Interlaboratory study of a supercritical fluid chromatography method for the determination of pharmaceutical impurities: Evaluation of multi-systems reproducibility.

Modern supercritical fluid chromatography (SFC) is now a well-established technique, especially in the field of pharmaceutical analysis. We recently demonstrated the transferability and the reproducibility of a SFC-UV method for pharmaceutical impurities by means of an inter-laboratory study. However, as this study involved only one brand of SFC instrumentation (Waters®), the present study extends the purpose to multi-instrumentation evaluation.

First inter-laboratory study of a Supercritical Fluid Chromatography method for the determination of pharmaceutical impurities.

Supercritical Fluid Chromatography (SFC) has known a strong regain of interest for the last 10 years, especially in the field of pharmaceutical analysis. Besides the development and validation of the SFC method in one individual laboratory, it is also important to demonstrate its applicability and transferability to various laboratories around the world. Therefore, an inter-laboratory study was conducted and published for the first time in SFC, to assess method reproducibility, and evaluate whether this chromatographic technique could become a reference method for quality control (QC) laboratories.

Natural compounds analysis using liquid and supercritical fluid chromatography hyphenated to mass spectrometry: Evaluation of a new design of atmospheric pressure ionization source.

The MS hyphenation performance of UniSpray®, a new design of atmospheric pressure ionization source was evaluated in both SFC and RPLC modes. Sensitivity, stability, versatility and matrix effects offered by the UniSpray were assessed in positive and negative ionization modes and systematically compared to an electrospray source (ESI) using 120 natural compounds covering an extended chemical space. In a first instance, a multivariate approach was used to screen and optimize the UniSpray source settings to maximize detection sensitivity.

A systematic investigation of sample diluents in modern supercritical fluid chromatography.

This paper focuses on the possibility to inject large volumes (up to 10μL) in ultra-high performance supercritical fluid chromatography (UHPSFC) under generic gradient conditions. Several injection and method parameters have been individually evaluated (i.e.

Quantitative Profiling of Endogenous Fat-Soluble Vitamins and Carotenoids in Human Plasma Using an Improved UHPSFC-ESI-MS Interface.

Analytical solutions enabling the quantification of circulating levels of liposoluble micronutrients such as vitamins and carotenoids are currently limited to either single or a reduced panel of analytes. The requirement to use multiple approaches hampers the investigation of the biological variability on a large number of samples in a time and cost efficient manner. With the goal to develop high-throughput and robust quantitative methods for the profiling of micronutrients in human plasma, we introduce a novel, validated workflow for the determination of 14 fat-soluble vitamins and carotenoids in a single run.

Optimized selection of liquid chromatography conditions for wide range analysis of natural compounds.

Plant secondary metabolites are an almost unlimited reservoir of potential bioactive compounds. In view of the wide chemical space covered by natural compounds, their comprehensive analysis requires multiple and complementary approaches. In this study, numerous chromatographic conditions were tested for the analysis of a set of 120 representative natural compounds covering a wide polarity range (18 log P units).

Ultra-high performance supercritical fluid chromatography coupled with quadrupole-time-of-flight mass spectrometry as a performing tool for bioactive analysis.

Secondary metabolites are an almost unlimited reservoir of potential bioactive compounds. In view of the wide chemical space covered by natural compounds, their comprehensive analysis requires multiple cutting-edge approaches. This study evaluates the applicability of ultra-high performance supercritical fluid chromatography coupled to quadrupole-time-of-flight mass spectrometry (UHPSFC-QqToF-MS) as an analytical strategy for plant metabolites profiling.

Ultra high performance supercritical fluid chromatography coupled with tandem mass spectrometry for screening of doping agents. II: Analysis of biological samples.

The potential and applicability of UHPSFC-MS/MS for anti-doping screening in urine samples were tested for the first time. For this purpose, a group of 110 doping agents with diverse physicochemical properties was analyzed using two separation techniques, namely UHPLC-MS/MS and UHPSFC-MS/MS in both ESI+ and ESI- modes. The two approaches were compared in terms of selectivity, sensitivity, linearity and matrix effects.

Ultra high performance supercritical fluid chromatography coupled with tandem mass spectrometry for screening of doping agents. I: Investigation of mobile phase and MS conditions.

The conditions for the analysis of selected doping substances by UHPSFC-MS/MS were optimized to ensure suitable peak shapes and maximized MS responses. A representative mixture of 31 acidic and basic doping agents was analyzed, in both ESI+ and ESI- modes. The best compromise for all compounds in terms of MS sensitivity and chromatographic performance was obtained when adding 2% water and 10mM ammonium formate in the CO2/MeOH mobile phase.

Comparison of liquid chromatography and supercritical fluid chromatography coupled to compact single quadrupole mass spectrometer for targeted in vitro metabolism assay.

The goal of this study was to evaluate the combination of powerful chromatographic methods and compact single quadrupole MS device for simple in vitro cytochrome P450 (CYP) inhibition assay, instead of more expensive triple quadrupole MS/MS detectors. For this purpose, two modern chromatographic approaches (ultra-high pressure liquid chromatography (UHPLC) and ultra-high performance supercritical fluid chromatography (UHPSFC)) were tested in combination with simple MS detector. To show the applicability for an in vitro CYP-mediated metabolism assay using the cocktail approach, a method was first developed in UHPLC-MS to separate a mixture of 8 probe substrates and 8 CYP-specific metabolites.

Evaluation of stationary phases packed with superficially porous particles for the analysis of pharmaceutical compounds using supercritical fluid chromatography.

Superficially porous particles (SPP), or core shell particles, which consist of a non-porous silica core surrounded by a thin shell of porous silica, have gained popularity as a solid support for chromatography over the last decade. In the present study, five unbonded silica, one diol, and two ethylpyridine (2-ethyl and 4-ethyl) SPP columns were evaluated under SFC conditions using two mixtures, one with 17 drug-like compounds and the other one with 7 drug-like basic compounds. Three of the SPP phases, SunShell™ 2-ethylpyridine (2-EP), Poroshell™ HILIC, and Ascentis(®) Express HILIC, exhibited superior performances relative to the others (reduced theoretical plate height (hmin) values of 1.

Modern analytical supercritical fluid chromatography using columns packed with sub-2 μm particles: a tutorial.

This tutorial provides an overview of the possibilities, limitations and analytical conditions of modern analytical supercritical fluid chromatography (SFC) using columns packed with sub-2 μm particles. In particular, it gives a detailed overview of commercially available modern SFC instrumentation and the detectors that can be employed (UV, MS, ELSD, FID, etc.).

Coupling state-of-the-art supercritical fluid chromatography and mass spectrometry: from hyphenation interface optimization to high-sensitivity analysis of pharmaceutical compounds.

The recent market release of a new generation of supercritical fluid chromatography (SFC) instruments compatible with state-of-the-art columns packed with sub-2μm particles (UHPSFC) has contributed to the reemergence of interest in this technology at the analytical scale. However, to ensure performance competitiveness of this technique with modern analytical standards, a robust hyphenation of UHPSFC to mass spectrometry (MS) is mandatory. UHPSFC-MS hyphenation interface should be able to manage the compressibility of the SFC mobile phase and to preserve as much as possible the chromatographic separation integrity.

Maximizing kinetic performance in supercritical fluid chromatography using state-of-the-art instruments.

Recently, there has been a renewed interest in supercritical fluid chromatography (SFC), due to the introduction of state-of-the-art instruments and dedicated columns packed with small particles. However, the achievable kinetic performance and practical possibilities of such modern SFC instruments and columns has not been described in details until now. The goal of the present contribution was to provide some information about the optimal column dimensions (i.

Evaluation of various chromatographic approaches for the retention of hydrophilic compounds and MS compatibility.

The goal of this study was to compare the performance of three separation techniques for the analysis of 57 hydrophilic compounds. RPLC, hydrophilic interaction liquid chromatography (HILIC) and subcritical fluid chromatography (SFC) were tested. The comparison was based on the retention, selectivity, peak shape (asymmetry and peak width) and MS sensitivity.

Evaluation and comparison of various separation techniques for the analysis of closely-related compounds of pharmaceutical interest.

The aim of the present work was to compare various separation techniques for the fast analysis of closely-related compounds, including structurally-related compounds, positional isomers, diastereoisomers, Z/E isomers. Three analytical techniques were evaluated, namely ultra high performance liquid chromatography (UHPLC), ultra high performance supercritical fluid chromatography (UHPSFC), both with sub-2μm particles, and capillary electrophoresis (CE) using non-aqueous solvents. To fairly compare the three analytical techniques, only two starting conditions for further method development were considered.

Comparison of ultra-high performance supercritical fluid chromatography and ultra-high performance liquid chromatography for the analysis of pharmaceutical compounds.

Currently, columns packed with sub-2 μm particles are widely employed in liquid chromatography but are scarcely used in supercritical fluid chromatography. The goal of the present study was to compare the performance, possibilities and limitations of both ultra-high performance liquid chromatography (UHPLC) and ultra-high performance supercritical fluid chromatography (UHPSFC) using columns packed with sub-2 μm particles. For this purpose, a kinetic evaluation was first performed, and van Deemter curves and pressure plots were constructed and compared for columns packed with hybrid silica stationary phases composed of 1.

Analysis of basic compounds by supercritical fluid chromatography: attempts to improve peak shape and maintain mass spectrometry compatibility.

While neutral and acidic compounds are well separated by supercritical fluid chromatography (SFC), basic analytes are more challenging to separate and often problems occur with their peak shapes. Two different methods were explored in the present paper to reduce these problems and maintain compatibility with mass spectrometry (MS). Five different, commercially available 2-ethylpyridine (2-EP) stationary phases were tested without a mobile phase additive using 92 pharmaceutical compounds with basic properties.