% at 500 mg MgO/L. The mechanism of inhibition could be attributed to the formation of superoxide species on the MgO surface.


2019 ◽  
Vol 26 (4) ◽  
pp. 1238-1244 ◽  
Author(s):  
Edmundo Fraga ◽  
Jesus D. Zea-Garcia ◽  
Armando Yáñez ◽  
Angeles G. De la Torre ◽  
Ana Cuesta ◽  
...  

In situ research of materials under moderate pressures (hundreds of bar) is essential in many scientific fields. These range from gas sorption to chemical and biological processes. One industrially important discipline is the hydration of oil well cements. Existing capillary cells in this pressure range are static as they are easy to design and operate. This is convenient for the study of single-phase materials; however, powder diffraction quantitative analyses for multiphase systems cannot be performed accurately as a good powder average cannot be attained. Here, the design, construction and commissioning of a cost-effective spinning capillary cell for in situ powder X-ray diffraction is reported, for pressures currently up to 200 bar. The design addresses the importance of reducing the stress on the capillary by mechanically synchronizing the applied rotation power and alignment on both sides of the capillary while allowing the displacement of the supports needed to accommodate different capillaries sizes and to insert the sample within the tube. This cell can be utilized for multiple purposes allowing the introduction of gas or liquid from both ends of the capillary. The commissioning is reported for the hydration of a commercial oil well cement at 150 bar and 150°C. The quality of the resulting powder diffraction data has allowed in situ Rietveld quantitative phase analyses for a hydrating cement containing seven crystalline phases.


2019 ◽  
Author(s):  
Hao Shi ◽  
Warren Zipfel ◽  
Ilana Brito ◽  
Iwijn De Vlaminck

ABSTRACTMapping the complex biogeography of microbial communities in situ with high taxonomic and spatial resolution poses a major challenge because of the high density and rich diversity of species in environmental microbiomes and the limitations of optical imaging technology. Here, we introduce High Phylogenetic Resolution microbiome mapping by Fluorescence In-Situ Hybridization (HiPR-FISH), a versatile and cost-effective technology that uses binary encoding and spectral imaging and machine learning based decoding to create micron-scale maps of the locations and identities of hundreds of microbial species in complex communities. We demonstrate the ability of 10-bit HiPR-FISH to distinguish 1023 E. coli strains, each fluorescently labeled with a unique binary barcode. HiPR-FISH, in conjunction with custom algorithms for automated probe design and segmentation of single-cells in the native context of tissues, reveals the intricate spatial architectures formed by bacteria in the human oral plaque microbiome and disruption of spatial networks in the mouse gut microbiome in response to antibiotic treatment. HiPR-FISH provides a framework for analyzing the spatial organization of microbial communities in tissues and the environment at single cell resolution.


2020 ◽  
Vol 170 ◽  
pp. 01018
Author(s):  
Nishigandh Pande ◽  
Adinath Jambhale ◽  
Dipika Jaspal ◽  
Jalinder Ambekar ◽  
Himanshu Patil

The synthesis of cost-effective and safe polymeric nanocomposite materials has been a subject of interest and study for material science researchers. Poly (N-Methyl Aniline) –Li nanocomposite has been synthesized by a one-pot in-situ method and has been explored as an electrolyte in the battery. Poly (N-Methyl Aniline)-Li nanocomposite prepared, has been characterized by UV-visible, FTIR, FE-SEM, X-ray diffraction techniques. A mechanism of interaction of lithiumion with nitrogen at the imine site has been proposed. The charge-discharge process of poly (N-Methyl Aniline) –Li nanocomposite, when used in the battery, has been discussed.


2020 ◽  
Vol 4 (4) ◽  
pp. 1-3
Author(s):  
Liu L

The mesoporous ZSM-5 zeolite containing MoCoP/Al2O3 catalyst (C12-ZSM5) with the mixture of Al2O3 and mesoporous ZSM- 5 zeolite as carrier was synthesized. The catalytic performance of C12-ZSM5 catalyst was evaluated by the hydrodesulfurization (HDS) of different diesel feedstock. The carriers and catalysts were characterized by N2 adsorption-desorption, pyridine-FTIR, X-ray diffraction (XRD) and CO in-situ FTIR (CO-FTIR) techniques. Results showed that mesoporous ZSM-5 can improve the acidity of the catalyst and increase the number of MoCoS active phases. The C12-ZSM5 catalyst had low HDS and HDN activity, because the acidic sites of mesoporous ZSM-5 were easily occupied by nitrogen compounds. The HDS activity of C12-ZSM5 catalyst was fully exploited by using graded packing technology, the sulfur content of product oil was 5.9 ng/μL. The relative HDS activity of C12-ZSM5 catalyst is 1.47 times that of FHUDS-8 catalyst.


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