Evaluation of pigments from methanolic extract of Tagetes erecta and Beta vulgaris as antioxidant and antibacterial agent

The Total Phenolic Content (TPC), antioxidant and antibacterial activities of methanolic extract of Marigold flower (MF) (Tagetes erecta) and Beet root (BR) (Beta vulgaris) were examined. The present work reveals that MF contained greater amount of TPC (42.5 mg/g GAE) as compared to BR (39.4 mg/g GAE). Methanolic extract of MF exhibited excellent DPPH free radical scavenging power (IC₅₀ 0.0716 mg/mL) and reducing power at 1 mg/mL concentration. Similar results have been obtained in FTC and TBA method. The results of antibacterial test indicated that the methanolic extract of MF and BR is significantly effective against both type of Gram-negative (Escherichia coli, Shigella dysenteriae) and Gram-positive (Bacillus subtilis, Staphylococcus aureus) bacterial strains. Therefore, the present study suggests that the Marigold and BR are promising source of herbal medicinal products with noteworthy antioxidant and antibacterial activity.     

A specific HPLC-UV method for the determination of cysteine and related aminothiols in biological samples

We present a highly selective and sensitive method for the determination of cysteine (Cys) and related aminothiols that play important roles in health and disease. The key step in the analysis is treatment with 1,1′-thiocarbonyldiimidazole (TCDI) that rapidly and quantitatively reacts with both the amino and thiol groups to form stable cyclic dithiocarbamates with intense UV absorption. Cys, homocysteine (hCys), and cysteinylglycine in plasma (75 μl), urine (100 μl), or cerebrospinal fluid (100–500 μl) were determined by separating and measuring their cyclic derivatives by a high performance liquid chromatograph (HPLC) connected to a UV detector. The chromatograms obtained using TCDI contained fewer and better-resolved peaks than those produced by less selective reagents used previously. Using chemically similar 2-methylcysteine as the internal standard, high repeatability (variation of less than 5%) and adequate sensitivity to detect small increments (10–20%) in the concentrations of cysteinylglycine and hCys were achieved. The HPLC method can also be modified to measure -penicillamine (greater than 0.8 μM) in plasma (50 μl) providing a potential method to monitor plasma levels of this drug in patients.     

Green chemical synthesis of fluorinated 1,3,5-triaryl-s-triazines in aqueous medium under microwaves as potential antifungal agents

Reasonable pure fluorinated s-triazines were synthesized in quantitative yield (96-99%) in 2-3 min in aqueous medium under microwaves, by reaction of fluorinated anilines and aqueous formaldehyde. All synthesized compounds have been screened in vitro for their antifungal activity against Rhizoctonia solani, Fusarium oxysporum, and Collectotrichum capsici.     

Thermal characterization of piezoelectric and non-piezoelectric Lead Meta-Niobate

Powerful tools like Differential Scanning Calorimetry (DSC) and DTA seem to be under-utilized for the emerging materials for high temperature piezoelectric sensors, while thermal aspects of such piezoelectric phase change are also of theoretical interest. Curie temperature of Lead Meta-Niobate (PbNb₂O₆ or PN) is 570 °C, much higher than that for widely used lead zirconate titanate, making PN potentially more attractive at high temperatures. However, the only specific heat measurement for PN appears to be the 2–25 K study by Lawless, leaving the Curie temperature region unexplored. For PN, piezoelectricity is possible for the meta-stable orthorhombic structure only. So, we prepared pure phase orthorhombic PN by quenching (Q) and the rhombohedral PN by slow-cooling (S). We report for the first time, to our knowledge, DSC across the Curie temperature for Q and S types of PN. We find clear and interesting DSC signals at the Curie temperature in heating and cooling graphs for quenched (Q) PbNb₂O₆ only and none for the slow-cooled (S) PbNb₂O₆.     

Specific determination of cysteine and penicillamine through cyclization to 2-thioxothiazolidine-4-carboxylic acids

A very simple and highly specific method for the determination of cysteine and penicillamine is presented. Treatment with 1,1'-thiocarbonyldiimidazole in slightly basic solutions converts cysteine rapidly and quantitatively to a very stable derivative, 2-thioxothiazolidine-4-carboxylic acid, which is not formed by thiols or amines. The cyclic derivative has a characteristic UV spectrum with a maximum at 272 nm and it can be quantified by one of two ways. (1) When only inorganic ions and common additives are present, a spectrophotometer or a plate reader capable of handling multiple samples is sufficient to estimate cysteine in the concentration range of 2-150 muM. Penicillamine is determined similarly by cyclization to 5,5-dimethyl-2-thioxothiazolidine-4-carboxylic acid. The method is also applicable to derivatives of cysteine modified only at the carboxyl group. (2) To determine cysteine in complex mixtures, a liquid chromatograph connected to a UV detector is used. The elution is rapid with well-separated peaks for the thiazolidine derivatives. The detection limit is 2 pmole of cysteine or penicillamine per injection and the detector response is linear up to 1 nmole. The usefulness of the method is demonstrated by determining cysteine and penicillamine in capsules and by measuring cysteine in a dietary supplement.     

Microwave assisted green chemical synthesis of novel spiro[indole-pyrido thiazines]: a system reluctant to be formed under thermal conditions

Spiro [3H-indole-3,2′-[4H] pyrido [3,2-e]-1,3-thiazine]-2,4′ (1H) diones, a class of previously unknown compound which does not form under conventional conditions, can be prepared by treatment of ‘in situ’ generated 3-indolylimine derivatives with 2-mercaptonicotinic acid under microwave irradiation in absence of any solvent or solid support in 85-92% yields in 3-8 min. The facile one pot reaction is generalized for a variety of ketones and amines to give pure pyrido [3,2-e] thiazine derivatives, which do not require further purification processes.     

Imparting Multifunctionality by Utilizing Biporosity in a Zirconium‐Based Metal–Organic Framework

In this work, we have synthesized nanocomposites made up of a metal–organic framework (MOF) and conducting polymers by polymerization of specialty monomers such as pyrrole (Py) and 3,4‐ethylenedioxythiophene (EDOT) in the voids of a stable and biporous Zr‐based MOF ( UiO‐66 ). FTIR and Raman data confirmed the presence of polypyrrole ( PPy ) and poly3,4‐ethylenedioxythiophene ( PEDOT ) in UiO‐66‐PPy and UiO‐66‐PEDOT nanocomposites, respectively, and PXRD data revealed successful retention of the structure of the MOF. HRTEM images showed successful incorporation of polymer fibers inside the voids of the framework. Owing to the intrinsic biporosity of UiO‐66 , polymer chains were observed to selectively occupy only one of the voids. This resulted in a remarkable enhancement (million‐fold) of the electrical conductivity while the nanocomposites retain 60–70 % of the porosity of the original MOF. These semiconducting yet significantly porous MOF nanocomposite systems exhibited ultralow thermal conductivity. Enhanced electrical conductivity with lowered thermal conductivity could qualify such MOF nanocomposites for thermoelectric applications.     

Transition-Metal-Free Reverse Reactivity of (2-Alkynyl)-Arylaldimines: Assembly of Functionalized Amino-Indinones

Transition-metal-free regioselective synthesis of functionalized amino-indenones by the reaction of ortho-alkynylaldehydes with a broad range of primary amines by intramolecular cyclization has been described. The designed reaction proceeds through KOH-mediated Prins-type cyclization and DMSO-promoted oxidation of the cyclopent-2-en-1-one system. The proposed mechanism and role of solvent were well supported by control experiments. For the first time, we have disclosed the reverse reactivity of (2-alkynyl)-arylaldimines in a super basic system.     

Intramolecularly coordinated azobenzene selenium derivatives: effect of strength of the Se···N intramolecular interaction on luminescence

A series of selenium derivatives (6-12) of 2-phenylazophenyl have been synthesized using o-lithiation route. The effect of the strength of the intramolecular Se···N interaction on the absorption spectra as well as emission spectra has been studied. The studies suggest that the secondary bonding Se···N interaction give rise to fluorescence, however, the strength of Se···N interaction cannot be directly correlated with the intensity of the fluorescence. TD-DFT calculations show that the main transition involved in the absorption spectra of the compound is the ligand based π-π* type.     

Metabolic profile of glyburide in human liver microsomes using LC‐DAD‐Q‐TRAP‐MS/MS

The sulfonylurea urea drug glyburide (glibenclamide) is widely used for the treatment of diabetes milletus and gestational diabetes. In previous studies monohydroxylated metabolites were identified and characterized for glyburide in different species, but the metabolite owing to the loss of cyclohexyl ring was identified only in mouse. Glyburide upon incubation with hepatic microsomes resulted in 10 metabolites for human. The current study identifies new metabolites of glyburide along with the hydroxylated metabolites that were reported earlier. The newly identified drug metabolites are dihydroxylated metabolites, a metabolite owing to the loss of cyclohexyl ring and one owing to hydroxylation with dehydrogenation. Among the 10 identified metabolites, there were six monohydroxylated metabolites, one dihydroxylated metabolite, two metabolites owing to hydroxylation and dehydrogenation, and one metabolite owing to the loss of cyclohexyl ring. New metabolites of glyburide were identified and characterized using liquid chromatography–diode array detector–quadruple‐ion trap–mass spectrometry/mass spectrometry (LC‐DAD‐Q‐TRAP‐MS/MS). An enhanced mass scan–enhanced product ion scan with information‐dependent acquisition mode in a Q‐TRAP‐MS/MS system was used to characterize the metabolites. Liquid chromatography with diode array detection was used as a complimentary technique to confirm and identify the metabolites. Metabolites formed in higher amounts were detected in both diode array detection and mass spectrometry detection. Copyright © 2012 John Wiley & Sons, Ltd.