Use of self assembled magnetic beads for on-chip protein digestion

The use of grafted trypsin magnetic beads in a microchip for performing protein digestion is described. The PDMS device uses strong magnets to create a magnetic field parallel to the flow with a strong gradient pointing through the center of the chip channel. This allows for the formation of a low-hydrodynamic resistance plug of magnetic trypsin beads that serves as a matrix for protein digestion. This device represents an inexpensive way of fabricating a multi open-tubular-like column with an appropriate pore size for proteins. Kinetics studies of the hydrolysis of a model peptide show a 100-fold increase in digestion speed obtained by the microsystem when compared to a batch wise system. This system also offers the great advantage of easy replacement, as the bead matrix is easily washed out and replaced. High performance and reproducibility for digesting recombinant human growth hormone are confirmed by analysing the digest products in both CE and MALDI-TOF MS. Similar sequence coverage (of about 44%) is obtained from MS analysis of products after 10 minutes on-chip and 4 h with soluble trypsin in bulk.     

Comb-like copolymers as self-coating,low-viscosity and high-resolution matrices for DNA sequencing

Comb-like copolymers with a polyacrylamide backbone and poly(N,N-dimethylacrylamide) grafts were prepared, as a way to combine the superior sieving properties of polyacrylamide with the self-coating properties of polydimethylacrylamide. These matrices function well in the absence of a capillary coating, and achieve separation performances for single-stranded DNA that are comparable to those of state-of-the-art long-chain linear polyacrylamide. Structural parameters such as the grafting density and the polymer molecular mass were varied, and good performance appears to be achieved with a relatively large range of parameters. Surprisingly, excellent separation is achieved even with matrices that have a viscosity as low as 200 mPa/s. A discussion of the physics underlying this behavior is provided.     

Sels d'aziridinium stables C-fonctionnalisés III: Synthèse et caractérisation d'aziridines protonées épimères à l'azote

Aziridinium ions were prepared from aziridines bearing a functionality on a ring carbon and as isolated crystalline fluorosulfate salts either by protonation in fluorosulfuric acid solution or by alkylation with methyl fluorosulfate. The structural assignement of these ions is based on nmr spectra and on quenching experiments with sodium carbonate. The configurations of the epimeric ions have been assigned by the nuclear Qverhauser effect and the stereoselectivity in protonation is disucussed.     

Some advantages of high temperature for the separation of pharmaceutical compounds with mass spectrometry detection

The beneficial effects of high temperature on separation and detection of basic compounds, the detection being performed by MS via ESI, are investigated. The influence of various parameters on both separation and detection performances is studied. These parameters include the mobile phase pH, the temperature, and the type of stationary phase. Experiments are performed under gradient elution conditions. The results obtained with four different supports, silica-, zirconia-, carbon-, and polymer-based columns, are compared by means of different criteria including the elution composition, the peak asymmetry, and the S/N. High temperature liquid chromatography at high pH with volatile buffers suitable for MS detection was shown to be an interesting choice for solutes with basic sites.     

Apparent equilibration time required for surfactant-oil-water systems to emulsify into the morphology imposed by the formulation. Part 2: Effect of sec-butanol concentration and initial location

Winsor type I equilibrated surfactant-oil-water (SOW) systems produce o/w emulsions upon stirring. However, if the surfactant is initially dissolved in the oil phase, the attained type after inmediate emulsification is usually w/o. If the SOW system is partially equilibrated, it could result in a normal o/w emulsion, as if it were fully equilibrated. The minimum contact time for that to happen, the so-called apparent equilibration time tAPE, was previously shown (Langmuir 2002, 18, 607) to strongly depend on formulation, surfactant molecular weight, and oil viscosity. The present report shows that it depends on alcohol concentration and location in the unequilibrated system.     

Covering a Ball with Smaller Equal Balls in ℝn

We give an explicit upper bound of the minimal number _T,n of balls of radius 1/2 which form a covering of a ball of radius T > 1/2 in ⁿ, n \geq 2. The asymptotic estimates of _T,n we deduce when n is large are improved further by recent results of Böröczky, Jr. and Wintsche on the asymptotic estimates of the minimal numberof equal balls of ⁿ covering the sphere S^n-1. The optimality of the asymptotic estimates is discussed.