Characteristics of immunosorbents used as a new approach to selective solid-phase extraction in environmental analysis

Summary The trace-level determination of organic pollutants in complex matrices is difficult and often not reliable because theccurrent extraction procedures are non-selective. New extraction sorbents involving antigen-antibody interactions, called immunosorbents (ISs), have been synthesised in order to trap a group of structurally related pollutants. The IS capacity is always high for the analyte-antigen used to make the antibodies, but can be low for some related compounds. In this work, we show the relationship that exists between capacity, break-through volume and recovery of analytes because of the competition between the structurally related compounds for antibody sites. Breakthrough due to the overloading of the column should be avoided because calibration curves are no longer linear. The capacity of two ISs, one made for trapping the triazine pesticide group and the second for the phenylurea, group, have been optimised by selecting silica with 50 nm pore size. Calibration curves are linear for all the compounds in a mixture of ten phenylureas up to a concentration of 5 to 10 μg L⁻¹ for each compound when handling 50 mL water samples through a precolumn packed with 0.22 g of IS. Under these conditions, reliable quantitative results are obtained because calibration curves are similar when compounds are alone or in a mixture. Application to the clean-up of soil extracts illustrates the high selectivity and the high potential of these new sorbents in environmental analysis. Presented at the 21^st ISC held in Stuttgart, Germany, 15^th–20^th September, 1996     

Synthesis of 4-Benzidinyl Butyric Acid: A Key Intermediate for Antibodies Production Against Benzidin

a four-step synthesis of monoalkylated benzidin is reported for immunogen preparation against benzidin dye. Use of 10% H₂SO₄/ dioxan for N-Boc cleavage avoids the cyclisation of 4-benzidinyl butyric acid into the corresponding lactam observed with the classical TFA/ CH₂Cl₂ system.     

Junction of ferromagnetic thin films

In this paper, starting from the classical 3D micromagnetic energy, we determine, via an asymptotic analysis, the free energy of two joined ferromagnetic thin films. We distinguish different regimes depending on the limit of the ratio between the small thicknesses of the two films.     

New Analytical Method using Coupled Enzymes for Determination of Polyunsaturated Fatty Acid Content in Olive Oil

A new, simple, and original method is described for specific measurement of polyunsaturated fatty acid content in olive oil. This analytical system uses coupled enzymes, lipase and lipoxygenase. The system consists of lipase-catalyzed hydrolysis of triacylglycerol and subsequent lipoxygenation of liberated polyunsaturated fatty acids. The hydroperoxy-fatty acids formed were easily monitored by spectrophotometry at 234 nm. After being optimized, the method was validated in terms of linearity, precision sensitivity, and recovery. Linear calibration graph was obtained in the range 50–500 µg mL^?1, with a correlation coefficient higher than 0.921 and a detection limit (S/N?=?3) of 15 µg mL^?1. The precision of the method (relative standard deviation) for within and between days is better than 7% and 12%, respectively. The proposed method was successfully applied to the estimation of polyunsaturated fatty acids level in olive oil samples and results obtained were in excellent agreement with those obtained by the classical official method. The proposed method is accurate, simple, cheap, and can be satisfactorily used for routine analysis of edible oils.     

Ferromagnetic thin multi-structures

In this paper, starting from the classical 3D non-convex and nonlocal micromagnetic energy for ferromagnetic materials, we determine, via an asymptotic analysis, the free energy of a multi-structure consisting of a nano-wire in junction with a thin film and of a multi-structure consisting of two joined nano-wires. We assume that the volumes of the two parts composing each multi-structure vanish with the same rate. In the first case, we obtain a 1D limit problem on the nano-wire and a 2D limit problem on the thin film, and the two limit problems are uncoupled. In the second case, we obtain two 1D limit problems coupled by a junction condition on the magnetization. In both cases, the limit problem remains non-convex, but now it becomes completely local.     

A theoretical study of band structure properties for III–V nitrides quantum wells

Reliable and precise knowledge about the strain and composition effects on the band structure properties is crucial for the optimization of InGaN based heterostructures for electronic and optoelectronic device applications. AlInGaN as quaternary barrier material permits to control the band gap and the lattice constant independently. Using the model solid theory and the multi-band k.p interaction model, we investigate the composition effects on band offsets and band structure for pseudomorphic Ga_1−xIn_xN/Al_zIn_yGa_1−y−zN (0 0 1) heterointerfaces having zinc-blende structure. The results show that both conduction and valence band states are strongly modified while varying In and Al contents in the well and barrier materials. Furthermore, it is found that using AlInGaN as the barrier material allows the design of heterostructures including InGaN wells with tensile, zero or compressive strain. Such results give new insights for III-nitride compounds based applications and especially may guide the design of white-light emission diodes.     

Evaluation of silica- and sepharose-based immunoaffinity sorbents for sample cleanup in determination of fumonisins B1 and B2 in corn products

Anti-fumonisin B1 polyclonal antibodies were isolated from the serum of rabbits, immobilized onto the surface of glutaraldehyde-activated silica or Sepharose CL-4B particles, and placed into empty small plastic solid-phase extraction cartridges. The immobilized antibodies were evaluated for their ability to retain fumonisin B1 and fumonisin B2. Cartridge capacity and elution conditions were determined, and the results were compared to those obtained with a commercially available cartridge. The cartridges, which were tested for their effectiveness to isolate the fumonisins from extracts of corn flour and nacho chips, detected fumonisins down to levels of about 20 ng/g. However, additional cleanup was required for detection at lower concentrations. With the use of a strong anion-exchange cartridge as a preliminary cleanup before immunoaffinity chromatography, the detection limit reached 2-5 ng/g in the products tested. The silica sorbent material exhibited strong interactions with the fumonisins, requiring acidified ethanol-water mixtures for elution and resulting in an additional degree of selectivity in isolating fumonisins from sample extracts. The silica-based immunoaffinity cartridges were successfully reused more than 10 times; the Sepharose-based cartridges were less robust. Liquid chromatography with fluorescence detection was used after prechromatographic derivatization with o-phthaldialdehyde-mercaptoethanol.     

Existence of solutions of a non-linear eigenvalue problem with a variable weight

We study the non-linear minimization problem on $H_0^1(\mathrm{\Omega })?L^q$ with $q=\frac{2n}{n?2}$, $\alpha >0$ and $n\ge 4$:

$\underset{\begin{array}{c}\hfill u\in H_0^1(\mathrm{\Omega })\hfill \\ \hfill {6u6}_{L^q}=1\hfill \end{array}}{\inf }?\underset{\mathrm{\Omega }}{\int }a(x,u)|\mathrm{?}u{|}^2?\lambda \underset{\mathrm{\Omega }}{\int }|u{|}^2$

where $a(x,s)$ presents a global minimum α at $(x_0,0)$ with $x_0\in \mathrm{\Omega }$. In order to describe the concentration of $u(x)$ around $x_0$, one needs to calibrate the behavior of $a(x,s)$ with respect to s. The model case is

$\underset{\begin{array}{c}\hfill u\in H_0^1(\mathrm{\Omega })\hfill \\ \hfill {6u6}_{L^q}=1\hfill \end{array}}{\inf }?\underset{\mathrm{\Omega }}{\int }(\alpha +|x{|}^{\beta }|u{|}^k)|\mathrm{?}u{|}^2?\lambda \underset{\mathrm{\Omega }}{\int }|u{|}^2.$

In a previous paper dedicated to the same problem with $\lambda =0$, we showed that minimizers exist only in the range $\beta <kn/q$, which corresponds to a dominant non-linear term. On the contrary, the linear influence for $\beta \ge kn/q$ prevented their existence. The goal of this present paper is to show that for $0<\lambda \le \alpha {\lambda }_1(\mathrm{\Omega })$, $0\le k\le q?2$ and $\beta >kn/q+2$, minimizers do exist.     

Immunochemical-based method for detection of hazelnut proteins in processed foods

A competitive enzyme-linked immunosorbent assay (ELISA) was developed to detect hazelnut by using polyclonal antibodies generated against a protein extract of roasted hazelnut. No cross-reactivity was observed in tests against 39 commodities, including many common allergens, tree nuts, and legumes. Hazelnut protein standard solutions at 0.45 ng/mL [inhibition concentration (IC80) of the competitive test] were clearly identified by the ELISA. An extraction and quantification method was developed and optimized for chocolate, cookies, breakfast cereals, and ice cream, major food commodities likely to be cross-contaminated with undeclared hazelnut during food processing. No sample cleanup was required when extracts were diluted 10-fold. Recovery results were generated with blank matrixes spiked at 4 levels from 1 to 10 microg/g hazelnut protein. With the developed extraction and sample handling procedure, hazelnut proteins were recovered at 64-83% from chocolate and at 78-97% from other matrixes. A confirmatory technique was developed with sodium dodecyl sulfate-polyacrylamide gel electrophoresis and Western transfer. The developed methods were applied to a small market survey of chocolate products and allowed the identification of undeclared hazelnut in these products.