Sedimentation field flow fractionation of immunoglobulin A coated polystyrene beads. Influence of carrier composition on complex characterization

The amount of immunoglobulin A (IgA) adsorbed on the surface of two different samples of polystyrene (PS) microbeads was evaluated using differential sedimentation field flow fractionation (SdFFF) analyses. For the first time, the SdFFF separations obtained by using, as mobile phase, solutions common to many biochemical procedures and applications have been compared and discussed. Good separation results were achieved in the different carriers, and the SdFFF gave equivalent mass per particle values in all carriers provided that the pH and ionic strength conditions of the eluents were well controlled. The IgA adsorption process onto PS occurred by maintaining unaltered the capacity of the PS-IgA substrate to selectively recognize anti-IgA (aIgA), as proven by elution of the ternary complex PS-IgA-aIgA and from the monitored lack of reaction when the PS-IgA was placed in contact with aIgE.     

Molecules Present in Plant Essential Oils for Prevention and Treatment of Colorectal Cancer (CRC)

Essential oils (EOs) are a complex mixture of hydrophobic and volatile compounds synthesized from aromatic plants, commonly present in the human diet. In recent years, many in vitro studies have suggested possible anticancer properties of single EO compounds, on colorectal cancer (CRC) cells. However, the majority of these studies did not compare the effects of these compounds on normal and cancer colon cells. By using NCM-460, a normal human mucosal epithelial cell line, Caco-2, a human colon epithelial adenocarcinoma cell line, and SW-620, colon cancer cells derived from lymph node metastatic site, we identified cinnamaldehyde, derived from cinnamon EO and eugenol, derived from bud clove EO, as compounds with a specific anticancer action selectively targeting the transformed colonic cells. Both cinnamaldehyde (75 µM) and eugenol (800 µM), after 72 h of treatment, were capable to induce apoptosis, necrosis and a cell cycle slowdown in Caco-2 and in SW-620, but not in NCM-460 cells. If associated with a targeted delivery to the colon, these two compounds could prove effective in the prevention or treatment of CRC.     

Synthesis of benzo-fused five- and six-membered heterocycles by palladium-catalyzed cyclocarbonylation

A novel and simple synthetic methodology, based on palladium-catalyzed cyclocarbonylation reaction, is presented for preparing five- and six-membered benzo-fused heterocycles. A mechanism for the process is also proposed and discussed.     

Sedimentation field flow fractionation and flow field flow fractionation as tools for studying the aging effects of WO₃ colloids for photoelectrochemical uses

WO₃ colloidal suspensions obtained through a simple sol–gel procedure were subjected to a controlled temperature aging process whose time evolution in terms of particle mass and size distribution was followed by sedimentation field flow fractionation (SdFFF) and flow field flow fractionation (FlFFF). The experiments performed at a temperature of 60 °C showed that in a few hours the initially transparent sol of WO₃ particles, whose size was less than 25 nm, undergoes a progressive size increase allowing nanoparticles to reach a maximum equivalent spherical size of about 130 nm after 5 h. The observed shift in particle size distribution maxima (SdFFF), the broadening of the curves (FlFFF) and the SEM–TEM observations suggest a mixed mechanism of growth-aggregation of initial nanocrystals to form larger particles. The photoelectrochemical properties of thin WO₃ films obtained from the aged suspensions at regular intervals, were tested in a biased photoelectrocatalytic cell with 1 M H₂SO₄ under solar simulated irradiation. The current–voltage polarization curves recorded in the potential range 0–1.8 V (vs. SCE) showed a diminution of the maximum photocurrent from 3.7 mA cm⁻² to 2.8 mA cm⁻² with aging times of 1 h and 5 h, respectively. This loss of performance was mainly attributed to the reduction of the electroactive surface area of the sintered particles as suggested by the satisfactory linear correlation between the integrated photocurrent and the cyclic voltammetry cathodic wave area of the W(VI) → W(V) process measured in the dark.     

Electrospray ionisation tandem mass spectrometric investigation of phenylpropanoids and secoiridoids from solid olive residue

This work is focused on the recovery and structural characterisation of bioactive compounds from SOR (solid olive residue), a low cost and widely available by-product in the Mediterranean basin. In the light of the interesting biological activities attributed both to secoiridoid and phenylpropanoids, the aim of this work was to carry out a systematic tandem mass spectrometric study for the identification and characterisation of these two class of compounds extracted from SOR derived from Coratina, a cultivar widely diffused in the south of Italy. Five phenylpropanoids, in addition to verbascoside, and two new secoiridoids were identified.     

Stereoselective synthesis and functionalization of N-alkyl-β-lactams

Novel polyfunctionalized N-alkyl-β-lactams were prepared with high stereoselectivity in an efficient manner by a palladium-catalyzed [2+2] carbonylative cycloaddition of allyl bromide with heteroarylidene N-alkyl-amines The type of alkyl group linked to the nitrogen atom influences the reaction stereoselectivity. Moreover, the C-3 and the C-4 positions of the azetidinone ring can be further stereoselectively functionalized inserting various groups through the generation of a stable azetidinyl carbanion and then captured by various electrophiles.     

Study of the phenolic composition of spanish and italian monocultivar extra virgin olive oils: Distribution of lignans, secoiridoidic, simple phenols and flavonoids

The aim of the present study was to compare the phenolic content in selected monocultivar extra virgin olive oils. Analyses were carried out by HPLC/DAD/MS on Picual, Picuda, Arbequina and Hojiblanca oils from Spain and Seggianese and Taggiasca oils from Italy. Oils from cultivar Picual showed similar characteristics to those of Seggianese oils, with total amounts of secoiridoids of 498.7 and 619.2 mg/L, respectively. The phenolic composition of Arbequina oils is close to that of the Taggiasca variety with lignans among the main compounds. The determination of free and linked OH-Tyr, by way of an acid hydrolysis, represents a rapid and suitable method, especially when standards are not available, to determine antioxidant potentialities in terms of MPC, particularly for fresh extra virgin olive oils rich in secoiridoidic derivatives.     

Stereoselective synthesis of heterosubstituted aziridines and their functionalization

Lithiated (α-chloroalkyl)heterocycles, generated by deprotonation with LDA at −78 °C in THF, add to various enantiopure imines affording ‘one pot’ chiral heterosubstituted aziridines in a diastereoselective manner. Lithiated heterosubstituted aziridines, obtained by deprotonation of the corresponding aziridines with n-BuLi at −78 °C in THF, were trapped by electrophiles (D₂O or CH₃I) with high stereoselectivity.     

Investigation of expected location of muonium in normal state in III–V semiconductors and associated muon hyperfine interaction

The location and hyperfine properties of muonium in AlP is investigated by the unrestricted Hartree-Fock cluster procedure. Two minima are found, one at the aluminium tetrahedral interstitial site, and the other at the corresponding phosphorus site. The former is deeper by 0.25 eV and separated from the other minimum by a steep maximum of 0.63 eV in the hexagonal region. Using the calculated electronic wave functions, the muon hyperfine constant, after vibrational averaging, comes out smaller than the value for free muonium, the ratio being 0.93. This value is, however, significantly higher than the experimental results in GaP and GaAs.Briefly reported in Abstract at American Physical Society meeting in New Orleans, March 1988, see Bull. Am. Phys. Soc. 33 (1988) 1364.     

Complementary use of flow and sedimentation field-flow fractionation techniques for size characterizing biodegradable poly(lactic acid) nanospheres

Poly(lactic acid) (PLA) nanoparticles were synthesized using a modified evaporation method, testing two different surfactants (sodium cholate and Pluronic F68) for the process. During their formulation the prodrug 5'-octanoyl-CPA (Oct-CPA) of the anti-ischemic N(6)-cyclopentyladenosine (CPA) was encapsulated. Three different purification methods were compared with respect to the influence of surfactant on the size characteristics of the final nanoparticle product. Flow and sedimentation field-flow fractionation techniques (FlFFF and SdFFF, respectively) were used to size characterize the five poly(lactic acid) particle samples. Two different combinations of carrier solution (mobile phase) were employed in the FlFFF analyses, while a solution of poly(vinyl alcohol) was used as mobile phase for the SdFFF runs. The separation performances of the two techniques were compared and the particle size distributions (PSDs), derived from the fractograms, were interpreted with the support of observations by scanning electron microscopy. Some critical aspects, such as the carrier choice and the channel thickness determination for the FlFFF, have been investigated. This is the first comprehensive comparison of the two FFF techniques for characterizing non-standard particulate materials. The two FFF techniques proved to be complementary and gave good, congruent and very useful information on the size distributions of the five poly(lactic acid) particle samples.