A simple zero length surface-modification approach for preparing novel bifunctional supports for co-immobilisation studies

A straightforward method of creating a bifunctional support possessing pre-defined ratios of amine and chloromethyl groups based upon a controlled conversion of standard Merrifield resin is presented. It avoids the extensive optimisation of reactant concentrations and reaction conditions required by existing methods. Furthermore, it avoids increases in the spacer/linker length that lead to detrimental reductions in the rigidity of the grafted layer. The method will allow for efficient, predictable and reproducible co-immobilisation of molecular species.     

Hydrogen/deuterium exchange on aromatic rings during atmospheric pressure chemical ionization mass spectrometry

It has been demonstrated that substituted indoles fully labelled with deuterium on the aromatic ring can undergo substantial exchange back to partial and even fully protonated forms during atmospheric pressure chemical ionisation (APCI) liquid chromatography/mass spectrometry (LC/MS). The degree of this exchange was strongly dependent on the absolute quantity of analyte, the APCI desolvation temperature, the nature of the mobile phase, the mobile phase flow rate and the instrument used. Hydrogen/deuterium (H/D) exchange on several other aromatic ring systems during APCI LC/MS was either undetectable (nitrobenzene, aniline) or extremely small (acetanilide) compared to the effect observed for substituted indoles. This observation has major implications for quantitative assays using deuterium‐labelled internal standards and for the detection of deuterium‐labelled products from isotopically labelled feeding experiments where there is a risk of back exchange to the protonated form during the analysis. Copyright © 2010 John Wiley & Sons, Ltd.     

Doubly diastereoselective conjugate addition of enantiopure lithium amides to enantiopure N-enoyl oxazolidin-2-ones: a mechanistic probe

The doubly diastereoselective conjugate addition of the antipodes of lithium N-benzyl-N-(α-methylbenzyl)amide to a range of enantiopure N-enoyl oxazolidin-2-ones has been used as a mechanistic probe to determine that the reactive conformation is the anti-s-cis form. The β-amino carbonyl products resulting from these conjugate addition reactions are useful templates for further elaboration into an α,β,α-pseudotripeptide.     

Effects of metal complexation on the accuracy of anodic stripping voltammetry

It is shown that the use of the method of standard additions for electrochemical quantitation, when complexation to form non-electroactive entities can occur, can lead to serious problems with accuracy. It is also shown that the errors can often be compensated through the use of correct calibration models.