Plasma phospholipids implicated in the matrix effect observed in liquid chromatography/tandem mass spectrometry bioanalysis: evaluation of the use of colloidal silica in combination with divalent or trivalent cations for the selective removal of phospholipids from plasma

The feasibility of the use of colloidal silica in combination with a number of divalent or trivalent cations for the removal of plasma phospholipids was evaluated by sequentially adding the two reagents (i.e., colloidal silica and a cation) directly to blank plasma samples or plasma samples spiked with analytes. Three representative plasma phospholipids were monitored to determine the efficiency of the phospholipids removal under different reagent combinations. The recovery of each spiked analyte was also monitored under each condition in order to determine if any of the analyte was removed along with the phospholipids. By optimizing the amounts of the reagents used and the sequence of the addition of the reagents, quantitative and reproducible removal of the phospholipids was achieved. Using the finally selected lanthanum cation, the removal of phospholipids was achieved with minimal concomitant loss of the ten investigated analytes which were carefully selected to incorporate functional groups that could potentially interact with the added reagents and hence could be removed along with the phospholipids. Copyright (c) 2008 John Wiley & Sons, Ltd.     

Structural analysis and thermochemistry of “A” type phosphostrontium carbonate hydroxyapatites

“A” type phosphostrontium carbonate hydroxyapatites, having the general formula Sr₁₀(PO₄)₆(OH)_(2−2x)(CO₃) _x with 0 ≤ x ≤ 1, were synthesised by solid gas reaction at high temperature. The samples were characterised by X-ray diffraction and infrared spectroscopy. Analysis of carbonate was achieved by coulometry and Rietveld refinement of the structure. Using an isoperibol calorimeter, the heat of solution of these products was measured at 298 K in 9 wt% nitric acid solution. Thermochemical cycle was proposed and complementary experiences were performed to reach the standard enthalpies of formation of these compounds. The results showed a decrease of the enthalpy of formation with the amount of carbonate introduced in the lattice, suggesting an increase of stability due to this kind of substitution.     

The phase diagram of CsNO<Subscript>3</Subscript>–RbNO<Subscript>3</Subscript>

The phase transitions of RbNO₃ and the binary phase diagram of (Cs,Rb)NO₃ were investigated at atmospheric pressure, using simultaneous direct and differential thermal analysis, μDTA and DSC techniques. A fourth phase transition of RbNO₃ has been observed at temperature near the melting point. The phase diagram of this system is characterised by a eutectic, two eutectoid and an azeotropic-like invariants. Three limited solid solutions and two continuous solid solutions have been detected at low temperature.