Non-destructive chromatographic methods were used to determine the hold-up volumes of four self-packed columns containing embedded phosphate groups. The stationary phases are named Diol-P-C10, Diol-P-C18, Diol-P-Benzyl and Diol-P-Chol. The hydrophobicity of organic ligands bound to the phosphate group increases in the benzyl< decyl < octadecyl
The study focuses on the application range of nitrous oxide as a hold-up time marker in supercritical fluid chromatography (SFC). This compound has been suggested a decade ago to be used as unretained marker, something that the field of SFC was missing for a long time, since its beneficial properties make it an ideal candidate as hold-up time marker. Determination of the hold-up volume and actual volumetric flow rates have always been problematic in SFC due to the compressibility of carbon dioxide and one part of this is the difficulty of hold-up time measurements.
View Article and Find Full Text PDFThe adsorption behaviour of caffeine and theophylline under hydrophilic interaction chromatography and purely aqueous conditions was investigated on four phosphodiester stationary phases. Solute adsorption isotherms were determined by frontal analysis or inverse method. The bi-Langmuir model was found to be the best choice to describe the behaviour of caffeine and theophylline adsorption in purely aqueous conditions, whereas the bi-Moreau model describes the adsorption phenomena in HILIC conditions.
View Article and Find Full Text PDFThe growing popularity of cannabis products and recent legalization of cannabis for recreational purposes have contributed to the increase of the demand for analytical methods able to give a detailed characterization of cannabis samples and derivatives. In this context, one of the aspects that is strongly emerging is about the hazardous potential of uncharacterised minor cannabinoids, including chiral ones, for which achiral potency testing methods currently employed do not give any information. For this reason, there is a growing interest towards the development of liquid chromatographic methods for the enantioseparation of cannabinoids.
View Article and Find Full Text PDFThis work reports about a screening of four adsorbents with different polarity employed for the separation of the main phytocannabinoids contained in Cannabis sativa L., under normal phase liquid chromatography (NPLC). The effect of polarity and type of interaction mechanisms of the adsorbents (namely Si-, CN-, Diol-, and NH-based SPs) on retention has been investigated under a variety of conditions either by using different combinations of apolar solvents (heptane or hexane) and alcohols (ethanol or isopropanol).
View Article and Find Full Text PDFHemp and cannabis industry is undergoing a renewed interest due to legalization of marijuana (a topic that all countries are discussing, especially in recent years) and the growing importance of therapeutic properties of cannabinoids. Together with an increment in the production of hemp and recreational cannabis, there has been an increasing demand for accurate potency testing of products (i.e.
View Article and Find Full Text PDFIn this work, a detailed study of mass transfer properties of trans-stilbene oxide (TSO) enantiomers on two Whelk-O1 chiral stationary phases (CSPs) has been performed. The CSPs were prepared by using both fully-porous silica particles of 2.5 μm particle diameter and superficially-porous ones of 2.
View Article and Find Full Text PDFA twin-column Multicolumn Countercurrent Solvent Gradient Purification (MCSGP) process has been developed for the purification of a therapeutic peptide, glucagon, from a crude synthetic mixture. This semi-continuous process uses two identical columns operating either in interconnected or in batch mode, thus enabling the internal recycle of the portions of the eluting stream which do not comply with purity specifications. Because of this feature, which actually results in the simulated countercurrent movement of the stationary phase with respect to the mobile one, the yield-purity trade-off typical of traditional batch preparative chromatography can be alleviated.
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