Validated TLC-densitometry method for the simultaneous analysis of pyrethroid insecticides in agricultural and domestic products

ABSTRACT: BACKGROUND: Pyrethroids are widely used for the control of pests and insects, as pyrethroids are believed to pose very little risk to human health and environment. However, exposure to the pyrethroids exceeding the label directions might adversely affect human health and environment. Hence a careful selection of environment friendly household product is required that must contain exactly the label claimed pyrethroids amount. RESULTS: A sensitive and robust TLC-densitometric method for simultaneous quantification of commonly used synthetic pyrethroids including esbiothrin, alpha-cypermethrin and cis/trans permethrin in agricultural and domestic products has been developed and validated. TLC aluminum plates, precoated with 0.2 mm thick layer of silica gel 60 F-254, were used for chromatographic process. Densitometric analysis of chromatoplates was carried out in absorbance mode at corresponding lamdamax of each pyrethroid. Equally valid common mobile phase for all pyrethroids consisted of hexane-dichloromethane-ethylacetate-formic acid (8:1.5:0.4:0.1 v/v/v/v) which provided sharp and symmetrical peaks of esbiothrin, alpha-cypermethrin, trans-permethrin and cis-permethrin, at Rf 0.31, 0.53, 0.6 and 0.65, respectively. Linear regression data for respective calibration curves showed a good linearity for all pyrethroids with r = 0.991-0.996. Limits of detection (LOD) and limits of quantification (LOQ) for all pyrethroids were found in the range of 1.6-2.8 and 4.9-8.5 ng/spot, respectively. CONCLUSIONS: The developed method is applicable for separating the mixture of pyrethroids and at the same time, it is also valid for separating their isomers. The method is reproducible, precise and accurate for the quantitative determination of pyrethroids in agricultural and domestic products.     

Double Suzuki cross‐coupling reaction of pyrimidine boronic acid: synthesis of new versatile dielectrophile

The double Suzuki cross‐coupling reaction has successfully been applied for the synthesis of 5,5′‐(5‐butoxy‐1,3‐phenylene)bis(2‐chloropyrimidine) with two reactive chloro groups and an alkoxy side chain starting from 2‐chloropyrimidin‐5‐ylboronic acid and 1,3‐dibromo‐5‐butoxybenzene. The reactivity of this dielectrophile was tested by reaction with aniline and phenol, a nitrogen and oxygen nucleophile, respectively. The new dielectrophile would further provide an ideal platform for the construction of large hetero‐atom bridged macrocycles for desired properties and functions in supramolecular and material chemistry. Copyright © 2012 John Wiley & Sons, Ltd.     

Cobalt titanate–cobalt oxide composite thin films deposited from heterobimetallic precursor

A single molecular heterobimetallic complex, [Co₂Ti(μ₃‐O)(TFA)₆(THF)₃] (1) [TFA = trifluoroacetate, THF = tetrahydrofuran], was synthesized, structurally and spectroscopically characterized and implemented as a single‐source precursor for the preparation of CoTiO₃–CoO composite thin films by aerosol‐assisted chemical vapour deposition (AACVD). The precursor complex was prepared by interaction of Co(OAc)₂.4H₂O [OAc = (CH₃COO^?)] with Ti(iso‐propoxide)₄ in the presence of trifluoroacetic acid in THF, and was analysed by melting point, CHN, FT‐IR, single‐crystal X‐ray diffraction and thermogravimetric analysis. The precursor complex thermally decomposed at 480 °C to give a residual mass corresponding to a CoTiO₃–CoO composite material. Good‐quality crystalline CoTiO₃–CoO composite thin films deposited at 500 °C by AACVD and characterized through powder X‐ray diffraction and scanning electron microscopy/energy‐dispersive X‐ray spectroscopy show that the crystallites have a rose‐flower‐like morphology with an average petal size in the range of 2–6 µm. Copyright © 2012 John Wiley & Sons, Ltd.     

Structural Characterization of Graphene Nanosheets for Miniaturization of Potentiometric Urea Lipid Film Based Biosensors

The present article describes a miniaturized potentiometric urea lipid film based biosensor on graphene nanosheets. Structural characterization of graphene nanosheets for miniaturization of potentiometric urea lipid film based biosensors have been studied through atomic force microscopy (AFM) and transmission electron microscopy (TEM) measurements. UV‐Vis and Fourrier transform IR (FTIR) spectroscopy have been utilized to study the pre‐ and postconjugated surfaces of graphene nanosheets. The presented potentiometric urea biosensor exhibits good reproducibility, reusability, selectivity, rapid response times (～4 s), long shelf life and high sensitivity of ca. 70 mV/decade over the urea logarithmic concentration range from 1×10^?6 M to 1×10^?3 M.     

Gold-surface binding of molecular switches studied by M?ssbauer spectroscopy

The nonanuclear coordination compound [Mo^IV{(CN)Fe^III(3-methyl-saldptn)}₈]Cl₄ exhibits multiple spin transitions (3-methyl-saldptn = N,N′-bis(3′′-methyl-2′′-hydroxy-benzyliden)-1,7-diamino-4-azaheptane). This spin crossover cluster is bound via a self-assembled monolayer onto a two dimensional array gold surface. M?ssbauer spectroscopy indicates that the thermally and optically induced spin crossover of the compound is maintained. Thereby, the foundation for its potential practical application (e.g. in the field of information storage) was laid.     

A Novel One Pot Synthesis of o‐Nitrophenylacetic Acid and Unexpected p‐Nitrobenzoic Acid by HNO3‐Mediated CH2 Extrusion Reaction of Phenylacetic Acid

The HNO₃‐mediated CH₂ extrusion reactions of phenylacetic acid lead to one pot synthesis of unexpected commercially important product 4‐nitrobenzoic acid through the formation of 4‐nitrophenylacetic acid and 2‐nitrophenylacetic acid.     

Effect of transmission fiber and amplifier noise on optical chaos synchronization

Optical chaos propagation has few constraints peculiar to itself which do not become as significant in conventional nonchaotic optical communication. We have investigated the effects of transmission fiber nonlinearities, dispersion and noise of erbium doped fiber amplifier (EDFA) on chaotic signal synchronization in lumped and distributed configuration. It is found that the effects of fiber dispersion can be easily compensated; however, the effects of fiber nonlinearity on chaos cannot be overdone and must be avoided. Three distinct configurations with different combinations of standard telecommunication fiber, dispersion compensation fiber and lumped and distributed EDF for amplification are analysed. The results are compared in terms of sync diagrams and noise figure. The chaos after propagation through distributed amplification performs better as compared to lumped amplification. Also, a new quantitative measure for the calculation of deviation in sync diagram of chaos is introduced.