Development of a corn flour certified reference material for the accurate determination of zearalenone.

A certified reference material (CRM, KRISS 108-01-002) for zearalenone in corn flour was developed to assure reliable and accurate measurements in testing laboratories. Commercially available corn flour underwent freeze-drying, pulverization, sieving, and homogenization. The final product was packed in amber bottles, approximately 14 g per unit, and preserved at -70 °C. 13C18-Zearalenone was used as an internal standard (IS) for the certification of zearalenone by isotope-dilution liquid chromatography-tandem mass spectrometry (ID-LC‒MS/MS) and for the analysis of α-zearalenol, ß-zearalenol, and zearalanone by LC‒MS/MS. The prepared CRM was sufficiently homogeneous, as the among-unit relative standard deviation for each mycotoxin ranged from 2.2 to 5.7 %. Additionally, the stability of the mycotoxins in the CRM was evaluated under different temperature conditions and scheduled test periods, including storage at -70°C, -20°C, and 4°C and room temperature for up to 12 months, 6 months, and 1 month, respectively. The content of each target mycotoxin in the CRM remained stable throughout the monitoring period at each temperature. Zearalenone content (153.6 ± 8.0 µg/kg) was assigned as the certified value. Meanwhile, the contents of α-zearalenol (1.30 ± 0.17 µg/kg), ß-zearalenol (4.75 ± 0.33 µg/kg), and zearalanone (2.09 ± 0.16 µg/kg) were provided as informative values.

Stereo-Controlled Synthesis of Vicinal Tertiary Carbinols: Application in the Synthesis of a Diol Substructure of Zaragozic Acid, Pactamycin and Ryanodol.

A novel and flexible approach for the stereo-controlled synthesis of vicinal tertiary carbinols is reported. The developed strategy featured a highly diastereoselective singlet-oxygen (O2 1 ) [4+2] cycloaddition of rationally designed cyclohexadienones (derived from oxidative dearomatization of the corresponding carboxylic-acid appended phenol precursors), followed by programmed "O-O" and "C-C" bond cleavage. In doing so, a highly functionalized and versatile intermediate was identified and prepared in synthetically useful quantity as a plausible precursor to access a variety of designed and naturally occurring vicinal tertiary carbinol containing compounds. Most notably, the developed strategy was successfully applied in the stereo-controlled synthesis of advanced core structures of zaragozic acid, pactamycin and ryanodol.

Fabrication of Ni/TiO2 visible light responsive photocatalyst for decomposition of oxytetracycline.

Nickel-impregnated TiO2 photocatalyst (NiTP) responding to visible light was prepared by the liquid phase plasma (LPP) method, and its photoactivity was evaluated in degrading an antibiotic (oxytetracycline, OTC). For preparing the photocatalyst, nickel was uniformly impregnated onto TiO2 (P-25) powder, and the nickel content increased as the number of LPP reactions increased. In addition, the morphology and lattice of NiTP were observed through various instrumental analyses, and it was confirmed that NiO-type nanoparticles were impregnated in NiTP. Fundamentally, as the amount of impregnated nickel in the TiO2 powder increased sufficiently, the band gap energy of TiO2 decreased, and eventually, the NiTP excited by visible light was synthesized. Further, OTC had a decomposition reaction pathway in which active radicals generated in OTC photocatalytic reaction under NiTP were finally mineralized through reactions such as decarboxamidation, hydration, deamination, demethylation, and dehydroxylation. In effect, we succeeded in synthesizing a photocatalyst useable under visible light by performing only the LPP single process and developed a new advanced oxidation process (AOP) that can remove toxic antibiotics.

Preparation of Cellulose-Based Activated Carbon Fibers with Improved Yield and Their Methylene Chloride Adsorption Evaluation.

The recent rapid growth of the battery industry has led to a rapid increase in methylene chloride emissions. Methylene chloride causes health and social problems in humans. In this study, cellulose-based activated carbon fibers (CACFs) with improved yield were prepared for the removal of methylene chloride. The concentration of ammonium phosphate in the pretreatment controlled the crosslink density of cellulose fibers and improved the yield. From the results, the specific surface area and total pore volume of cellulose-based activated carbon fibers pretreated with ammonium phosphate (AP-CACFs) were determined to be 1920-2060 m2/g and 0.83-1.02 cm3/g, respectively, and the total yield improved by 6.78-11.59% compared to that of CACFs (4.97%). In particular, a correlation between the textural properties of CACFs and methylene chloride adsorption/desorption behavior was obtained. This correlation can be used to develop efficient adsorbents for methylene chloride removal.

Development of isotope dilution-liquid chromatography/tandem mass spectrometry as a candidate reference method for the accurate determination of patulin in apple products.

The incidence of patulin (PAT) in fruit products is a worldwide concern due to its acute and chronic toxic effects. Therefore, accurate and reliable PAT measurements are important for preventing consumer health risks. Our previous method, which was based on a common technique that uses ethyl acetate extraction and liquid chromatography-tandem mass spectrometry with isotope dilution (ID-LC-MS/MS), has shown great performance for the determination of PAT in apple products. However, prolonged extraction times and multistep clean-up processes were required to sufficiently eliminate the matrix interferences. Herein, a feasible alternative ID-LC-MS/MS method was successfully established, employing simplified and reliable sample preparation steps. The clean-up process was performed using molecularly imprinted polymer-solid-phase extraction (MIP-SPE) cartridges, which eliminated matrix interferences and facilitated the trace quantification. While the previous method used a multimode LC column for the retention of polar patulin, the current method used a UPLC HSS T3 column, which further improved the peak sharpness and reduced the run time. The method was validated by measuring fortified samples in the concentration range of 5‒100 µg/kg. The accuracy varied between 97.8 and 102.0%, with relative standard deviation for interday and intraday precision being below 3%. The measurement uncertainty was lower than 4% (at a 95% level of confidence). Therefore, this method demonstrated adequate metrological quality with greatly enhanced performance over various reported methods. Additional key benefits of this method are easy manipulation, short preparation time, and lower consumption of hazardous solvents. Finally, the method was successfully applied to commercially available apple-based products.

Comparison of Pore Structures of Cellulose-Based Activated Carbon Fibers and Their Applications for Electrode Materials.

This study presents the first investigation of cellulose-based activated carbon fibers (RACFs) prepared as electrode materials for the electric double-layer capacitor (EDLC) in lieu of activated carbon, to determine its efficacy as a low-cost, environmentally friendly enhancement alternative to nanocarbon materials. The RACFs were prepared by steam activation and their textural properties were studied by Brunauer-Emmett-Teller and non-localized density functional theory equations with N2/77K adsorption isotherms. The crystallite structure of the RACFs was observed by X-ray diffraction. The RACFs were applied as an electrode material for an EDLC and compared with commercial activated carbon (YP-50F). The electrochemical performance of the EDLC was analyzed using galvanostatic charge/discharge curves, cyclic voltammetry, and electrochemical impedance spectroscopy. The results show that the texture properties of the activated carbon fibers were influenced by the activation time. Crucially, the specific surface area, total pore volume, and mesopore volume ratio of the RACF with a 70-min activation time (RACF-70) were 2150 m2/g, 1.03 cm3/g and 31.1%, respectively. Further, electrochemical performance analysis found that the specific capacitance of RACF-70 increased from 82.6 to 103.6 F/g (at 2 mA/cm2). The overall high specific capacitance and low resistance of the RACFs were probably influenced by the pore structure that developed outstanding impedance properties. The results of this work demonstrate that RACFs have promising application value as performance enhancing EDLC electrode materials.

A Study on Superior Mesoporous Activated Carbons for Ultra Power Density Supercapacitor from Biomass Precursors.

A kenaf-derived activated carbon (KAC) for a high-power density supercapacitor was developed in this study through phosphoric acid activation. The N2/77K isothermal adsorption-desorption curve was used to estimate the textural properties of KAC based on BET and BJH and the pore size distribution based on NLDFT. The electrochemical properties of KAC were analyzed by using the coin-type cell applying 1 M SPBBF4/PC electrolyte, and the specific surface area and total pore volume were 1490-1942 m2/g and 1.18-3.18 cm3/g, respectively. The pore characteristics of KAC varied according to the activation temperature, and most KAC showed a mesoporous structure. As the activation temperature increased, the mesopore volume increased up to 700 °C, then decreased. The mesoporous structure of KAC resulted in a substantial decrease in the Warburg impedance as the ion diffusion resistance decreased. Hence, the specific capacitance of KAC decreased from 82.9 F/g to 59.48 F/g as the charge-discharge rate increased from 1 mA/g to 10 mA/g, with the rate of reduction at approximately 30%. The rate of reduction of KAC's specific capacitance was 50% lower compared with commercial activated carbon; hence, KAC is a more suitable electrode-active material for high power density supercapacitors.

Comparison of the Characteristics of Recycled Carbon Fibers/Polymer Composites by Different Recycling Techniques.

In this study, three recycling methods, namely, mechanical grinding, steam pyrolysis, and the supercritical solvent process, which are used to acquire recycled carbon fibers (RCFs), were compared for their application in synthesizing polymer-matrix composites. RCF-reinforced polyethylene (PE) composites were prepared to compare the mechanical properties of the composites generated using the three recycling methods. The PE/RCF composites exhibited 1.5 times higher mechanical strength than the RCF-reinforced PE composites, probably because of the surface oxidation effects during the recycling processes that consequently enhanced interfacial forces between the RCF and the matrix. Further, the steam pyrolysis process showed the highest energy efficiency and can thus be applied on a large production scale in domestic recycled CF markets.

All-fiber integrated saturable absorber-tunable wavelength filter for Q-switching laser in both C- and L-bands.

We proposed and experimentally demonstrated combining a nonlinear optic saturable absorber and a wideband-tunable spectral filter in a single graphene oxide (GO) film deposited fiber optic device. The GO film was prepared on the cleaved facet of an optical fiber applying two sequential processes: the electrical deposition to make a thick GO film using an arc fusion splicer, followed by the laser pulse drilling to form a multi-layered GO film. The GO deposited fiber facet and a pristine fiber facet formed an asymmetric Fabry-Perot interferometer (FPI), whose spectral response was flexibly controlled by adjusting the air gap between them. An all-fiber ring laser cavity was built using the proposed device as a tunable saturable absorber along with erbium-doped fiber as a gain medium in the L-band. Stable Q-switching laser pulse trains were successfully generated, whose pulse duration was in the order of a few microseconds and its peak wavelength was tunable over 40nm from 1564 to 1604nm covering both C-and L-bands. At a certain condition, we also obtained Q-switching pulses simultaneously lasing at the double wavelengths, 1573.3 and 1586.7nm. Detailed device fabrication processes and laser characteristics are described to elucidate the high potential of 2-dimensional material films in nonlinear optics.

Decomposition of naproxen by plasma in liquid process with TiO2 photocatslysts and hydrogen peroxide.

Naproxen (NPX), one of the representative non-steroidal anti-inflammatory drug (NSAID) ingredients, was decomposed by plasma in liquid process (PiLP). Strongly oxidized species generated in the plasma field of the PiLP, such as OH radicals, were confirmed by optical emission spectroscopy Increasing the operation parameters (pulse width, frequency and applied voltage) of the power supply promoted plasma field generation and OH radical generation, and affected the NPX decomposition rate. Although the NPX decomposition reaction rate was improved by up to 18-30% by adding TiO2 photocatalyst powder and H2O2 to PiLP, but the optimal addition amount should be determined considering the plasma generation and scavenger effects. A decomposition pathway was proposed, in which NPX was mineralized into CO2 and H2O through five intermediates mainly by decarboxylation, demethylation, hydroxylation, and dehydration reactions via hydroxyl radicals.

Protective Effects of Gintonin on Reactive Oxygen Species-Induced HT22 Cell Damages: Involvement of LPA1 Receptor-BDNF-AKT Signaling Pathway.

Gintonin is a kind of ginseng-derived glycolipoprotein that acts as an exogenous LPA receptor ligand. Gintonin has in vitro and in vivo neuroprotective effects; however, little is known about the cellular mechanisms underlying the neuroprotection. In the present study, we aimed to clarify how gintonin attenuates iodoacetic acid (IAA)-induced oxidative stress. The mouse hippocampal cell line HT22 was used. Gintonin treatment significantly attenuated IAA-induced reactive oxygen species (ROS) overproduction, ATP depletion, and cell death. However, treatment with Ki16425, an LPA1/3 receptor antagonist, suppressed the neuroprotective effects of gintonin. Gintonin elicited [Ca2⁺]i transients in HT22 cells. Gintonin-mediated [Ca2⁺]i transients through the LPA1 receptor-PLC-IP3 signaling pathway were coupled to increase both the expression and release of BDNF. The released BDNF activated the TrkB receptor. Induction of TrkB phosphorylation was further linked to Akt activation. Phosphorylated Akt reduced IAA-induced oxidative stress and increased cell survival. Our results indicate that gintonin attenuated IAA-induced oxidative stress in neuronal cells by activating the LPA1 receptor-BDNF-TrkB-Akt signaling pathway. One of the gintonin-mediated neuroprotective effects may be achieved via anti-oxidative stress in nervous systems.

Characteristics of hydrogen production by photocatalytic water splitting using liquid phase plasma over Ag-doped TiO2 photocatalysts.

Hydrogen production from water was investigated by applying liquid plasma (LPP) to photocatalytic splitting of water. The optical properties of LPP due to water emission were also evaluated. The correlation between the optical properties of plasma and the formation of active species in water was investigated with the photocatalytic activity of hydrogen production. TiO2 was also doped with Ag to evaluate the effect of enhancing photocatalytic activity. The photocatalytic activity was evaluated by the rate of hydrogen production, and the effect of hydrogen formation was also investigated by injecting methanol as an additive. As a result of examining the luminescence properties of LPP, it showed high luminescence in the 309 nm UV region and the 656 nm visible region. The hydrogen doping rate was increased in the Ag-doped TiO2 photocatalyst. Ag-doped TiO2 has wider light absorption into the visible region and narrower band gap. Due to these properties, the rate of hydrogen generation is superior to TiO2 photocatalysts. The photochemical reaction with LPP and photocatalyst in aqueous solution with CH3OH showed a significant increase in hydrogen production rate. The increase in hydrogen production by injection of additives is because the optical properties of generating OH radicals are improved and CH3OH is decomposed to act as an electron donor to improve hydrogen production.

Bias reduction in the quantitative analysis of a target analyte present in a limited quantity in human plasma using dual-mode heart-cutting two-dimensional liquid chromatography coupled with isotope dilution mass spectrometry.

Dual-mode heart-cutting two-dimensional liquid chromatography (DMHC 2D-LC) was applied to isotope dilution mass spectrometry (IDMS) to reduce the bias in the quantitative analysis of a target analyte present in a limited quantity in human plasma. Based on a Waters I-Class LC system, the DMHC 2D-LC system was operated in one- and two-dimensional modes to facilitate the determination of heart-cutting time and the efficient trapping of the target LC eluate. Experiments to determine the feasibility of coupling with IDMS were performed with triple quadrupole mass spectrometry using folic acid standards and/or 13 C5 -folic acid. To validate the performance of the DMHC 2D-LC/IDMS system on a complex sample, human plasma was analyzed for folic acid and the result was compared with that obtained using conventional single-column LC. The total run time of the DMHC 2D-LC system was 20 min, the same as that of the single-column LC system. The peak profile of the spiked 13 C5 -folic acid obtained with single-column LC/MS was affected by matrix effects, but resolved with DMHC 2D-LC/MS, thus improving the accuracy of the analysis. The DMHC 2D-LC/IDMS system showed reliable performance in analyzing the target analyte in human plasma, eliminating matrix effects and saving analysis time.

Removal of toluene using ozone at room temperature over mesoporous Mn/Al2O3 catalysts.

The catalytic oxidation of toluene with ozone at room temperature was carried out over hierarchically ordered mesoporous catalysts (CeO2 (meso), Mn2O3 (meso), ZrO2 (meso), and γ-Al2O3 (meso)) and Al2O3 with various textural properties and phases (γ-Al2O3 (meso), γ-Al2O3 (13 nm), and α-Al2O3) to examine the effects of the nature of the catalyst on the catalytic activity. The catalysts were characterized by N2-physisorption measurements, powder X-ray diffraction, temperature programmed reduction, X-ray photoelectron spectroscopy and scanning transmission electron microscopy with energy dispersive spectroscopy. Among the ordered mesoporous catalysts, γ-Al2O3 (meso) had the highest toluene removal efficiency because of its highest surface area and pore volume, which in turn was selected for further investigation. Manganese (Mn) was introduced to various Al2O3 to improve the toluene removal efficiency. Comparing the Mn-loaded catalysts supported on various Al2O3 with different crystalline phases or pore structures, Mn/γ-Al2O3 (meso), had the highest catalytic activity as well as the highest CO2/CO ratio. The higher activity was attributed to the larger surface area, weaker interaction between Mn and Al2O3, and larger portion of Mn2O3 phase. The increase in ozone concentration led to an improvement in the carbon balance but this enhancement was insufficient due to the deposition of by-products on the catalyst. After long term tests at room temperature, the reaction intermediates and carbonaceous deposits of the used catalysts were identified.

Preparation and Characterization of Bimetallic Fe-Ni Oxide Nanoparticles Using Liquid Phase Plasma Process.

The Fe-Ni oxide bimetallic nanoparticles (FNOBNPs) were synthesized in the liquid phase plasma (LPP) method employed an iron chloride and nickel chloride as metal precursors. The sphericalshaped FNOBNPs were synthesized by the LPP process and, the size of particles was growing along with the progression of LPP reaction. The synthesized FNOBNPs were comprised of Fe3O4 and NiO. Iron had a higher reduction potential than nickel and resulted in higher iron composition in the synthesized FNOBNPs. The control of molar ratio of metal precursors in initial reactant solution was found that it could be employed as a means to control the composition of the elements in FNOBNP.

Facile Synthesis of Chromium Oxide on Activated Carbon Electrodes for Electrochemical Capacitor Application.

Chromium oxide/carbon nanocomposites (COCNC) were synthesized by using a liquid phase plasma process, and the electrical properties of the supercapacitor electrode were investigated. Spherical chromium oxide (Cr2O3) nanoparticles with the size of 100-150 nm were dispersed uniformly on activated carbon powder surface. The quantity of chromium oxide nanoparticle precipitate increased with increasing LPP reaction time and the specific capacitance of COCNC increased with increasing LPP reaction time.

Fast recovery process of carbon fibers from waste carbon fibers-reinforced thermoset plastics.

In this work, we report a fast recycling process for carbon fiber-reinforced thermosetting resin matrix composites, to obtain recycled carbon fibers. Steam (H2O) was selected as an oxidant to decompose the resin of the composites. The recycling reaction temperature and time were set in the range of 600-800 °C and 60 min, respectively. The recovery yield, surface morphologies, and mechanical properties including tensile strength and modulus of the recovered fibers were measured to evaluate the recycling efficiency. Microstructural properties of the recycled fiber were observed by X-ray studies, and the correlation of mechanical properties of the fibers with crystallite size and distribution was also evaluated. In conclusion, the carbon fibers were successfully recycled, while retaining 65% and 100% of the fibers' original tensile strength and modulus, respectively. 100% recovery yield was achieved in 60 min of decomposition time and 140 min of total process time.

Optimization and Application of Paper-Based Spray Ionization Mass Spectrometry for Analysis of Natural Organic Matter.

In this study, paper-based ionization techniques-paper spray ionization (PSI) and paper spray chemical ionization (PSCI)-were evaluated and applied for high-resolution mass spectrometry (MS)-based analysis of natural organic matter (NOM). Methanol:isopropyl alcohol (50:50, v/v) and ethanol emerged as good spray solvents for PSI, and hexane:dichloromethane (50:50, v/v) was a good spray solvent for PSCI. PSI-MS spectra could be obtained with NOM samples on the microgram scale, which is a critical advantage over conventional electrospray ionization (ESI)-MS when the amount of available sample is limited. In addition, PSI is more tolerant to salt contamination than ESI for NOM analysis. PSCI preferentially ionized less polar compounds, which may not be ionized well using ESI. Therefore, PSCI can be used as a complementary method to ESI or PSI. Comparison of the numbers of peaks obtained with ESI-, PSI-, and PSCI-MS showed that employing PSI and PSCI can increase the number of compounds that can be detected by high-resolution MS. In conclusion, the data presented in this study showed that PSI and PSCI are suitable ionization techniques for NOM analysis. To the best of our knowledge, this is the first study evaluating and applying PSI and PSCI for NOM analysis.

Enhanced Electrochemical Performance of Carbon Nanotube with Nitrogen and Iron Using Liquid Phase Plasma Process for Supercapacitor Applications.

Nitrogen-doped carbon nanotubes (NCNTs) and iron oxide particles precipitated on nitrogen-doped carbon nanotubes (IONCNTs) were fabricated by a liquid phase plasma (LPP) process for applications to anode materials in supercapacitors. The nitrogen element and amorphous iron oxide nanoparticles were evenly disseminated on the pristine multiwall carbon nanotubes (MWCNTs). The electrochemical performance of the NCNTs and IONCNTs were investigated and compared with those of pristine MWCNTs. The IONCNTs exhibited superior electrochemical performance to pristine MWCNTs and NCNTs. The specific capacitance of the as-fabricated composites increased as the content of nitrogen and iron oxide particles increased. In addition, the charge transfer resistance of the composites was reduced with introducing nitrogen and iron oxide.

Paper Spray Chemical Ionization: Highly Sensitive Ambient Ionization Method for Low- and Nonpolar Aromatic Compounds.

Sensitivity is an important factor determining successful mass spectrometry (MS) analysis of metabolome, protein, drugs, and environmental samples. Currently, nanoelectrospray ionization (ESI) is widely used as a sensitive ionization method. However, application of nano-ESI is limited to polar molecules and there is no atmospheric pressure ionization technique developed that can be used for MS analysis of low- and nonpolar compounds with sensitivity that can match with nano-ESI. Herein, we propose paper spray chemical ionization (PSCI) as an ionization technique that can be used to analyze low- and nonpolar aromatic compounds with high sensitivity. PSCI is based on paper spray ionization utilizing corona discharge phenomenon. PSCI can sensitively and quantitatively detect down to picogram (or femtomole) levels of low- and nonpolar aromatic compounds.