Development and Validation of a Reliable UHPLC-MS/MS Method for Simultaneous Quantification of Macrocyclic Lactones in Bovine Plasma

A fast, accurate and reliable ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) method was developed for simultaneous quantification of ivermectin (IVER), doramectin (DORA), and moxidectin (MOXI) in bovine plasma. A priority for sample preparation was the eradication of possible infectious diseases to avoid travel restrictions. The sample preparation was based on protein precipitation using 1% formic acid in acetonitrile, followed by Ostro^® 96-well plate pass-through sample clean-up. The simple and straightforward procedure, along with the short analysis time, makes the current method unique and suitable for a large set of sample analyses per day for PK studies. Chromatographic separation was performed using an Acquity UPLC HSS-T3 column, with 0.01% acetic acid in water and methanol, on an Acquity H-Class ultra-high performance liquid chromatograph (UHPLC) system. The MS/MS instrument was a Xevo TQ-S^® mass spectrometer, operating in the positive electrospray ionization mode and two multiple reaction monitoring (MRM) transitions were monitored per component. The MRM transitions of m/z 897.50 > 753.4 for IVER, m/z 921.70 > 777.40 for DORA and m/z 640.40 > 123.10 for MOXI were used for quantification. The method validation was performed using matrix-matched calibration curves in a concentration range of 1 to 500 ng/mL. Calibration curves fitted a quadratic regression model with 1/x2 weighting (r ≥ 0.998 and GoF ≤ 4.85%). Limits of quantification (LOQ) values of 1 ng/mL were obtained for all the analytes, while the limits of detection (LOD) were 0.02 ng/mL for IVER, 0.03 ng/mL for DORA, and 0.58 ng/mL for MOXI. The results of within-day (RSD < 6.50%) and between-day (RSD < 8.10%) precision and accuracies fell within acceptance ranges. No carry-over and no peak were detected in the UHPLC-MS/MS chromatogram of blank samples showing good specificity of the method. The applicability of the developed method was proved by an analysis of the field PK samples.     

Modeling of the mode dynamics generated by Madison Symmetric Torus machine utilizing a modified sine-Gordon equation

In this paper, a new dynamic model is presented for the experimental data generated by the Madison Symmetric Torus (MST) machine. The model is based on a modified sine-Gordon (SG) dynamic equation. The modified sine-Gordon equation model effectively captures the behavior of the slinky mode in reversed-field pinch experiments. In addition, this paper demonstrates how the derived model accurately describes the behavior of the localized magnetohydrodynamic mode (slinky mode) that appears in reversed-field pinch toroidal magnetic confinement systems. The modified SG equation model is solved analytically by using the perturbation method. The resulting model is fit to match a variety of experimental results in the MST reversed-field pinch experiment. The efficacy of the newly developed model in effectively representing the slinky mode is verified by comparing obtained analytical solution to experimentally measured data.     

Electron-ion recombination in a helium plasma produced by laser

Experimental investigation of the recombination coefficients in a helium plasma produced by laser is reported. The relative contribution of electronic collision processes and of atomic collision processes on the values of the recombination coefficients are pointed out according to the value of the neutral pressure of helium.     

Acoustic Analysis Findings in Objective Laryngopharyngeal Reflux Patients

OBJECTIVE: The aim of this study was to identify the effects of objective laryngopharyngeal reflux (LPR) on the acoustic parameters of patients by comparing their voice samples with that of control subjects. STUDY DESIGN: Prospective study in two tertiary reference hospitals. METHODS: 48 consecutive patients with symptoms related to LPR and 64 control subjects were included in the study. Suspected LPR patients underwent a 24-hour ambulatory pH monitoring, and 25 (52%) of them were shown to have objective LPR. Acoustical evaluation results of objective LPR patients were compared with that of symptomatic LPR patients and control subjects. RESULTS: All frequency perturbation values obtained from objective and symptomatic LPR patients were higher than the control subjects (P<0.01). Mean fundamental frequency, amplitude perturbation measures, and noise-to-harmonics ratio were not significantly different between groups. CONCLUSION: LPR patients have significantly different frequency perturbation values than control subjects.     

The kinetics study of the reduction of Fast Green dye with cetylpyridinum chloride as cationic surfactant

The kinetics of the reaction of Fast Green dye (FG) with cetylpyridinum chloride was studied in alkaline medium by UV-Visible spectrophotometer. Reduction of Fast Green dye was carried out by varying the fast green dye concentration, cetylpyridinum chloride concentration and concentration of sodium hydroxide. In the present study the reduction of dye was carried out in order to reduce the color content. The interaction of dye was carried out with reducing analyte (cetylpyridinum chloride). The rate of the reaction was determined by varying the above parameters at different temperatures. It was observed that the reduction followed pseudo first-order kinetics with respect to dye, surfactant, OH⁻ ion concentration according to the following reaction pathway. The mechanism for the photo bleaching of the dye has been proposed and well confirmed by the data simulation procedure. The activation parameters of the reaction like entropy of activation (ΔS) and free energy of activation (ΔG) showed the extremely solvated states of transient complex which was less disorderly arranged than the oxidized form of dye, whereas E _a values reflects a high amount of energy required for the reduction of dye with cetylpyridinum chloride.     

A facile preparation of donut-like supramolecular tannic acid-Fe(III) composite as biomaterials with magnetic,conductive, and antioxidant properties

Tannic acid (TA) complexes with various metal ions are prepared in buffer solutions by readily adjusting the pH, but there is no normalizing method to produce ferric tannate complexes. In this study, TA-Fe(III) complex was prepared in reverse microemulsion medium by reaction of TA as ligand with Fe(III) in 1:3 ligand:metal ion molar ratio. The complex was characterized by SEM, AFM, FT-IR, elemental analysis, AAS measurement, and Brunauer-Emmett-Teller (BET) method. Furthermore, magnetic susceptibility was tested with the Gouy method, and electronic spectral studies of TA-Fe(III) complex were completed with solid UV–vis measurements. The thermal stability was also studied by TGA analysis. These studies show that the ligand molecules have octahedral arrangement around Fe(III) and the complex is paramagnetic. The bandgap energy of the complex was calculated as 3.42 eV with solid UV–vis analysis. To determine antioxidant activity of the complex, Total Phenol Content (TPC) and Trolox Equivalent Antioxidant Concentration (TEAC) methods were used. The complex has great antioxidant properties with TPC = 45 ± 1 mg L^?1 GAE and TEAC = 296 ± 2 mM trolox g^?1 for dry sample.     

Switchable solvent based liquid phase microextraction of palladium coupled with determination by flame atomic absorption spectrometry

A switchable solvent-based micro-extraction method for pre-concentration and separation of ultratrace palladium was developed prior to its flame atomic absorption spectrometric detection. Reverse change of hydrophilicity of N,N-dimethylcyclohexylamine (DMA) was achieved by reaction with carbonated water. The hydrophilic bicarbonate salt of the protonated DMA was used as extractant for palladium complexed with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP). Formation of the hydrophobic form of switchable solvent from hydrophilic form of switchable solvent phase was achieved by addition of sodium hydroxide into the extractant-sample solution. The effect of key parameters affected extraction recovery was studied and optimised by using Plackett–Burman design, central composite design and three dimension (3D) surfaces response. The calibration plot was linear in the range 0.015–1.6 mg L^?1 of palladium with a correlation coefficient of 0.999. The limit of detections values of palladium for liquid and solid samples were 4.28 μg L^?1 and 0.54 µg g^?1, respectively. The pre-concentration factor was 37.5. The accuracy was confirmed by determination of palladium in certified reference material. The procedure was also applied for determination of palladium content of real samples as automotive catalytic converter, roadside dust, sea water and river water.