Sample Preparation Route Research Articles

Measurement of particle size distribution of tripalmitin crystals in a model solution using a laser diffraction method

AbstractThe form and size distribution of tripalmitin (PPP) crystals formed by quenching a solution in a batch crystallizer have been studied using scanning electron microscopy and a laser diffraction technique. Although the accuracy of the laser technique for particle sizing was affected by the nonsphericity of the crystals, the technique proved to be effective and very reproducible. Crystals recovered by filtration and sonication for laser sizing exhibited markedly different particle size distributions (PSD) and shapes compared to those prepared using another standard route, namely, suspension in butanol and centrifugation. Solutions of 2–10 wt% PPP in a paraffin solvent were crystallized at 25–40°C and displayed two ranges of behavior: (i) rapid growth under strongly supersaturated conditions, yielding narrow PSD of plate and needle‐like crystals; and (ii) slow growth in the metastable regime, yielding spherulitic aggregates of platelets that broke down under sonication during preparation for laser sizing. Suspension in alcohol followed by centrifugation yielded aggregates that did not break down under sonication, indicating that the sample preparation route affected the result of the analysis.

Capillary electrophoresis–mass spectrometry coupling versus micro-high-performance liquid chromatography–mass spectrometry coupling: a case study

Capillary zone electrophoresis (CZE) and micro-high-performance liquid chromatography (μ-HPLC) coupled to electrospray ionisation (ESI) mass spectrometry were compared with respect to their applicability to problems arising in pharmaceutical drug research and development. Both techniques, which are similar with regard to their operational parameters, were coupled to an API III plus triple quadrupole mass spectrometer using laboratory-built interfaces. The results achieved with the two combinations were compared for sensitivity and general applicability to the quantitative analysis of pharmaceuticals in biological fluids. Midazolam, the 8-chloro-6-(2-fluoro-phenyl)-1-methyl-4H-imidazo-[1,5-a][1,4]-benzodiazepine, and three of its metabolites were used as test compounds, either as standard solution or after sample clean-up from human plasma. Following different sample preparation routes, liquid–liquid extraction or solid-phase extraction, differences in detection limits as well as robustness in CZE or μ-HPLC coupled with ion spray mass spectrometry (IS-MS) were investigated. Detection limits of about 500 pg/ml for the drug and 2 ng/ml for the metabolites were achieved, using 1 ml of human plasma, only when liquid–liquid extraction was used for sample preparation. Sample preparation using the simpler and faster solid-phase extraction route resulted in deterioration of the separation or clogging of the columns. In all cases, when standard solutions or sample extracts were used, CZE–ESI-MS provided both different selectivity and greater sensitivity.

Atomic structure of undoped Σ=5 symmetrical-tilt grain boundary in strontium titanate

Strontium titanate is an important electroceramic material which, under appropriate processing and dopant additions exhibits both varistor and Grain Boundary Layer Capacitor (GBLC) behavior. The presence of electrically active grain boundaries is essential for obtaining these properties. The first step towards correlating the grain boundary structure to properties is to determine the detailed atomic structure of the boundary, which includes its geometric structure, chemistry and electronic structure. We present here our TEM investigation of the atomic structure of an undoped (“pristine”) symmetrical tilt grain boundary in SrTiO3. This provides the basic reference structure, changes to which can be studied as a function of doping and/or processing parameters, and correlated to electrical and dielectric properties.Self-supported TEM samples were made from bicrystals of SrTiO3 through the conventional sample preparation route. Fig. 1 shows a high resolution electron micrograph (Hitachi H9000) of a representative grain boundary region in the sample.