Peptide structural analysis using continuous Ar cluster and C60 ion beams

A novel application of time-of-flight secondary ion mass spectrometry (ToF-SIMS) with continuous Ar cluster beams to peptide analysis was investigated. In order to evaluate peptide structures, it is necessary to detect fragment ions related to multiple neighbouring amino acid residues. It is, however, difficult to detect these using conventional ToF-SIMS primary ion beams such as Bi cluster beams. Recently, C₆₀ and Ar cluster ion beams have been introduced to ToF-SIMS as primary ion beams and are expected to generate larger secondary ions than conventional ones. In this study, two sets of model peptides have been studied: (des-Tyr)-Leu-enkephalin and (des-Tyr)-Met-enkephalin (molecular weights are approximately 400 Da), and [Asn¹ Val⁵]-angiotensin II and [Val⁵]-angiotensin I (molecular weights are approximately 1,000 Da) in order to evaluate the usefulness of the large cluster ion beams for peptide structural analysis. As a result, by using the Ar cluster beams, peptide molecular ions and large fragment ions, which are not easily detected using conventional ToF-SIMS primary ion beams such as Bi₃ ⁺, are clearly detected. Since the large fragment ions indicating amino acid sequences of the peptides are detected by the large cluster beams, it is suggested that the Ar cluster and C₆₀ ion beams are useful for peptide structural analysis.     

Water Structure Modification by Sugars and Its Consequence on Micellization Behavior of Cetyltrimethylammonium Bromide in Aqueous Solution

Water structure modification by sugars with a wide difference in stereoregular structures ranging from monosaccharide to trisaccharide and its consequence on the micellization behavior of cetyltrimethylammonium bromide (CTAB) in aqueous medium have been investigated. The characteristic variation in water absorption peaks in the presence of d(?)fructose has been studied by near-infrared spectroscopy. The analyses show that the hydrogen bonding capability of d(+)glucose, d(?)fructose, sucrose, trehalose and raffinose is mainly responsible for the variation in water-additive interactions. The critical micelle concentration determined by specific conductivity measurement and aggregation number determined by steady state fluorescence quenching method show significant variations in presence of additives for CTAB in aqueous solution. The sugars interact with the water structure to varying extents owing to differences in hydrogen bonding capability depending on the stereoregularity of the structure. This induces differences in the microenvironment for competition between the hydrophobic interaction and degree of hydration of the hydrophilic group of the surfactant to ultimately influence the micellization behavior in aqueous solution.     

Analysis of drug interactions with serum proteins and related binding agents by affinity capillary electrophoresis: A review

Biomolecules such as serum proteins can interact with drugs in the body and influence their pharmaceutical effects. Specific and precise methods that analyze these interactions are critical for drug development or monitoring and for diagnostic purposes. Affinity capillary electrophoresis (ACE) is one technique that can be used to examine the binding between drugs and serum proteins, or other agents found in serum or blood. This article will review the basic principles of ACE, along with related affinity-based capillary electrophoresis (CE) methods, and examine recent developments that have occurred in this field as related to the characterization of drug–protein interactions. An overview will be given of the various formats that can be used in ACE and CE for such work, including the relative advantages or weaknesses of each approach. Various applications of ACE and affinity-based CE methods for the analysis of drug interactions with serum proteins and other binding agents will also be presented. Applications of ACE and related techniques that will be discussed include drug interaction studies with serum agents, chiral drug separations employing serum proteins, and the use of CE in hybrid methods to characterize drug binding with serum proteins.     

Synthesis and biological studies of complexes of 2- amino-<Emphasis Type="Italic">N</Emphasis>(2-aminobenzoyl) benzohydrazide with Co(II), Ni(II), and Cu(II)

The present work is concerned with the synthesis and coordination compounds of 2-amino-N(2-aminobezoyl) benzohydrazide (ABH). The ligand was synthesized by the reaction of methylanthranilate and hydrazine in 2:1 molar ratio. It can be viewed as a modified form of hydrazide. The ligand was characterized by ¹H-NMR, ¹³C-NMR, mass spectrometry, elemental analysis, and infrared studies. The ligand has got -NH₂ moeity, the site for chelation. The complexes of Co(II), Ni(II), and Cu(II) chlorides and bromides were prepared. These complexes were characterized by elemental analysis, infrared, conductance, and magnetic susceptibility studies. Infrared spectra studies confirmed the formation of complexes, while elemental studies suggested the complexation of [M(ABH)X₂] (where X = Cl⁻ or Br⁻) composition.     

Armatans A and B,New Antimicrobial Isoflavans from Colutea armata

Chemistry of Natural Compounds - Armatans A (1) and B (2), new isoflavans, have been isolated from the EtOAc-soluble fraction of the MeOH extract of Colutea armata Hemsl. &amp; Lace, along with...     

SPE-GC-MS for the Determination of Halogenated Acetic Acids in Drinking Water

The development and optimization of analytical methods for the better monitoring of disinfection by-products especially haloacetic acids in water are key step in order to estimate human exposure to such products after chlorination. A reliable and accurate analytical method is needed in order to reach the levels of concentration required by United States Environmental Protection Agency regulations. In this study a method was developed for determining halogenated acetic acids in drinking water, involving solid phase extraction, methylation derivatization, and GC-MS. The new SPE-GC-MS-SIM method is capable of analyzing all nine acids at extremely low μg L^–1 level. Run time is significantly reduced without compromising analytical results. The major advantages of the method are the simplicity of the chromatography, short run time and low detection limits. The method performance, limits of detection and spiking recovery were evaluated and the results proved that the accuracy and precision were good. This method outperforms previous GC-MS methods especially for the determination of dibromoacetic, dibromochloroacetic, dichlorobromoacetic and tribromoacetic acids. The method has been used to analyse domestic tap water and water samples collected at a local water treatment plant.

     

An In Vitro Study of the Interaction of Copper(II) Salicylates with Genomic DNA Using Gel Electrophoresis and Gel Permeation Chromatography

This papers describes the in vitro interaction of copper(II) acetylsalicylate and copper(II) salicylate with genomic DNA isolated from human blood. The two drug substances were found to bind to DNA after incubation with whole blood over night. Bonding was confirmed by detection of separated DNA electrophoresis bands for copper, copper(II) acetylsalicylate, copper(II) salicylate, acetylsalicylic acid and salicylic acid. Drug–DNA interactions were observed during electrophoresis in the form of fragmentation by formation of two bands when compared to controls. Gel permeation chromatography parameters also confirmed the occurrence of fragmentation. The use of gel permeation chromatography parameters as a measure of fragmentation of DNA is discussed. The fragmentation of genomic DNA after incubation with copper(II) acetylsalicylate and copper(II) salicylate suggested that these drug substances might be responsible for cytotoxicity in vivo.

     

Facile,eco-friendly,one-pot protocol for the synthesis of indole-imidazole derivatives catalyzed by amino acids

An efficient, convenient green approach for the synthesis of indole-based 2,4,5-trisubstituted and 1,2,4,5-tetrasubstituted imidazoles by multicomponent reaction of substituted 2-arylindole-3-carbaldehydes, benzil, substituted anilines, and ammonium acetate using catalytic amino acid (glycine) in ethanol is described. Several amino acids have also been evaluated as organic catalysts for these reactions. The structures of the compounds have been established on the basis of infrared, mass, and ¹H NMR spectral data. The mild reaction conditions, inexpensive/economical reagents, and good yield show the usefulness of this approach.