Amperometric sensing of hydrogen peroxide using a glassy cabon electode modified with silver nanoparticles on poly(alizarin yellow R)

A sensitive amperometric sensor for hydrogen peroxide (HP) was constructed that is based on a glassy carbon electrode (GCE) modified with silver nanoparticles on poly(alizarin yellow R). The polymer was electropolymerized onto the surface of the GCE by cyclic voltammetry (CV), and the AgNPs were then electrodeposited onto its surface. The electrode was characterized by scanning electron microscopy and CV, and used for amperometric determination of HP. The electrode exhibits a favorable catalytic activity towards the reduction of HP, with a linear response range from 1.0???M to 450???M and a detection limit of 0.32???M. The sensor also displays high selectivity, excellent reproducibility, and good long-term stability.

Feasibility of light-emitting diode uses for annular reactor inner-coated with TiO2 or nitrogen-doped TiO2 for control of dimethyl sulfide

Limited environmental pollutants have only been investigated for the feasibility of light‐emitting diodes (LED) uses in photocatalytic decomposition (PD). The present study investigated the applicability of LEDs for annular photocatalytic reactors by comparing PD efficiencies of dimethyl sulfide (DMS), which has not been investigated with any LED‐PD system, between photocatalytic systems utilizing conventional and various LED lamps with different wavelengths. A conventional 8 W UV/TiO₂ system exhibited a higher DMS PD efficiency as compared with UV‐LED/TiO₂ system. Similarly, a conventional 8 W visible‐lamp/N‐enhanced TiO₂ (NET) system exhibited a higher PD efficiency as compared with six visible‐LED/NET systems. However, the ratios of PD efficiency to the electric power consumption were rather high for the photocatalytic systems using UV‐ or visible‐LED lamps, except for two LED lamps (yellow‐ and red‐LED lamps), compared to the photocatalytic systems using conventional lamps. For the photocatalytic systems using LEDs, lower flow rates and input concentrations and shorter hydraulic diameters exhibited higher DMS PD efficiencies. An Fourier‐transformation infrared analysis suggested no significant absorption of byproducts on the catalyst surface. Consequently, it was suggested that LEDs can still be energy‐efficiently utilized as alternative light sources for the PD of DMS, under the operational conditions used in this study.     

Tris(hydroxymethyl)aminomethane-modified magnetic microspheres for rapid affinity purification of lysozyme

A novel affinity purification method for lysozyme (LZM) based on functionalized magnetic microspheres was developed. Tris(hydroxymethyl)aminomethane (Tris)-modified magnetic microspheres with specific affinity toward LZM were prepared using Tris as ligand and silica-coated magnetic microshperes as support. Transmission electron microscopy and magnetic property measurement results showed that the Tris-modified magnetic microspheres have a very good core-shell structure and high magnetization.The maximum binding capacity of LZM was about 108.6 mg/g magnetic microspheres. LZM purified from chicken egg white had high purity and well-maintained activity of 8140 U/mg. This magnetic-mediated LZM purification strategy has advantages of high efficiency, low cost and easy operation.     

Synthesis, Crystal Structure, and Biological Activity of Naphthalen-2-y1-4-methyl-1,2,3-thiadiazole-5-carboxylate

The title compound naphthalen-2-y1-4-methy1-1,2,3-thiadiazole-5-carboxylate(C14H10N2O2S,Mr = 270.31)was synthesized by the reaction of 4-methyl-1,2,3-thiadiazole-5-carbonyl chloride with 2-naphthol,and its structure was characterized by IR,1H NMR,high-resolution mass spectrometry and single-crystal X-ray diffraction.The crystal belongs to orthorhombic,space group Pbcn with a = 23.475(5),b = 9.6640(19),c = 10.814(2)(A°),β = 90.00°,Z= 8,V= 2453.2(9)(A°)3,Mr = 270.30,Dc = 1.464 g/cm3,μ= 0.262 mm-1,F(000)= 1120,R = 0.0444 and wR = 0.1099.X-ray analysis revealed that the thiadiazole and naphthalene rings were non-planar,while,the thiadiazole ring and the ester group were essentially planar,and two intermolecular hydrogen bonds C(6)-H(6)…O(1)and C(14)-H(14)…O(1)were observed.The preliminary biological test showed that the title compound had antifungal and antivirus activities against tobacco mosaic virus.     

Characterization and Identification of a Chymotryptic Hydrolysate of Alpha-Lactalbumin Stimulating Cholecystokinin Release in STC-1 Cells

Alpha-lactalbumin hydrolysate is of significant interest, due to its potential application as a source of bioactive peptides in nutraceutical and pharmaceutical domains. This study was focused on the cholecystokinin (CCK) family compounds which are small peptides involved in the satiety control. The action of chymotryptic hydrolysate of alpha-lactalbumin on cholecystokinin release from intestinal endocrine STC-1 cells was investigated. We demonstrated for the first time that a chymotryptic hydrolysate of alpha-lactalbumin was able to highly stimulate CCK-releasing activity from STC-1 cells. The peptidic hydrolysate was characterized by LC/MS and MS/MS, thus highlighting the presence of 11 fractions containing 21 peptides, each potentially having the desired activity.     

Simultaneous multiresidue determination of 48 pesticides in Yeongsan and Sumjin River water using GC-NPD and confirmation via GC-MS

In a continuation of our earlier work, a multiresidual analytical method using 48 frequently used neutral pesticides in a water matrix was developed and validated in this study. The samples were extracted with dichloromethane and the pesticides were analyzed via GC-NPD followed by confirmation with GC-MS. Good linearity was detected over a concentration range of 0.01-1.0 microg/mL with correlation coefficients (r(2) ) in excess of 0.982. The recoveries were measured between 70.7 and 111.4% for the majority of the targeted pesticides with relative standard deviations (RSDs) of less than 20%. The LODs and LOQs were in ranges of 0.1-2 and 0.33-6.6 microg/L, respectively. A total of 66 water samples were collected from different locations in Yeongsan and the Sumjin River, Republic of Korea, and were analyzed in accordance with the developed method. None of the water samples were determined to contain any of the targeted pesticides. The method has been shown to be simpler, faster, and more cost-effective than the method established by the Environmental Protection Agency (EPA).     

N-heterocyclic carbene-silver complexes: Potential conductive materials for silver pastes in electronic applications

New organosilver complexes, silver(I) tetraalkylbis(benzimidazolidene) halide [1a-3a] and silver(I) dimethyl-N,N′-hexyl(imidazolyl) bromide [4a], were synthesized and incorporated into electroconductive silver pastes. Complex 3a had a 15-fold higher conductivity than conventional silver salt pastes, specifically silver(I) hexanoate, and exhibited a smooth, homogeneous surface after reductive heat-treatment of the silver paste. While the conductivity of silver(I) hexanoate can be increased by up to 33% by the addition of a supporting silver source, such as Ag₂O, the conductivity of 3a was markedly decreased by Ag₂O treatment. Thus, 3a can be used in silver pastes with moderate conductivity and can reduce the amount of conventional silver supporting materials without loss of electroconductivity.     

Seasonal variations in metabolite profiling of the fruits of Ligustrum lucidum Ait

The metabolite profiling of fruits of the herb Ligustrum lucidum Ait collected during different months has been performed using ultra-performance liquid chromatography with quadrupole time-of-flight mass spectrometry (UPLC/QTOFMS) and multivariate statistical analysis techniques. The markers such as oleuropein acid, neonuezhenide, specnuezhenide, oleuropein and ligustrosidic acid accountable for such variations were identified through the loadings plot of principal component analysis (PCA), and the tentative identification of the markers is completed by comparing the mass spectra and retention times with those of reference compounds and/or tentatively assigned by matching empirical molecular formulae and MS/MS data with those of the known compounds published. Furthermore, one of the chemical markers, such as specnuezhenide, which is water-soluble, biologically active and also the predominant compound in this crude drug, was quantified by ultra-performance liquid chromatography coupled with a tunable UV detector (UPLC-TUV). The developed UPLC method provides good linearity (r(2)=0.9991), repeatability (RSD=2.96%), intra- and inter-day precisions (RSD=0.21%, 0.96%), with accuracies of 99.18-100.26% and a recovery of specnuezhenide of 97.57%. The fruits of L. lucidum Ait collected from August to December were tested. The results clearly show that the fruits of L. lucidum Ait harvested in October have the highest yields of specnuezhenide. It is also noted that the variations of content of specnuezhenide obtained by both methods have a strong correlation. This suggests that the newly proposed strategy is a reliable and simple method for the rapid discrimination of subtle variations, within the same plant species or strains, due to different seasonal collection times.     

Simple and accurate quantitative analysis of seven prohibited threshold substances in human urine by liquid chromatography/tandem mass spectrometry in doping control

A simple and accurate liquid chromatography/tandem mass spectrometry (LC/MS/MS) method has been developed and validated for the quantitative determination of ephedrine, pseudoephedrine, methylephedrine, cathine, salbutamol, morphine and epitestosterone in human urine. Urine samples were spiked with internal standard and diluted with acetonitrile. After centrifugation, the supernatants were directly analyzed by LC/MS/MS using the selected reaction monitoring (SRM) mode. The linearity, intra- and inter-day precision, accuracy, limit of detection (LOD) and limit of quantification (LOQ) were evaluated and the method was found to be accurate and reproducible for the quantitation of threshold substances. When the method was applied to the analysis of blind urine samples for the proficiency test, the results were close to the nominal concentrations, within 87.7-106.6% of nominal values, suggesting that the developed methods can be successfully applied to routine doping analyses.