Application of prediction intervals to the interpretation of the robustness study of a UHPLC method for the separation of cannabinoids.

Design of Experiments (DoE) is a well-established tool used for analytical methods robustness studies, because of its ability to assess the effect of a great number of factors in a minimal number of experiments. However, when assessing the robustness of an analytical method the analysis of the individual effect of each factor is not sufficient on its own. Some factors may not influence the robustness of the method, but their effect combined with the effects of other factors may have a significant contribution on the robustness of the method, which is not given by conventional analysis of DoE results.

Sub/supercritical fluid chromatography versus liquid chromatography for peptide analysis.

The aim of this study was to evaluate the potential of ultra-high performance supercritical fluid chromatography (UHPSFC) for peptide analysis by comparing its analytical performance to several chromatographic approaches based on reversed-phase liquid chromatography (RPLC), hydrophilic interaction liquid chromatography (HILIC) and mixed-mode liquid chromatography. First, the retention behavior of synthetic peptides with 3 to 30 amino acids and different isoelectric points (acid, neutral, and basic) was evaluated. For all the tested conditions (13 peptides in 8 conditions), only 4 results were not exploitable (not retained or not eluted), confirming that all the tested chromatographic conditions can be successfully applied when analyzing a wide range of diverse peptides.

New perspective for the in-field analysis of cannabis samples using handheld near-infrared spectroscopy: A case study focusing on the determination of Δ-tetrahydrocannabinol.

The aim of the present study was to explore the feasibility of applying near-infrared (NIR) spectroscopy for the quantitative analysis of Δ-tetrahydrocannabinol (THC) in cannabis products using handheld devices. A preliminary study was conducted on different physical forms (entire, ground and sieved) of cannabis inflorescences in order to evaluate the impact of sample homogeneity on THC content predictions. Since entire cannabis inflorescences represent the most common types of samples found in both the pharmaceutical and illicit markets, they have been considered priority analytical targets.

The analysis of cannabinoids in cannabis samples by supercritical fluid chromatography and ultra-high-performance liquid chromatography: A comparison study.

The aim of this work was to develop a supercritical fluid chromatographic method to study the applicability of this emerging technique to cannabinoid analysis and showcase its advantages. During method development, the authors focused on nine phyto-cannabinoids to assess the selectivity needed to potentially perform the quantitation of each cannabinoid. After method development, robustness studies were carried out on this method to gain more information about its qualitative behavior (in terms of critical resolutions) when varying some crucial parameters (concentration of additive, column temperature, starting gradient conditions and column batch).

Implementation of a generic liquid chromatographic method development workflow: Application to the analysis of phytocannabinoids and Cannabis sativa extracts.

A generic liquid chromatographic method development workflow was developed and successfully applied to the analysis of phytocannabinoids and Cannabis sativa extracts. Our method development procedure consists in four steps: At the end, this method development workflow was performed in less than 4 days and minimizes the costs of the method development in liquid chromatography.