A combination of analytical techniques is generally necessary to properly characterize complex lipid materials. Chromatographic separation in conjunction with spectroscopic characterization was utilized for the analysis of the triacylglycerols in the seeds ofAquilegia vulgaris. Reversed-phase high-performance liquid chromatography (HPLC), micropacked argentation supercritical fluid chromatography (SFC), and combinations of the two techniques were used. The fatty acid profile was determined by gas chromatography/mass spectrometry of the picolinyl esters and by gas chromatography/flame-ionization detection of the methyl esters. The major components were also identified by direct inlet mass spectrometry. The excellent selectivity of packed fused silica argentation SFC for the separation of triacylglycerols was demonstrated.

PurposeA versatile methodology is demonstrated for improving dissolution kinetics, gastrointestinal (GI) absorption, and bioavailability of protein kinase inhibitors (PKIs).MethodsThe approach is based on nanoparticle precipitation by sub- or supercritical CO2 together with a matrix-forming polymer, incorporating surfactants either during or after nanoparticle formation. Notably, striking synergistic effects between hybrid PKI/polymer nanoparticles and surfactant added after particle formation is investigated.ResultsThe hybrid nanoparticles, consisting of amorphous PKI embedded in a polymer matrix (also after 12 months), display dramatically increased release rate of nilotinib in both simulated gastric fluid and simulated intestinal fluid, particularly when surfactants are present on the hybrid nanoparticle surface. Similar results indicated flexibility of the approach regarding polymer identity, drug load, and choice of surfactant. The translation of the increased dissolution rate found in vitro into improved GI absorption and bioavalilability in vivo was demonstrated for male beagle dogs, where a 730% increase in the AUC0–24h was observed compared to the benchmark formulation. Finally, the generality of the formulation approach taken was demonstrated for a range of PKIs.ConclusionsHybrid nanoparticles combined with surfactant represent a promising approach for improving PKI dissolution rate, providing increased GI absorption and bioavailability following oral administration.Electronic supplementary materialThe online version of this article (doi:10.1007/s11095-013-1191-4) contains supplementary material, which is available to authorized users.

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A method for quantitative analysis of neutral lipids has been developed. Four different techniques have been combined for this purpose—supercritical fluid chromatography (SFC), silver ion chromatography, packed microcolumns and miniaturized evaporative light‐scattering detection (ELSD). The development and optimization of the method are discussed. The separation of a series of vegetable, fish and hydrogenated oils was demonstrated. Application of eluent composition programming resulted in excellent separation of complex samples. Packed microcolumn argentation SFC provides at least as high a separation power as corresponding high‐performance liquid chromatography methods. The combination of packed microcolumn SFC and miniaturized ELSD constitutes a powerful analytical system for the quantitative analysis of triacylglycerols.

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