Simultaneous Determination of Olanzapine and Fluoxetine by HPLC

A rapid, specific reversed phase HPLC method has been developed for simultaneous determination of olanzapine and fluoxetine in their formulations. Chromatographic separation of these two pharmaceuticals was carried out on an Inertsil C₁₈ reversed phase column (150 mm × 4.6 mm, 5 μm) with a 40:30:30 (v/v/v) mixture of 9.5 mM sodium dihydrogen phosphate (pH adjusted to 6.8 ± 0.1 with triethylamine), acetonitrile and methanol as mobile phase. The flow rate 1.2 mL min⁻¹ and the analytes are monitored at 225 nm. Paroxetine was used as internal standard. The assay results were linear from 25 to 75 μg mL⁻¹ for olanzapine (r ² ≥ 0.995) and 100–300 μg mL⁻¹ for fluoxetine (r ² ≥ 0.995), showed intra- and inter-day precision less than 1.0%, and accuracy of 97.7–99.1% and 97.9–99.0%. LOQ was 0.005 and 0.001 μg mL⁻¹ for olanzapine and fluoxetine, respectively. Separation was complete in less than 10 min. Validation of the method showed it to be robust, precise, accurate and linear over the range of analysis.     

Fractional distribution of graphene oxide and its potential as an efficient and reusable solid catalyst for esterification reactions

Graphene oxide (GrO) prepared by the Hummers method was separated into three different fractions (GrO₅₀₀₀, GrO₂₀₀₀, and GrO_res) on the basis of their dispersion stability in the water. Infrared, nuclear magnetic resonance, X‐ray photoelectron spectroscopy, and elemental analyses revealed that GrO₅₀₀₀ possesses a high degree of oxygen functionalities including phenolic, carboxylic, and ?OSO₂H groups, compared with the other fractions. The GrO₅₀₀₀ was found to be a highly efficient and reusable solid catalyst for the esterification of various carboxylic acids with a variety of alcohols to furnish corresponding esters in high to excellent yields. The catalytic activity of the GrO₅₀₀₀ was attributed to the ability of highly polar GrO₅₀₀₀ scaffold to adsorb/attract reactants, where the acid functionalities of GrO₅₀₀₀ facilitated the esterification process efficiently. The chemical and structural features of GrO₅₀₀₀ were discussed to understand the improved catalytic activity compared with GrO₂₀₀₀ and conventional solid acid catalysts. Copyright © 2014 John Wiley & Sons, Ltd.     

Nonlinear Optical Switching in Regioregular Porphyrin Covalent Organic Frameworks

Covalent organic frameworks (COFs) have garnered immense scientific interest among porous materials because of their structural tunability and diverse properties. However, the response of such materials toward laser‐induced nonlinear optical (NLO) applications is hardly understood and demands prompt attention. Three novel regioregular porphyrin (Por)‐based porous COFs—Por‐COF‐HH and its dual metalated congeners Por‐COF‐ZnCu and Por‐COF‐ZnNi—have been prepared and present excellent NLO properties. Notably, intensity‐dependent NLO switching behavior was observed for these Por‐COFs, which is highly desirable for optical switching and optical limiting devices. Moreover, the efficient π‐conjugation and charge‐transfer transition in ZnCu‐Por‐COF enabled a high nonlinear absorption coefficient (β=4470 cm/GW) and figure of merit (FOM=σ₁/σ_o, 3565) value compared to other state‐of‐the‐art materials, including molecular porphyrins (β≈100–400 cm/GW), metal–organic frameworks (MOFs; β≈0.3–0.5 cm/GW), and graphene (β=900 cm/GW).     

Normal- and Reversed-Phase Thin-Layer Chromatography of Three Structurally Related Organophosphorus Pesticides of Forensic Importance

JPC – Journal of Planar Chromatography – Modern TLC - Recently, considerable numbers of poisoning cases have been reported owing to the ingestion of three structurally related...     

The effect of spin dilution on magnetism of the linear chain system β-Cu2?xZnxV2O7

We have measured the magnetic susceptibility (χ) and heat capacity (C _p) of β-Cu_2−x Zn _x V₂O₇ (x = 0, 0.05, 0.1, 0.15, 0.2, 0.3, 2) in the temperature range 2–300 K. A one-dimensional alternating exchange Heisenberg antiferromagnetism (HAF) is observed in all compositions with chains of infinite length. The intra-chain exchange remains uniform and decreases marginally with dilution of the magnetic state. A cooperative ordering is seen in the magnetic chains for all Zn concentrations (x ≤ 0.3). The temperature of occurrence of this transition decreases with increasing Zn concentration. Though the conventional spin-wave theory has been used here to describe the properties of the ordered phase, the presence of some contributions like the lattice heat capacity in C _p and the Curie-Weiss term in susceptibility introduces some uncertainties in the estimation of the proportions contributed by the spin system. Therefore, the nature of the ordered phase could not be ascertained unambiguously.     

Effect of a small disruption of the Ca site on the geometrically frustrated magnetic behavior of Ca3CoRhO6

The compound, Ca₃CoRhO₆, containing magnetic Co-Rh chains intervened by Ca ions, has been known to be one of the few exhibiting ‘partially disordered antiferromagnetic structure (PDA)’ due to geometrical frustration. Here, we report the influence of partial replacement of Ca by Y on the magnetic anomalies by investigating the solid solution, Ca_3−xY _xCoRhO₆, by bulk measurements. There are profound changes in the magnetic behavior, the most notable one being that the features attributable to spin-chain magnetism and PDA structure get suppressed dramatically by a small replacement of Ca by Y (x<0.3), despite the fact that the magnetic chain is not disrupted. This finding suggests that this compound is on the verge of PDA-structural-instability.