LiFePO4-Based Composite Electrode Material: Synthetic Approaches,Peculiarities of the Structure,and Regularities of Ionic Transport Processes

Russian Journal of Electrochemistry - This article discusses approaches to the synthesis of composite cathode materials based on lithium-intercalated transition metal phosphates (by the example of...     

Simultaneous determination of eight synthetic permitted and five commonly encountered nonpermitted food colors in various food matrixes by high-performance liquid chromatography

A simple and sensitive HPLC method has been developed for the simultaneous determination of eight permitted food colors and five commonly encountered nonpermitted colors in various food commodities, including sugar-, fat-, and starch-based food matrixes. The method uses a specific food category-based cleanup/treatment procedure before color extraction to avoid the interference of food matrixes, and to obtain the optimal color extraction. Analysis was performed on a reversed-phase C18 micro-Bondapak column with ammonium acetate and acetonitrile gradient elution as the mobile phase; a programmable lamda max-specific visible detection was used to monitor colors to obtain the higher sensitivity and expanded scope needed for multicolor blends having diverse absorption maxima. All colors showed good linearity, with regression coefficients of 0.9974-0.9999. The LOD and LOQ values ranged from 0.01 to 0.12 mg/L, and from 0.04 to 0.83 mg/L or mg/kg, respectively. The intraday and interday precision tests produced good RSD values, and the recoveries from different food matrixes ranged from 82 to 104%. The method offers high sensitivity for analysis of a wide variety of food matrixes containing a broad scope of multicolor blends. Two nonpermitted colors, orange II and metanil yellow, were found. Also, a number of samples contained permitted colors at levels two- to seven-fold higher than those prescribed.     

Microwave-assisted synthesis and reversed-phase high-performance liquid chromatographic separation of diastereomers of (R,S)-baclofen using ten chiral derivatizing reagents designed from trichloro-s-triazine

Four dichloro-s-triazine (DCT) and five monochloro-s-triazine (MCT) chiral derivatizing reagents (CDRs) were synthesized by incorporating amino acid amide moieties as chiral auxiliaries in trichloro-s-triazine and its 6-methoxy derivative, respectively. Another MCT reagent was synthesized by substitution of two chlorine atoms with two different amino acid amides in trichloro-s-triazine. These reagents were used for synthesis of diastereomers of (R,S)-baclofen under microwave irradiation (i.e. 60 s at 85% power using DCT reagents and 90 s at 85% power using MCT reagents). The diastereomers were separated on a reversed-phase C18 column using mixtures of methanol with aqueous trifluoroacetic acid (TFA) with UV detection at 230 nm. The separation behavior in terms of retention times and resolutions obtained for the two sets of diastereomers prepared with DCT and MCT reagents were compared among themselves and among the two groups. Longer retention times and better resolutions were observed with DCT reagents as compared to MCT reagents. The calibration curves were linear for both (R)- and (S)-baclofen in the concentration range 50-500 μg/ml. The average regression was 0.999 for both (R)- and (S)-baclofen. The RSD for (R)-baclofen was 0.40-0.86% for intra-day precision and 0.60-1.40% for inter-day precision and these values for (S)-baclofen were 0.52-0.75% and 0.64-1.32%, respectively. The recovery was 97.2-98.9% for (R)- and 97.0-98.9% for (S)-baclofen. The limit of detection was 1.63ng/ml and 1.52ng/ml for (R)- and (S)-baclofen, respectively.     

Identification of degraded products of aldicarb due to the catalytic behavior of titanium dioxide/polyacrylonitrile nanofiber

Photocatalytic properties of fibers containing TiO₂ nanoparticles were explored for use as a self-decontaminating material using degradation of the pesticide aldicarb as the model toxin. During the analysis of the aldicarb treated sample by liquid chromatography (LC) with diode array detector (DAD), an unidentified peak was found at relative retention time (RT) 3.9 min when compared to aldicarb and major metabolites, aldicarb sulfoxide, and aldicarb sulfone. An analytical method was developed to confirm and identify this degradation product. LC–APCI/MS techniques were used first to analyze molecular ions and major fragments comparing retention times and spectra with those of known standards. FTIR and LC–MS/MS techniques were used to confirm the identity of the degradation product as 2-propenal, 2-methyl-, O-[(methylamino)carbonyl]oxime.     

A study on the control of dye solution temperature on the line-width and wavelength stability of a copper vapour laser pumped single mode dye laser

This paper presents a study on the line-width and wavelength stability of a single mode narrow line-width (≈ 100 MHz) dye laser pumped by a copper vapour laser, with and without precision temperature control of dye solution. The single mode dye laser system was based on a specially designed SS metal dye cell and grazing incidence grating (GIG) dye resonator with intra-cavity double prism beam expander and etalon. A high precision wavelength-meter was used to record the line-width and frequency stability data. With the coarse dye solution temperature control of 23 ± 2 °C, dye laser line-width varied in a periodic fashion (in every 30 s) between 100 and 770 MHz. Frequency stability was ± 215 MHz (1 min). This is attributed to switching from single to double mode due to temperature induced cavity length change. For the precise dye solution control of 23 ± 0.1 °C, the periodic variation of the line-width was removed completely and the line-width was always ≤ 100 MHz. The frequency stability also improved to ± 42 MHz (1 min). It is established that the dye temperature control is very crucial for achieving, highly frequency stable single axial mode operation.     

High repetition rate mid-infrared generation with singly resonant optical parametric oscillator using multi-grating periodically poled MgO:LiNbO3

A high repetition rate mid-infrared singly resonant optical parametric oscillator (OPO) using MgO-doped multi-grating periodically poled LiNbO₃ (MgO:PPLN) is demonstrated. A 1064 nm Q-switched Nd:YVO₄ laser at 10 kHz repetition rate and pulse width of 17.8 ns was used to pump the OPO. The period of the quasi-phase matched (QPM) grating in the multi-grating MgO:PPLN chip varied from 25.5 to 31.5 μm in steps of 0.5 μm. This corresponds to the generation of a signal beam from 1.37 to 1.64 μm and an idler beam from 3.0 to 4.8 μm, respectively. A maximum signal power of 250 mW and idler power of 140 mW has been obtained with an input pump beam of power 1.92 W, for a grating period of 30.5 μm. A maximum optic-optic conversion efficiency of 20% and 7.4% in the idler has been observed. It has been observed that the output power increases as the period of the grating increases.     

Effect of Substrate Temperature on the Growth of Molybdenum Trioxide Thin Films

Crystallography Reports - Molybdenum oxide is one of the most important inorganic material, which exhibits several phases, such as MoO3, MoO2, Mo4O11, Mo5O14, etc. Among them, molybdenum trioxide...     

A validated LC‐MS/MS assay for simultaneous quantification of methotrexate and tofacitinib in rat plasma: application to a pharmacokinetic study

A highly sensitive, specific and rapid LC‐ESI‐MS/MS method has been developed and validated for simultaneous quantification of methotrexate (MTX) and tofacitinib (TFB) in rat plasma (50 μL) using phenacetin as an internal standard (IS), as per the US Food and Drug Administration guidelines. After a solid‐phase extraction procedure, the separation of the analytes and IS was performed on a Chromolith RP_18e column using an isocratic mobile phase of 5 m m ammonium acetate (pH 5.0) and acetonitrile at a ratio of 25:75 (v/v) using flow‐gradient with a total run time of 3.5 min. The detection was performed in multiple reaction monitoring mode, using the transitions of m/z 455.2 → 308.3, m/z 313.2 → 149.2 and m/z 180.3 → 110.2 for MTX, TFB and IS, respectively. The calibration curves were linear over the range of 0.49–91.0 and 0.40–74.4 ng/mL for MTX and TFB, respectively. The intra‐ and interday accuracy and precision values for MTX and TFB were <15% at low quality control (QC), medium QC and high QC and <20% at lower limit of quantification. The validated assay was applied to derive the pharmacokinetic parameters for MTX and TFB post‐dosing of MTX and TFB orally and intravenously to rats. Copyright © 2014 John Wiley & Sons, Ltd.