Electrospray Ionization Mass Spectrometry (ESI-MS) as a Useful Tool for Fast Evaluation of Anion and Cation Complexation Abilities of a Cyclam Derivative

Electrospray ionization mass espectrometry (ESI-MS) has been used for the study of a cyclam derivative noncovalent interactions. At acidic pH, diprotonated macrocycle bound to different anionic species were observed. The selectivity shown by competitive experiments is rationalized with the help of semiempirical theoretical calculations. At basic pH, the base peak corresponded to the macrocycle-alkaline metal complexes, and again competition experiments showed different binding strength. Finally, experiments carried out in the presence of transition metal salts allowed the detection of the complexes present in the mixture and revealed their different kinetic behavior.     

Study of Nanocrystalline BiMnO3‐‐PbTiO3: Synthesis,Structural Elucidation,and Magnetic Characterization of the Whole Solid Solution

In the last ten years, the study and the search for new multiferroic materials have been a major challenge due to their potential applications in electronic technology. In this way, bismuth‐containing perovskites (BiMO₃), and particularly those in which the metal M position is occupied by a magnetically active cation, have been extensively investigated as possible multiferroic materials. From the point of view of synthesis, only a few of the possible bismuth‐containing perovskites can be prepared by conventional methods but at high pressures. Herein, the preparation of one of these potential multiferroic systems, the solid solution xBiMnO₃‐(1?x)PbTiO₃ by mechanosynthesis is reported. Note that this synthetic method allows the oxides with high x values, and more particularly the BiMnO₃ phase, to be obtained as nanocrystalline phases, in a single step and at room temperature without the application of external pressure. These results confirm that, in the case of Bi perovskites, mechanosynthesis is a good alternative to high‐pressure synthesis. These materials have been studied from the point of view of their structural characteristics by precession electron diffraction and magnetic property measurements.     

Development of an automatic solid phase extraction and liquid chromatography mass spectrometry method by using a monolithic column for the analysis of Cyclosporin A in human plasma

A sensitive and specific and automated liquid chromatography-electrospray mass spectrometric (LC-ESI-MS) assay for the quantification of Cyclosporin A in human plasma was developed. Following a simple protein precipitation step, the supernatant was extracted on-line and directly injected into the system LC-ESI-MS. A relatively new type of monolithic column consisting of a silica rod with bimodal pore structure was used to achieve a retention time of 2.4 min with a very low backpressure at a flow rate of 1 ml/min. The assay was linear from 0.050 to 1.000 μg/ml. The mean recovery was 91%. The mean inter-day and intra-day precisions were 1.85% and 2.83%, respectively. The combination of the automated solid phase extraction and the low retention time achieved with this columns increase the throughput and decrease the time of analysis of each sample. This technology is useful in order to improve the efficiency of the bioanalytical studies.     

Simultaneous metabolic mapping of different anatomies by 1H HR-MAS chemical shift imaging

Analytical and Bioanalytical Chemistry - Localized information on a specimen is considered indispensable for deciphering biological activity. Magnetic resonance spectroscopy is a notable method...     

Study of nanocrystalline BiMnO3-PbTiO3: synthesis, structural elucidation, and magnetic characterization of the whole solid solution

In the last ten years, the study and the search for new multiferroic materials have been a major challenge due to their potential applications in electronic technology. In this way, bismuth-containing perovskites (BiMO(3)), and particularly those in which the metal?M position is occupied by a magnetically active cation, have been extensively investigated as possible multiferroic materials. From the point of view of synthesis, only a few of the possible bismuth-containing perovskites can be prepared by conventional methods but at high pressures. Herein, the preparation of one of these potential multiferroic systems, the solid solution xBiMnO(3)-(1-x)PbTiO(3) by mechanosynthesis is reported. Note that this synthetic method allows the oxides with high x values, and more particularly the BiMnO(3) phase, to be obtained as nanocrystalline phases, in a single step and at room temperature without the application of external pressure. These results confirm that, in the case of Bi perovskites, mechanosynthesis is a good alternative to high-pressure synthesis. These materials have been studied from the point of view of their structural characteristics by precession electron diffraction and magnetic property measurements.     

In vivo trapping of polyketide intermediates from an assembly line synthase using malonyl carba(dethia)-N-acetyl cysteamines

Early-stage intermediates in the biosynthesis of erythromycin A by Saccharopolyspora erythraea were intercepted by malonyl carba(dethia)-N-acetyl cysteamines, generated in vivo from the hydrolysis of the corresponding methyl esters.     

Enzymatic resolution of (±)-cis-2-aminocyclopentanol and (±)-cis-2-aminocyclohexanol

(±)-cis-N-Benzyloxycarbonyl-2-aminocyclopentanol was efficiently resolved by O-acylation with Pseudomonas cepacia lipase, as was (±)-cis-N-benzyloxycarbonyl-2-aminocyclohexanol when Candida antarctica lipase was used.