Synthesis,characterization and biological analysis of transition metal complexes with macro cyclic ligands derived from adipic acid,ethylenediamine with diethyloxalate and diethylmalonate

Macro-cyclic ligands from adipic acid, ethylenediamine with diethyloxalate and diethylmalonate and their respective metal complexes of Mn(II), Co(II), Ni(II), Cu(II), and Zn(II) with macro cyclic ligands (LO) and (LM) L [N,N′-bis(2-aminoethyl)hexanediamide] were synthesized successfully. These metal complexes were characterized by Fourier transform infrared, ultraviolet visible spectrometry, proton nuclear magnetic resonance spectroscopy, and mass Spectrometry, CHNS and thermogravimetric analysis. The elemental analysis confirms the structures for Mn(II), Co(II) and Ni(II) complexes similar to octahedral geometry, Cu(II) complexes as a square planar geometry and Zn(II) complexes in the tetrahedral geometry. The molar conductivities of all the metal complexes were taken in 10^?3 M DMSO, and values of all the metal complexes showed their electrolytic nature which indicates the presence of chloride ions. Thermal analysis supports as the metal complexes are thermally stable. The result of antimicrobial activity against various microorganisms confirms that the metal complexes are potent bactericides and fungicides than the ligand. Metal complexes of LO with Cu(II) and Zn(II) were found to be highly active against S. typhimurium than the complexes of LM.

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Disposable electrochemical flow cells for catalytic adsorptive stripping voltammetry (CAdSV) at a bismuth film electrode (BiFE)

Catalytic adsorptive stripping voltammetry (CAdSV) has been demonstrated at a bismuth film electrode (BiFE) in an injection-moulded electrochemical micro-flow cell. The polystyrene three-electrode flow cell was fabricated with electrodes moulded from a conducting grade of polystyrene containing 40% carbon fibre, one of which was precoated with Ag to enable its use as an on-chip Ag/AgCl reference electrode. CAdSV of Co(II) and Ni(II) in the presence of dimethylglyoxime (DMG) with nitrite employed as the catalyst was performed in order to assess the performance of the flow cell with an in-line plated BiFE. The injection-moulded electrodes were found to be suitable substrates for the formation of BiFEs. Key parameters such as the plating solution matrix, plating flow rate, analysis flow rate, solution composition and square-wave parameters have been characterised and optimal conditions selected for successful and rapid analysis of Co(II) and Ni(II) at the ppb level. The analytical response was linear over the range 1 to 20 ppb and deoxygenation of the sample solution was not required. The successful coupling of a microfluidic flow cell with a BiFE, thereby forming a “mercury-free” AdSV flow analysis sensor, shows promise for industrial and in-the-field applications where inexpensive, compact, and robust instrumentation capable of low-volume analysis is required.     

Determination of caffeine in black tea leaves by Fourier transform infrared spectrometry using multiple linear regression

A simple and fast analytical procedure was developed for the determination of caffeine in black tea leaves. The method is based on multiple linear regression treatment of Fourier transform infrared spectrometric data obtained in the wave number range 1800–1300 cm⁻¹ after extraction of caffeine in CHCl₃ from tea samples, wetted with an aqueous solution of NH₃ (0.1 M). The procedure requires no complex sample preparation. It provided a limit of detection of 0.035 mg/ml, a sampling frequency of 6 h⁻¹ and a coefficient of variation of 0.8% for five independent measurements of a tea sample with 3.68% w/w caffeine content. This procedure provides a drastic reduction in the consuming organic solvent for each sample compare to that of the reference chromatographic determination. The accuracy of technique is evaluated by comparing the obtained results with those of a reference HPLC technique. An average value of 3.60±0.07% w/w was obtained by HPLC for a powdered tea sample which is compromising when is compared to 3.68±0.03% (w/w) obtained by this FTIR technique.     

Separation and sensitive determination of quercetin in <Emphasis Type="Italic">Rosa canina</Emphasis> L. using solidified floating organic drop microextraction followed by high-performance liquid chromatography determination

Quercetin is a polyphenolic flavonoid found in many plants and is used as a nutritional supplement. It has been reported to have biological properties that may play an important role in the prevention of human diseases, such as cancer, cardiovascular diseases, diabetes, ulcer, cataract and allergies. In this research, solidified floating organic drop microextraction coupled to high-performance liquid chromatography was used to extract and determine quercetin in Rosa canina L., growing in different areas of Lorestan Province in Iran. The effect of important experimental variables such as type and volume of extracting organic solvent, extraction temperature and time, pH and effect of ionic strength on the extraction recovery was investigated and optimized. Under the optimum extraction conditions, a linear response was obtained over the range of 0.5–40 µg mL^?1. Relative standard deviation (RSD%) and enrichment factor were found to be 3.4% and 230, respectively. The proposed method was applied successfully for the determination of quercetin in calycles and fruit of R. canina L. samples. The results showed good agreement compared with those obtained by a validated standard method.     

Unexpected structure of a C. difficile toxin A ligand necessitates an annotation correction in a popular screening library

The structure of the pentasaccharide S259-1 in the Consortium for Functional Glycomics was investigated using a variety of techniques. Surprisingly, the structure differs from the structure assumed from the previously established specificity of the human fucosyltransferase FUT-III used in the last step of chemoenzymatic synthesis. When presented with a tetrasaccharide substrate containing both type I and type II disaccharide moieties, the enzyme generates a pentasaccharide in which the type II moiety is preferentially fucosylated. The unexpected product generated by FUT-III in this case highlights the importance of performing detailed structural analysis on products generated by enzymes.     

Comparison of photosynthetic components of wheat genotypes under rain-fed and irrigated conditions

The major environmental factor limiting the range of adaptation for wheat is drought. Fourteen wheat genotypes (Triticum aestivum L.) were grown under two environments (irrigated and rain fed) to determine physiological and photosynthetic responses to drought. Combined analysis of variance of the data showed that the environment was a significant source of variation for leaf chlorophyll content (LCC), stomatal conductance (g(s)) and grain yield (GY). Wheat genotypes differed significantly for LCC, g(s) and GY. All the measured traits under water-stress conditions except maximum photochemical efficiency of PSII (F(v)/F(m)) were lower than those under nonstress conditions. Mean GY in rain-fed conditions was 11.26% lower than that in irrigated conditions. The genotypes number 13 (Marvdasht) and 8 (M-81-13) exhibited the highest GY per unit area in both irrigation and rain-fed conditions. It was concluded that the higher LCC and g(s) under drought-stress conditions could possibly be the proper criteria for screening the drought-tolerant wheat genotypes under field conditions.