Organometallic complexes in ascidian embryonic development: II. Effects on different stages and larvae

The effects of the organometallic compounds Bu₂Sn-D -(?;)sorbitol, Bu₂Sn-D -(+)glucose, Bu₂Sn-D -(?)fructose and Bu₂Sn-D -(+)glyceraldehyde were tested in vivo on different stages of Ascidian development, larval movement and metamorphosis. Organotin(IV) complexes are organometallic compounds widely used as industrial biocides, antifouling agents and agricultural fungicides and are toxic to a range of organisms. Two-cell stage embryos, if incubated for one hour in the organotin (IV) solutions, stopped the cleavage, which was restored when they were transferred into normal sea water. The gastrula stage was seriously affected in 10^?4mol dm^?3 solutions of the above-mentioned complexes: 85% of the embryos were anomalous neurulae with open neural folds, 5% were twisted larvae. The gastrulae, when incubated for 1 h in 10^?5mol dm^?3 solutions, developed twisted larvae in ovular envelopes and immobile larvae with twisted tails. Larvae treated with 10^?4mol dm^?3 and 10^?5 mol dm^?3 Bu₂Sn-D -(?)sorbitol, Bu₂Sn-D -(+)glucose and Bu₂Sn-D -(+)glyceraldehyde solutions stopped swimming, did not metamorphose and afterwards underwent cytolysis. An initial hyperactivity of circular movements, followed by immobility, was observed in the larvae incubated in Bu₂Sn-D -(?;)fructose.     

Efficient BiVO4 Photoanodes by Postsynthetic Treatment: Remarkable Improvements in Photoelectrochemical Performance from Facile Borate Modification

Water‐splitting photoanodes based on semiconductor materials typically require a dopant in the structure and co‐catalysts on the surface to overcome the problems of charge recombination and high catalytic barrier. Unlike these conventional strategies, a simple treatment is reported that involves soaking a sample of pristine BiVO₄ in a borate buffer solution. This modifies the catalytic local environment of BiVO₄ by the introduction of a borate moiety at the molecular level. The self‐anchored borate plays the role of a passivator in reducing the surface charge recombination as well as that of a ligand in modifying the catalytic site to facilitate faster water oxidation. The modified BiVO₄ photoanode, without typical doping or catalyst modification, achieved a photocurrent density of 3.5 mA cm^?2 at 1.23 V and a cathodically shifted onset potential of 250 mV. This work provides an extremely simple method to improve the intrinsic photoelectrochemical performance of BiVO₄ photoanodes.     

An enhanced beam-theory model of the mixed-mode bending (MMB) test—Part II: Applications and results

The paper presents an enhanced beam-theory (EBT) model of the mixed-mode bending (MMB) test, whereby the specimen is considered as an assemblage of two sublaminates partly connected by an elastic–brittle interface. Analytical expressions for the compliance, energy release rate, and mode mixity are deduced. A compliance calibration strategy enabling numerical or experimental evaluation of the interface elastic constants is also presented. Furthermore, analytical expressions for the crack length correction parameters—analogous to those given by the corrected beam-theory (CBT) model for unidirectional laminated specimens—are furnished for multidirectional laminated specimens, as well. Lastly, an example application to experimental data reduction is presented.     

Cohesive failure analysis of an array of IC chips bonded to a stretched substrate

The paper presents a mechanical model for predicting the cohesive failure of a periodic array of integrated circuit (IC) chips adhesively bonded to a stretched substrate. A unit cell of the layered structure consisting of the IC chips, adhesive layer, and substrate is modeled as an assembly of two elastic Timoshenko beams, representing the chip and substrate, connected by an elastic interface, representing the adhesive. Accordingly, the stresses and energy release rate (ERR) in the adhesive layer – responsible for the premature cracking of the adhesive and debonding of the IC chips – are identified with the corresponding quantities computed for the elastic interface. Expressions for the adhesive stresses and ERR are given in terms of geometrical dimensions and material properties, combined with integration constants obtained numerically via the multi-segment analysis method. For comparison, the stresses in the adhesive are also computed based on a finite element model, and the ERR is evaluated using the virtual crack-closure technique (VCCT). The analytical predictions and numerical results match fairly well, considering the effects of key factors, such as the distance between adjacent chips, the chip size, the material properties of adhesive and substrate. The interaction between the chips is shown to have relevant effects on the adhesive stresses. In particular, only the mode II contributes to the ERR which increases with the ratio of the chip size to the distance between the chips and with the compliance of the adhesive and substrate layers.     

Development and Validation of a Fast Reversed-Phase Ion-Pairing Liquid Chromatographic Method for Simultaneous Determination of Eight Cephalosporin Antibiotics in Pharmaceutical Formulations

A fast and reliable single method was developed for rapid screening of cephalosporin oral dosage forms aimed to the detection of counterfeit and substandard drugs that might be illegally commercialised. Nine cephalosporin compounds, ceftibuten, cefatrizine, cefadroxil, cefaclor, cefprozil (Z) and (E)-isomers, cefixime, cephalexin and cefradine were separated in a six minutes chromatographic run by using a Symmetry^® C18 column (50 × 4.6 mm I.D., 3.5 μm particle size) and an UV detector set at 254 nm. The mobile phase consisted of a mixture of acetonitrile-methanol-phosphate buffer (50 mM) containing 1-pentanesulfonic acid sodium salt (7 mM) adjusted to pH=2.1 with phosphoric acid (9:13:78 v/v/v). Validation of the method showed it to be robust, precise, accurate and linear over the concentration range of analysis.     

Identification and determination of corticosteroids in adrenal gland extracts for pharmaceutical use by HPLC

Summary Some HPLC procedures with isocratic or gradient elution are reported for the identification and determination of most of the characteristic components of cortical extracts. The proposed solvent systems were: A) for normal phase chromatography, mixtures of chloroform-methanol-water on silica columns. B) For reversed phase chromatography, mixtures of methanol-water or acetonitrile-water or tetrahydrofuran-water on octadecyl silica columns of different brands. With these systems it was possible to identify and determine, in addition to the principal corticosteroids, some minor components of the cortical extracts as the 20β-dihydroderivatives of compounds F, E, A, B, the 17-ketosteroids adrenosterone, 11β-hydroxyandrostendione and androstendione and finally, progesterone and 17-OH progesterone. In reversed phase chromatography it was also possible, by monitoring the effluent at 205 nm, to reveal the 5α- and 5β-tetrahydroderivatives of the main corticosteroids and to separate them from most of the steroidal components of the adrenal extracts; in these conditions it was also possible to reveal some characteristic, unknown components of the cortical extracts. Some results of quantitative analysis of cortical extracts are also reported, comparing different analytical procedures. Presented at the 15th International Symposium on Chromatography, Nürnberg, October 1984     

Focused Microwave-Assisted Extraction and LC Determination of Ketoprofen in the Presence of Preservatives in a Pharmaceutical Cream Formulation

A simple and rapid open-vessel focused microwave-assisted extraction (FMAE) method followed by LC analysis was developed for the determination of ketoprofen lysine salt in the presence of methyl p-hydroxybenzoate and propyl p-hydroxybenzoate preservatives in topical cream. Extraction were performed in acetone/potassium dihydrogenphosphate (25 mM, pH 3.0) (70:30 v/v) by reaching a target temperature of 65 °C in a 10 min linear ramp. The chromatographic separation was performed on a Discovery RP-Amide C16 column (250 × 4.6 mm I.D., 5 μm particle size). The optimal mobile phase consisted of acetonitrile/potassium dihydrogen phosphate 25 mM adjusted to pH 3.0 with phosphoric acid (50:50 v/v). The complete analytical procedure was validated with regard to limit of quantification, linearity, precision and accuracy. The method was linear over the concentration range of 0.08–0.12 mg mL⁻¹; the relative standard deviations of intra- and inter-day assays were 1.9–2.3 and 1.8% respectively. The limit of quantification was 0.54 μg mL⁻¹. The proposed method shows many advantages as short extraction time, little solvent consumption without requiring further sample clean-up steps before liquid chromatographic analysis and is proposed for vast scale screening of cream dosage forms aimed to the detection of counterfeit and substandard drugs.

     

An enhanced beam-theory model of the mixed-mode bending (MMB) test—Part I: Literature review and mechanical model

The paper presents a mechanical model of the mixed-mode bending (MMB) test used to assess the mixed-mode interlaminar fracture toughness of composite laminates. The laminated specimen is considered as an assemblage of two sublaminates partly connected by an elastic–brittle interface. The problem is formulated through a set of 36 differential equations, accompanied by suitable boundary conditions. Solution of the problem is achieved by separately considering the two subproblems related to the symmetric and antisymmetric parts of the loads, which for symmetric specimens correspond to fracture modes I and II, respectively. Explicit expressions are determined for the interfacial stresses, internal forces, and displacements.