Fate of CS2 in viscose process: a chemistry perspective

Cellulose dissolution in the viscose process has been facilitated through derivatization by carbon disulphide (CS₂) at xanthation stage by converting alkali cellulose (AC) to cellulose xanthate (CX). CX formation has been always accompanied with sulphur based byproducts formation as dictated by the mechanism published in earlier study (Gondhalekar et al. (Cellulose 26 3 1595–1604, 2019)). The sulphur byproducts formed during viscose synthesis are sodium sulphide (Na₂S), sodium trithiocarbonate (Na₂CS₃: TTC) and other minor sulphur compounds. These byproducts continue to form during ripening process as dictated by time and temperature coupled with concentration of free caustic and CS₂ present in the system. These byproducts get converted into sodium sulphate (Na₂SO₄), hydrogen sulphide (H₂S), CS₂ and other sulphurous compounds during spinning. Overall, uncontrolled ripening without parametric optimization adversely impacts raw material (RM) consumption and creates sustainability challenges. Overall optimization based on viscose process fundamental insights presented in this study will effectively help in achieving operational excellence by reducing rate of undesired reactions to improve RM specific consumption and will compliment overall sustainability efforts in viscose industry.

     

Determination of Atovaquone in Human Plasma by LC-MS-MS and Its Application to a Bioequivalence Study

A sensitive and selective method for the determination of atovaquone in human plasma was developed and validated. The procedure employed the use of an internal standard (chlorothalidone) and a solvent extraction step. Detection was by electrospray ionization tandem mass spectrometry with multiple reaction monitoring. The method showed a linear range from 50 to 2,000 ng mL^?1. The extraction recovery was determined to be 84.91 ± 6.42% (SD), the intra- and inter-day assay accuracy (relative error) was within 7.57% and precision (RSD) was below 6.06%. The method was successfully employed to analyze plasma samples and evaluate the pharmacokinetics of atovaquone in human volunteers.     

A Synthesis of 1,5-DI-O-Acetyl-3-Azido-2,3-Dideoxy-D-Ribofuranose

Abstract

The renewed interest in azido-nucleosides, particularly when the aziodo group is present at position 3, has been intensified¹ since the approval of 3′-azido-thymidine (1) for the treatment of AIDS. Moreover, 3′-amino-2,3-dideoxy-nucleosides are also important due to various biological activities associated ^3-5 with them. In dealing with the synthesis of such molecules, 3-azido-2,3-dideoxy-pentoses have been realised as valuable synthons.     

Simultaneous LC Estimation of Glimepiride and Metformin in Glimepiride Immediate Release and Metformin Sustained Release Tablets

In the present study, a simple, rapid and precise liquid chromatographic method was developed and validated for the simultaneous determination of glimepiride and metformin in sustained release formulation. The separation was achieved on a Nucleosil 100-5SA column, 250 × 4.6 mm i.d., 5 μm using a mobile phase composed of 1.7 % ammonium dihydrogen phosphate buffer pH 3.0: acetonitrile (70:30 v/v).The instrumental settings were a flow rate of 1.0 ml min⁻¹ and a detector wavelength of 230 nm. The retention time of glimepiride and metformin were 5.1 and 11.3, respectively. The developed method was validated in terms of specificity, sensitivity, linearity, range, accuracy, precision and ruggedness. The proposed method was successfully applied to the sustained release pharmaceutical dosage form for the simultaneous determination of glimepiride and metformin without any interference by excipients.

     

Alternative LC–MS–MS Method for Simultaneous Determination of Proguanil, Its Active Metabolite in Human Plasma and Application to a Bioequivalence Study

An alternative rapid and sensitive liquid chromatography–tandem mass spectrometry method has been developed and validated for simultaneous analysis of proguanil (PRO) and cycloguanil (CYC) in human plasma. The analytes were extracted from human plasma by solid phase extraction. Riluzole (RIL) was used as an internal standard for proguanil and cycloguanil. A HyPURITY Advance C18 column provided chromatographic separation of analytes followed by detection with mass spectrometry. The method involves simple isocratic chromatography conditions and mass spectrometric detection in the positive ionization mode using an API-4000 system. The proposed method has been validated with linear range of 1.5–150.0 ng mL^?1 for PRO and 0.5–50.0 ng mL^?1 for CYC. The inter-run and intra-run precision values are within 2.54, 9.19% for PRO and 1.99, 10.69% for CYC at LOQ levels. The overall recoveries for PRO and CYC were 102.52 and 106.72%, respectively. Total elution time was as low as 2.50 min. This validated method was used successfully for analysis of plasma samples from a bioequivalence study.     

Synthesis and characterization of excess magnesium MgB2 superconductor under inert carbon environment

The structural, transport and magnetic properties of MgB₂ superconductor heavily blended with Mg is studied. The samples are synthesized with a new approach in both, pressed carbon environment and in flowing argon. The excess magnesium used is observed to play dual role: one being the prevention of Mg losses during the synthesis process and hence maintaining the stoichiometry of MgB₂ phase, and second being the formation of Mg milieu probably all around the MgB₂ grains to give a dense structure. Excess Mg also improves the grain connectivity by going into the pores and there by minimizing the insulating junctions. The residual resistivity of the sample is observed to decrease from 57.02 μΩ cm to 10.042 μΩ cm as it is progressively filled with superconductor–normal–superconductor (SNS) type junctions amongst the grains by the virtue of increased magnesium content. The synthesized samples devoid of porosity show the superconducting transition, T_c in the range of 39–34 K as of clean MgB₂ samples, though overloaded with Mg. The excess Mg resulted in enhanced critical current density, J_c from 6.8 × 10³ A cm^?2 to 5.9 × 10⁴ A cm^?2 at 20 K and 10 kOe, with reasonable decrease in the superconducting transition. Thus our samples being overloaded with Mg impart mechanical strength and competitive superconducting properties, which forms a part of interest.     

Core–shell nanostructures and nanocomposites of Ag@TiO2: effect of capping agent and shell thickness on the optical properties

Two different shell-forming reagents viz. titanium isopropoxide and titanium hydroxyacylate, have been employed to obtain core–shell nanostructures of Ag@TiO₂. However, nanocomposites were formed when the shell-forming agent, titanium isopropoxide, was added before breaking the micelles. Titanium hydroxyacylate has been used for the first time as a shell-forming agent which resulted in uniform core–shell structures of Ag@TiO₂ with core diameter ranging from 10 to 40 nm and a shell thickness of 10–50 nm. The low rate of hydrolysis of titanium hydroxyacylate than titanium isopropoxide (used in other methods) appears to be responsible for the uniform shell thickness. The presence of capping agent (2-mercaptoethanol) disrupts the formation of a uniform shell structure of Ag@TiO₂. HRTEM, IR, and XPS studies of Ag@TiO₂ synthesized using capping agent show the formation of Ag₂S coated with an amorphous layer of TiO₂. A red shift of 25 and 10 nm was observed in the surface plasmon band of silver for Ag@TiO₂ core–shell structures (compared with that of silver nanoparticles) synthesized using titanium hydroxyacylate and titanium isopropoxide, respectively. The presence of capping agent (2-mercaptoethanol) masks the surface plasmon peak. Photoluminescence studies show an increase in the emission intensity for the core–shell structures when compared to that of TiO₂ nanoparticles.     

Effect of complexing agent on the properties of electrochemically deposited Cu2ZnSnS4 (CZTS) thin films

The Cu₂ZnSnS₄ (CZTS) thin films have been electrochemically deposited on Mo-coated glass substrate from weak acidic medium (pH 4.5-5) at room temperature. The effect of complexing agent (tri-sodium citrate) on the structural, morphological and compositional properties of CZTS thin films has been investigated. The as-deposited and annealed thin films were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM),EDAX and X-ray photoelectron spectroscopy (XPS) techniques for their structural, morphological, compositional and chemical properties, respectively. XRD studies reveal that the amorphous nature of as-deposited thin film changes into polycrystalline with kesterite crystal structure after annealing in Ar atmosphere. The film prepared without complexing agent showed well-covered surface morphology on the substrate with some cracks on the surface of the film whereas those prepared using complexing agent, exhibited uneven and slightly porous and some overgrown particles on the surface of the films. After annealing, morphology changes into the flat grains, uniformly distributed over the entire surface of the substrate. The EDAX and XPS study reveals that the films deposited using 0.2 M tri-sodium citrate are nearly stoichiometric.     

La2O3/TFE： An efficient system for room temperature synthesis of Hantzsch polyhydroquinolines

Lanthanum oxide（La2O3） in combination with 2,2,2-trifluoroethanol（TFE） was found to be an efficient system for the one-pot, four-component synthesis of Hantzsch polyhydroquinoline derivatives from aromatic aldehydes, dimedone, ethyl acetoacetate and ammonium acetate at ambient temperature. The catalyst is heterogeneous and reusable, hence can be separated easily and reused. The present method is featured by mild reaction conditions, use of heterogeneous catalyst, non-chromatographic purification,short reaction time and high yields, which make it an attractive route for the synthesis of polyhydroquinolines.