Alkali Phosphonate Metal–Organic Frameworks

A new family of porous metal–organic frameworks (MOFs), namely alkali phosphonate MOFs, is reported. [Na₂Cu(H₄TPPA)] ⋅ (NH₂(CH₃)₂)₂ ( GTUB-1 ) was synthesized using the tetratopic 5,10,15,20-tetrakis[p-phenylphosphonic acid] porphyrin ( H₈-TPPA ) linker with planar X-shaped geometrical core. GTUB-1 is composed of rectangular void channels with BET surface area of 697 m² g⁻¹. GTUB-1 exhibits exceptional thermal stability. The toxicity analysis of the ( H₈-TPPA ) linker indicates that it is well tolerated by an intestinal cell line, suggesting its suitability for creating phosphonate MOFs for biological applications.     

The determination of β-agonist residues in bovine tissues using liquid chromatography–tandem mass spectrometry

We aimed to develop a rapid, simple and reproducible method based on LC–tandem mass spectrometry (LC–MS/MS) to analyze β-agonist residues (clenbuterol, zilpaterol, ractopamine and isoxsuprine) in bovine tissues. The method was validated in accordance with the European Council Decision 2002/657/EC. The samples were homogenized, and then 10 mL of an acetate buffer was added to a 5-g sample. The sample was then centrifuged at 12,000 rpm and filtered. Sodium hydroxide (2 m ) was added to adjust pH of the sample that was centrifuged again. The extract was filtered through a solid-phase extraction column. The residue was re-dissolved in 250 μL acetonitrile and then subjected to LC–MS/MS. The separation was done on a C₁₈ column. The mobile phase consisted of 0.1% formic acid in deionized water and 0.1% formic acid in methanol. The mean recoveries of β-agonists were in the range of 84.3%–119.1% with relative standard deviations (%RSDs) of 0.683%–4.05%. Decision limits and detection capabilities of the analytes ranged from 0.0960 to 4.9349 μg/kg and from 0.0983 to 5.0715, respectively. This method was used to detect four β-agonists in 100 bovine muscle, 100 liver and 100 kidney tissues from a slaughterhouse. No residue was found above the maximum residue limit level.     

Molecular simulation of the adsorption of MTBE in silicalite, mordenite, and zeolite beta

The use of methyl tertiary butyl ether (MTBE) as a gasoline additive has resulted in serious environmental problems following spills and leaks, primarily due to MTBE's high solubility in water. Remediation technologies have involved air stripping, advanced oxidation, and sorption on granular activated carbons (GAC). Hydrophobic zeolites, such as silicalite, dealuminated Y, mordenite, and beta, have been of interest in recent studies for the removal of MTBE from water. Some of these materials have shown a better performance than GAC particularly in the microg/L range. We made Monte Carlo and molecular dynamics simulations of the adsorption of pure MTBE in silicalite, mordenite, and zeolite beta with different Na+ loadings at room temperature to reveal the factors affecting the adsorption process. The results show that although the three zeolites studied here have similar pore volumes, the pore structure of zeolite beta causes a significant difference on the predicted amount of MTBE adsorbed. It was found that the position of the Na+ cations has an important effect at lower pressures. Within the range of [Na+] studied, the amount of Na+ was not found to be critical on the adsorption capacity of any of the zeolites studied, except at very low pressures in silicalite and zeolite beta.     

Simultaneous Determination and Drug Dissolution Testing of Combined Amlodipine Tablet Formulations Using RP-LC

In the proposed work, the simultaneous analysis of amlodipine–rosuvastatin and amlodipine–atorvastatin in their dosage forms was achieved. Simultaneous dissolution profiles of the amlodipine–rosuvastatin and amlodipine–atorvastatin tablets are realized using Apparatus II with a simple, accurate and precise RP-LC method. The mobile phase consisting of 0.2 % H₃PO₄ and pH 5:methanol:acetonitrile (46:27:27) was used. The samples of 10 µL were injected onto a Zorbax SB C18 (100 mm, 4.6 mm, 3.5 µm particle size) column with 1.2 µL min⁻¹ flow rate. The samples were detected at 236 nm. By plotting peak area ratios vs. concentration, the linearity for amlodipine–rosuvastatin and amlodipine–atorvastatin was determined. With the developed RP-LC method, AML, ROS and ATOR were detected within the range of 0.25–10, 0.5–10 and 0.25–25 µg mL⁻¹, respectively. LOD and LOQ values were also calculated as 0.028, 0.058, 0.021 and 0.095 µg mL⁻¹, 0.195 µg mL⁻¹, 0.070 µg mL⁻¹ for AML, ROS and ATOR, respectively. System suitability tests parameters, such as capacity factor, selectivity to previous peak, selectivity to next peak, resolution to previous peak, resolution to next peak, tailing factor, theoretical number of plates, were performed and found coherent with the ICH guideline parameters. The proposed method has been extensively validated in terms of recovery, and recovery results were between 99 and 101 %. For proving the precision, between-day and within-day repeatability results of the method were proposed. The method can be used for the simultaneous determination of amlodipine–rosuvastatin and amlodipine–atorvastatin.

     

Development of a compact self-focusing piezoelectric generator using electrical pre-strain piezocomposite material

New clinical concepts in lithotripsy demand small shock heads. Reducing the size of piezoelectric shock heads will only be possible if the pressure generated at the surface of each transducer can be increased so that, the total pressure at the focus remains very high. So, we propose a new method allowing the generation of large surface pressures. It is well known that the piezoelectric rods in piezocomposite material are more fragile in the extension mode than in the compression mode. For this reason, actuators are mechanically pre-stressed between two flasks. This method cannot be used for transducers working at high frequencies, about 0.5 MHz. For this reason, we proposed to electrically pre-strain the piezoelectric material by applying high electric field in the opposite direction of the polarisation. In a first mode we proposed to pre-strain in continuous mode the transducer. Unfortunately we noticed a rapid de-poling and re-poling in the inverse direction. In a second mode to reduce depolarisation, this field was applied only during a short time just before the generation of the pulse which generate the compressive wave and in a third mode, the transducer was re-poled between two successive electrical pulses. Using this last method, it was possible to increase the maximum pressure at the surface of a 20 mm diameter plane piston to 20% and reach 4 MPa. According to this idea a very compact shock wave generator was designed. The generator made of a 1-3 piezocomposite material has a diameter of 120 mm and focused at 120 mm. The maximum pressure and the width of the compressive wave at the focus were, respectively, 60 MPa and 1.5 micros. The focal zone measured at -3 dB is an ellipsoid 6 mm high in the propagating axis and 3 mm width in the perpendicular direction. The efficacy of this generator was measured as the number of shocks necessary to totally disintegrate plaster balls 15 mm in diameter mimicking the kidney stones. At full power the number of shocks was only 150 which is rather the same number as the one obtained using electrohydraulic machine generally considered as the gold standard. This results show that piezoelectric material may be advantageously used for the manufacturing of shock wave generators.     

Fully Developed Forced Convection Heat Transfer in a Porous Channel with Asymmetric Heat Flux Boundary Conditions

An analytical study is performed on steady, laminar, and fully developed forced convection heat transfer in a parallel plate channel with asymmetric uniform heat flux boundary conditions. The channel is filled with a saturated porous medium, and the lower and upper walls are subjected to different uniform heat fluxes. The dimensionless form of the Darcy–Brinkman momentum equation is solved to determine the dimensionless velocity profile, while the dimensionless energy equation is solved to obtain temperature profile for a hydrodynamically and thermally fully developed flow in the channel. Nusselt numbers for the lower and upper walls and an overall Nusselt number are defined. Analytical expressions for determination of the Nusselt numbers and critical heat flux ratio, at which singularities are observed for individual Nusselt numbers, are obtained. Based on the values of critical heat flux ratio and Darcy number, a diagram is provided to determine the direction of heat transfer between the lower or upper walls while the fluid is flowing in the channel.     

Development of a PVDF low-cost shock-wave hydrophone

During a few past years a series of shock-wave generators for lithotripsy and/or tissue destruction studies have been developed in our laboratory. Based on the experiences in shock wave measurements and the drawbacks in existing hydrophones, we have developed a very low-cost, wideband, reproducible shock-wave hydrophone. The key element of this device is the rapidly mounting, disposable PVDF membrane. This is a commercially available PVDF shock gauge which is poled by a patented cyclic poling technique. To obtain the widest possible bandwidth, we have adopted a special coplanar membrane design. The PVDF film is sandwiched between the surfaces of a P.V.C. and a metallic plate of brass which the latter is in contact with the surrounding medium. On the other hand, the active lead is isolated from medium and it is in contact with an isolating liquid (degassed petroleum) held in a cylindrical chamber over the membrane. By the incorporation of this design, the hydrophone can be used for shock wave measurements even in conductive media like different physiological liquids, with a negligible change of sensitivity.     

Surface Propensity of Anions in a Binary Ionic-Liquid Mixture Assessed by Full-Range Angle-Resolved X-ray Photoelectron Spectroscopy and Surface-Tension Measurements

Angle-resolved X-ray photoelectron spectroscopy and contact-angle measurements guided by a signal attenuation model are utilized to extract molar composition and anion enrichment in the vacuum interface of a binary ionic liquid mixture, having a common quaternary ammonium cation and two different anions. By using the intensity ratio of the F1s peaks belonging to the two different anions recorded at the full electron take-off angle range, from 0° to 80°, we have determined that only a fractionally covered and anion enriched surface layer can predict the AR-XPS data, which is also consistent with surface tension measurements. Moreover, the more bulky and non-spherical anion enrichment is evident even at the conventional and the so assumed bulk sensitive take-off angle of 0°. This methodology provides a surface enrichment factor of the molecular ions and clearly serves as an experimental evidence for recently debated surface layering and/or island structure in ionic liquid systems.