Determination of abamectin in citrus fruits using SPE combined with dispersive liquid–liquid microextraction and HPLC–UV detection

A new pretreatment method, SPE combined with dispersive liquid–liquid microextraction, was proposed for the determination of abamectin in citrus fruit samples for the first time. In this method, fruit samples were extracted by ultrasound‐assisted extraction followed by SPE. Then, the SPE was used as a disperser solvent in the next dispersive liquid–liquid microextraction step for further purification and enrichment of abamectin. The effects of various parameters on the extraction efficiency of the proposed method were investigated and optimized. Good linearity of abamectin was obtained from 0.005 to 10.0 mg/kg for B_1a and from 0.05 to 10.0 mg/kg for B_1b with correlation coefficient (r²) of 0.998 for B_1a and 0.991 for B_1b, respectively. The LODs were 0.001 and 0.008 mg/kg (S/N = 3) for B_1a and B_1b, respectively. The relative recoveries at three spiked levels were ranged from 87 to 96% with the RSD less than 11% (n = 3). The method has been successfully applied to the determination of abamectin in citrus fruit samples.     

Magnetic metal-organic frameworks for the extraction of trace amounts of heavy metal ions prior to their determination by ICP-AES

Microchimica Acta - The authors describe the preparation of two kinds of metal-organic frameworks (MOFs), referred to as TMU-8 and TMU-9. The MOFs were applied to the preconcentration of the ions...     

Influence of a nanosecond pulsed laser on aluminium alloys: Distribution of oxygen

Nanosecond laser pulses may produce both thermal melting (as femtosecond and picosecond pulses) or ultrafast nonthermal melting depending on the pulse fluence. This was demonstrated experimentally by Sokolowski-Tinten et al. [1], who found that the transformation of GaAs into its liquid state occurs within several tens of picoseconds at fluences close to the melt threshold due to thermal melting under highly superheated conditions or within several hundred femtoseconds via carrier excitation for very high fluences. The processes occurring under high energetic fs pulse irradiation could be described more precisely with the help of the theoretical work of Stampfli et al. In this work, a nanosecond pulsed laser (Nd:Yag) is used to irradiate an aluminum alloy sample. The oxygen distribution is studied as a function of distance in order to get an idea about the temperature distribution.     

The Performance of the Time-Frequency Analysis Software (TF32) in the Acoustic Analysis of the Synthesized Pathological Voice

The purpose of this study was to examine the algorithm-measuring capabilities used in the Time-Frequency Analysis Software Program for 32-bit Windows (TF32) for measuring fundamental frequency (F0), its dependent measures, and signal-to-noise ratio (SNR). The stability, accuracy, and linearity of its algorithm to systematic changes in aspiration noise and/or spectral slope (to mimic the perceptual characteristics of breathiness, roughness, and hoarseness) were evaluated using its analysis output to five female and five male synthesized voices. TF32 was used to calculate F0, Jitter%, Shimmer%, and SNR for each of the synthesized signals. The findings indicate that although TF32 produced stable results for male synthesized samples, they were not accurate when measuring F0, Jitter%, and Shimmer% with the addition of noise and variations in open quotient independently and in combination. In contrast, TF32 was neither stable nor accurate in making the same measurements for female synthesized samples. However, TF32 was stable and accurate in measuring SNR for male and most of female voices. These results point to an inappropriate F0 extraction algorithm in TF32 and stress the need for further research to remediate the algorithm or to identify a superior one.     

Modeling catalyst nucleation for carbon nanotube growth by chemical-vapor and plasma-enhanced chemical-vapor deposition methods

The nucleation of the nickel nanoparticles on substrates, a critical process in the growth of carbon nanotubes, has been modeled analytically using thermodynamic and statistical theories. It was hypothesized that during the initial stages of the annealing process smaller nanoparticles with the size of about 5 nm form and, subsequently, randomly hop to make larger nanoparticles. The minimum and maximum diameter of the nickel nanoparticles can be obtained from the derived expressions. In addition, the size-dependent probability of forming the nanoparticles was examined at various temperatures and plasma power densities in chemical-vapor deposition and plasma-enhanced chemical-vapor deposition methods, respectively. The theoretical results presented agreed very well with experimental data.     

Comparison of ultrasound-assisted emulsification and dispersive liquid–liquid microextraction methods for the speciation of inorganic selenium in environmental water samples using low density extraction solvents

Herein, ultrasound-assisted emulsification microextraction (USAEME) and dispersive liquid–liquid microextraction (DLLME) methods based on applying low-density organic solvents have been critically compared for the speciation of inorganic selenium, Se(IV) (selenite) and Se(VI) (selenate) in environmental water samples by gas chromatography-flame ionization detection (GC-FID). At pH 2 and T = 75 °C for 7 min, only Se(IV) was able to form the piazselenol complex with 4-nitro-o-phenylenediamine. Piazselenol was extracted using an extraction solvent and was injected into a GC-FID instrument for the determination of Se(IV). Conveniently, Se(VI) remained in the aqueous phase. Total inorganic selenium was determined after the reduction of Se(VI) to Se(IV) and prior to the above procedures. The Se(VI) concentration was calculated as the difference between the measured total inorganic selenium and Se(IV) content. The effect of various experimental parameters on the efficiencies of the two methods and their optimum values were studied with the aid of response surface methodology and experimental design. Under the optimal conditions, the limit of detections (LODs) for Se(IV) obtained by USAEME-GC-FID and DLLME-GC-FID were 0.05 and 0.11 ng mL⁻¹, respectively. The relative standard deviations (RSDs, n = 6) for the measurement 10 ng mL⁻¹ of Se(IV) were 5.32% and 4.57% with the enrichment factors of 2491 and 1129 for USAEME-GC-FID and DLLME-GC-FID, respectively. Both methods were successfully applied to the analysis of inorganic selenium in different environmental water samples and certified reference material (NIST SRM 1643e).     

Pyridine analogues of the antimetastatic Ru(III) complex NAMI-A targeting non-covalent interactions with albumin

A series of pyridine-based derivatives of the antimetastatic Ru(III) complex imidazolium [trans-RuCl(4)(1H-imidazole)(DMSO-S)] (NAMI-A) have been synthesized along with their sodium-ion compensated analogues. These compounds have been characterized by X-ray crystallography, electron paramagnetic resonance (EPR), NMR, and electrochemistry, with the goal of probing their noncovalent interactions with human serum albumin (hsA). EPR studies show that the choice of imidazolium ligands and compensating ions does not strongly influence the rates of ligand exchange processes in aqueous buffer solutions. By contrast, the rate of formation and persistence of interactions of the complexes with hsA is found to be strongly dependent on the properties of the axial ligands. The stability of noncovalent binding is shown to correlate with the anticipated ability of the various pyridine ligands to interact with the hydrophobic binding domains of hsA. These interactions prevent the oligomerization of the complexes in solution and limit the rate of covalent binding to albumin amino acid side chains. Electrochemical studies demonstrate relatively high reduction potentials for these complexes, leading to the formation of Ru(II) species in aqueous solutions containing biological reducing agents, such as ascorbate. However, EPR measurements indicate that while noncovalent interactions with hsA do not prevent reduction, covalent binding produces persistent mononuclear Ru(III) species under these conditions.