Phytochemical investigation and antifeedant activity of Premna latifolia leaves

The essential oil of Premna latifolia Roxb. was obtained by hydrodistillation of fresh leaves of the plant having an oil yield of 0.05%, both non-polar and essential oil were analysed by GC and GC-MS. Hexane fraction of the leaves of P. latifolia was transesterified and analysed by GC and GC-MS, 40 non-polar components were identified comprising 89.3%. The most abundant fatty acid constituents were hexadecanoic acid (25.04%), 8,11,14-docosatrienoic acid (13.62%), octadecanoic acid (6.82%), 9,12-octadecadienoic acid (4.19%) and 29 components were investigated in the essential oil which comprises 78.1%. The most abundant oil constituents were 1-octen-3-ol (35.69%), terpendiol II (7.19%), δ-guaiene (7.49%) 2-undecanone (4.80%) and α-pinene (3.27%). Different extracts were also tested against polyphagous crop pest Spodoptera litura for antifeedant activity. Essential oil showed maximum growth reduction of 56.83% followed by chloroform extract of 43.93%.     

Determination of organophosphate pesticides at a carbon nanotube/organophosphorus hydrolase electrochemical biosensor

An amperometric biosensor for oganophosphorus (OP) pesticides based on a carbon nanotube (CNT)-modified transducer and an organophosphorus hydrolase (OPH) biocatalyst is described. A bilayer approach with the OPH layer atop of the CNT film was used for preparing the CNT/OPH biosensor. The CNT layer leads to a greatly improved anodic detection of the enzymatically generated p-nitrophenol product, including higher sensitivity and stability. The sensor performance was optimized with respect to the surface modification and operating conditions. Under the optimal conditions the biosensor was used to measure as low as 0.15 μM paraoxon and 0.8 μM methyl parathion with sensitivities of 25 and 6 nA/μM, respectively.     

Enhanced ionic conductivity in novel nanocomposite gel polymer electrolyte based on intercalation of PMMA into layered LiV3O8

In the present work, a novel polymer electrolyte based on poly(methyl methacrylate) (PMMA)/layered lithium trivanadate (LiV₃O₈) nanocomposite has been investigated. X-ray diffraction (XRD) study shows that d-spacing is increased from 6.3?±?0.1 Å to 12.8?±?0.1 Å upon intercalation of the polymer into the layered LiV₃O₈. Room temperature ionic conductivity of the obtained nanocomposite gel polymer electrolyte is found to be superior to that of conventional PMMA-based gel polymer electrolyte. Enhancement in ionic conductivity of the nanocomposite gel electrolyte is attributed to the formation of a two-dimensional channel as a result of decreased interaction between Li⁺ and V₃O ₈ ^? layers as confirmed by FTIR. SEM results show aggregation of nanocomposite particles resulting from extension of some of the polymer chains from interlayer to the edge providing paths for Li⁺ ion transport. Interfacial stability of nanocomposite gel electrolyte is also found to be better than that of the conventional PMMA-based gel polymer electrolyte.     

New catanionic surfactants, phase stability and synthesis of ultrafine CdS nanoparticles

A systematic study on the water-intake capacity of the microemulsion formed using a catanionic surfactant (synthesized by taking equimolar mixture of acid and amine) with varying hydrocarbon chain length of the acid has been carried out. A decrease in the water-intake capacity with increase in the chain length was observed. Shorter chain length of co-surfactant (1-butanol compared to 1-octanol) led to higher water-intake capacity of microemulsions which may also be attributed to the high hydrophilic-lipophilic balance (HLB) of 1-butanol. Three new microemulsions based on catanionic surfactants have been used to synthesize quantum dots of CdS. The size of CdS quantum dots decreased with increase in chain length of the acid component of the catanionic surfactant.     

Trace determination of parabens in cosmetics and personal care products using fabric‐phase sorptive extraction and high‐performance liquid chromatography with UV detection

A simple, fast, and sensitive analytical protocol using fabric‐phase sorptive extraction followed by high performance liquid chromatography with ultraviolet detection has been developed and validated for the extraction of five parabens including methylparaben, ethylparaben, propylparaben, butylparaben, and benzylparaben. In the present work, sol‐gel polyethylene glycol coated fabric‐phase sorptive extraction membrane is used for the preconcentration of parabens (polar) from complex matrices. The use of fabric‐phase sorptive extraction membrane provides a high surface area which offers high sorbent loading, shortened equilibrium time, and overall decrease in the sample preparation time. Various factors affecting the performance of fabric‐phase sorptive extraction, including extraction time, eluting solvent, elution time, and pH of the sample matrix, were optimized. Separation was performed using a mobile phase consisting of water:acetonitrile (63:37; v/v) at an isocratic elution mode at a flow rate of 0.9 mL/min with wavelength at 254 nm. The calibration curves of the target analytes were prepared with good correlation coefficient values (r² > 0.9955). The limit of detection values range from 0.252 to 0.580 ng/mL. Finally, the method was successfully applied to various cosmetics and personal care product samples such as rose water, deodorant, hair serum, and cream with extraction recoveries ranged between 88 and 122% with relative standard deviation <5%.     

Stability‐indicating HPLC method for simultaneous quantification of 14 impurities in excedrin tablet formulations and identification of new impurity by LC–MS in accelerated stability studies

We developed novel stability‐indicating HPLC method for simultaneous estimation of 14 impurities in excedrin tablet, a formulation with a combination of acetaminophen, aspirin, and caffeine. In addition, a new impurity that was generated through degradation of aspirin at high temperatures during the accelerated stability conditions was positively identified and confirmed, using liquid chromatography–mass spectrometry technique. The HPLC method was optimized using the Inertsustain C₁₈, 250 × 4.6 mm, 5.0 μm column, employing simple gradient method. Forced degradation studies were performed under acidic, basic, oxidative and thermal conditions to prove the scope and stability‐indicating the nature of the method. The optimized method was validated as per the International Conference on Harmonization guidelines. The HPLC method showed linearity from LOQ concentration to 21 μg mL^?1. Precision and intermediate precision values were <5% RSD. The validated HPLC method is currently applied for the routine testing of excedrin tablet formulations in quality control laboratories.     

RP-HPLC method for simultaneous estimation of lamivudine, tenofovir disoproxil fumarate and efavirenz in tablet formulation

A simple, rapid, and precise reversed-phase high-performance liquid chromatographic method for the simultaneous determination of lamivudine, tenofovir disoproxil fumarate and efavirenz in bulk and tablet dosage form has been developed and validated. Chromatography was performed on a 150 mm × 4.6 mm i.d., 5-μm particle, Phenomenex Luna C₁₈ column with 30: 45: 25 (v/v/v) acetonitrile: methanol: water as mobile phase at a flow rate of 0.5 mL/min. UV detection was done at 258 nm; lamivudine, tenofovir disoproxil fumarate and efavirenz were eluted with retention times of 3.27, 4.58 and 10.90 min, respectively. The method was validated in accordance with ICH guidelines. Validation revealed the method is specific, rapid, accurate, precise, reliable and reproducible. Calibration plots were linear over the concentration ranges 1–6 μg/mL for lamivudine and tenofovir disoproxil fumarate and 2–12 μg/mL for efavirenz. Limits of detection were 0.05, 0.09 and 0.11 μg/mL and limits of quantification were 0.15, 0.28 and 0.34 μg/mL for lamivudine, tenofovir disoproxil fumarate and efavirenz, respectively. The high recovery and low coefficients of variation confirm the suitability of the method for the simultaneous determination of these three drugs in bulk and tablets.     

Fly ash supported NiO as an efficient catalyst for the synthesis of xanthene and its molecular docking study against plasmodium glutathione reductase

A novel fly ash supported NiO (FA–NiO) nanocomposite solid heterogeneous catalyst has been prepared by impregnation of Ni(NO₃)₂ · 6H₂O on thermally activated fly ash (FA) support. FT-IR spectroscopy, X-ray diffraction analysis, scanning electron microscopy, TEM and BET techniques were employed to characterize the catalyst. The catalytic adeptness of FA–NiO was tested and optimized in xanthene formation. Catalyst gave very high yield and good purity. Stability of the catalyst could be promising as it easily recovered and reused giving a similar yield up to four cycles. FA–NiO is an efficient catalyst providing an environmentally clean process for xanthene formation and for developing a revolutionary way to use the majority of waste fly ash. Further, we have also performed docking simulation between 1ONF and a xanthene molecule to evaluate binding orientation and affinity of the ligand.     

Vitamin B6 cofactor derived chemosensor for the selective colorimetric detection of acetate anions

A novel vitamin B₆ cofactor derived anion sensor L for the selective colorimetric detection of acetate has been developed by the condensation of pyridoxal and 2-aminothiophenol. The sensor L showed a noteworthy change in the visible region of the spectrum and was detected by the ‘naked-eye’ for both acetate and fluoride anions in DMSO but selectively for acetate in DMSO/H₂O (88:12, v/v). The anion recognition ability of L was investigated by spectroscopic (UV–vis and ¹H NMR) and DFT methods.     

A visual strip sensor for determination of iron

A visual strip has been developed for sensing iron in different aqueous samples like natural water and fruit juices. The sensor has been synthesized by UV-radiation induced graft polymerization of acrylamide monomer in microporous poly(propylene) base. For physical immobilization of iron selective reagent, the in situ polymerization of acrylamide has been carried out in the presence of 1,10-phenanthroline. The loaded strip on interaction with Fe(II) in aqueous solution turned into orange red color and the intensity of the color was found to be directly proportional to the amount of Fe(II) in the aqueous sample. The minimal sensor response with naked eye was found for 50 ng mL⁻¹ of Fe in 15 min of interaction. However, as low as 20 ng mL⁻¹ Fe could be quantified using a spectrophotometer. The detection limit calculated using the 3s/S criteria, where ‘s’ is the standard deviation of the absorbance of blank reagent loaded strip and ‘S’ is the slope of the linear calibration plot, was 1.0 ng mL⁻¹. The strip was applied to measure Fe in a variety of samples such as ground water and fruit juices.