Phenolic composition of pomegranate peel extracts using an liquid chromatography-mass spectrometry approach with silica hydride columns.

The peels of different pomegranate cultivars (Molla Nepes, Parfianka, Purple Heart, Wonderful and Vkunsyi) were compared in terms of phenolic composition and total phenolics. Analyses were performed on two silica hydride based stationary phases: phenyl and undecanoic acid columns. Quantitation was accomplished by developing a liquid chromatography with mass spectrometry approach for separating different phenolic analytes, initially in the form of reference standards and then with pomegranate extracts. The high-performance liquid chromatography columns used in the separations had the ability to retain a wide polarity range of phenolic analytes, as well as offering beneficial secondary selectivity mechanisms for resolving the isobaric compounds, catechin and epicatechin. The Vkunsyi peel extract had the highest concentration of phenolics (as determined by liquid chromatography with mass spectrometry) and was the only cultivar to contain the important compound punicalagin. The liquid chromatography with mass spectrometry data were compared to the standard total phenolics content as determined by using the Folin-Ciocalteu assay.

Separation of 1,3-dimethylamylamine and other polar compounds in a dietary supplement formulation using aqueous normal phase chromatography with MS.

Five ingredients (caffeine, L-arginine, creatine, ß-alanine, and 1,3-dimethylamylamine) from a workout supplement were separated by HPLC with UV detection and LC-MS using an analytical column based on silica hydride operating in aqueous normal phase mode. While RP methods were observed to be inadequate for the analysis due to low retention, aqueous normal phase chromatography was able to readily retain and resolve the analytes. After method development on the HPLC-UV system, the conditions were successfully transferred to an LC-MS system for analysis. Based on calibration curve data, estimates of 63.5, 380.3, and 13.1 mg/serving (5.50 g) were obtained for creatine, l-arginine, and 1,3-dimethylamylamine, respectively. Standard addition data results were compared to those of the calibration curve study, and the two values differed by less than 1% in the case of creatine. The conditions are suitable for further development as a reliable means of quantitating the analytes in workout supplement formulations.

Analysis of thiopurines using aqueous normal phase chromatography.

The chromatography of several thiopurines is investigated using aqueous normal phase (ANP) conditions in conjunction with a silica hydride-based column. Both isocratic and gradient elution modes are tested. Detection of higher concentration samples is done by UV to demonstrate feasibility in this format while lower concentration samples utilize mass spectrometry (MS). Repeatability of successive runs is also tested with particular attention to gradient methods where the equilibration time of the stationary phase can be evaluated.

Separation Differences Among Phenyl Hydride, UDC Cholesterol and Bidentate C8 Stationary Phases for Stability Indicating Methods of Tetracyclines: Journal of Liquid Chromatography & Related Technologies.

Formulation extracts of tetracycline hydrochloride (HCl), minocycline hydrochloride (HCl), and doxycycline hyclate were degraded by strong acidic conditions and heating. Subsequently, components of the extracts were separated by Bidentate C8, Phenyl Hydride and Cholesterol (UDC) HPLC columns operating in the reverse phase mode. The Phenyl Hydride column was able to baseline separate minocycline from the observed degradant, while partial or total co-elution was observed with the other two columns using otherwise identical method conditions. For both the degraded tetracycline HCl and doxycycline hyclate extracts, the UDC column gave the best resolution for the critical pair. The findings suggest that the postulated secondary retention mechanisms of π-π interactions from the Phenyl Hydride and shape selectivity from the UDC can provide superior resolution for structurally similar analytes compared to hydrophobic interactions alone.