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

Spaggiari, Dany; Mehl, Florence; Desfontaine, Vincent; Perrenoud, Alexandre Grand-Guillaume; Fekete, Szabolcs; Rudaz, Serge; Guillarme, Davy

doi:10.1016/j.chroma.2014.10.055

Cited by 41 publications

(24 citation statements)

References 28 publications

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“…Similar sensitivity for LC-MS and SFC-MS was observed also for the analysis of ketoprofen in human plasma [111]. Using a new and simple single quadrupole device, the sensitivities obtained in UHPSFC-MS were found to be about 3-fold lower than those in UHPLC-MS [109]. Therefore, the sensitivity of resulting UHPSFC-MS method is strongly dependent on the mass analyzer type and the type of analyte.…”

Section: Application Of Sfc To the Analysis Of Pharmaceuticals In Biosupporting

confidence: 70%

“…However, again, only retention was discussed, while their influence on ionization process and sensitivity remained neglected. In the study of Spaggiari et al [109], MeOH was found a superior organic modifier than isopropanol with improved MS sensitivity. Similarly to the previous report [106], 2% water was added to the organic modifier being MeOH with 10 mM ammonium formate, due to an important increase in sensitivity in ESI+.…”

Section: Application Of Sfc To the Analysis Of Pharmaceuticals In Biomentioning

confidence: 97%

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Supercritical fluid chromatography in pharmaceutical analysis

Desfontaine

Guillarme

Francotte

et al. 2015

Journal of Pharmaceutical and Biomedical Analysis

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102

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Section: Application Of Sfc To the Analysis Of Pharmaceuticals In Biosupporting

confidence: 70%

Section: Application Of Sfc To the Analysis Of Pharmaceuticals In Biomentioning

confidence: 97%

Supercritical fluid chromatography in pharmaceutical analysis

Desfontaine

Guillarme

Francotte

et al. 2015

Journal of Pharmaceutical and Biomedical Analysis

Self Cite

208

102

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“…One criticism when analyzing biological material in SFC-MS is related to the fact that some endogenous compounds (e.g., polar metabolites and residual proteins or enzymes) may not be eluted from the column, due to their strong interactions through H-bonding with the polar stationary phase commonly employed in SFC [15]. This is why it is essential to perform a suitable sample preparation able to eliminate as much undesired endogenous compounds as possible.…”

Section: Which Matrices and Sample Preparation Techniques Are Suitablmentioning

confidence: 98%

SFC–MS Versus RPLC–MS for Drug Analysis in Biological Samples

2015

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Keywords: MS • plasma • SFC-MS • supercritical fluid chromatography • urine Brief overview of modern supercritical fluid chromatography & coupling of SFC with MSThe advantages of supercritical fluid chromatography (SFC) over LC have been widely described in the past and include enhanced kinetic performance, due to the lower fluid viscosity and better solute diffusion coefficient; lower consumption of organic solvents; highly efficient chiral separation in presence of a supercritical fluid; and improvement of productivity at the preparative scale [1][2][3]. However, all these benefits were restricted by the lack of robustness/reliability, limited sensitivity and poor quantitative performance of old-generation SFC systems. This is certainly why SFC has never been considered as a forefront separation technique since its discovery in 1962 [4]. Over the last few years, a new generation of instruments and columns has appeared on the market. These new systems tackle the above-mentioned shortcomings. In addition, they also make SFC compatible with the most recent column types, such as the ones packed with fully porous sub-2 μm particles, or with sub-3 μm superficially porous particles [5].When dealing with the analysis of biological samples, another important aspect to consider is compatibility of the separation technique with MS, as this detector allows improving selectivity, sensitivity and identification power [6]. In theory, the coupling of SFC with ESI source should be straightforward since the mobile phase is composed of a high proportion of CO 2 , which should enhance the evaporation step during the ionization process. However, it is also important to keep in mind that CO 2 is decompressing through the transfer line between SFC and MS, leading to possible analyte precipitation and poor retention time repeatability. For these reasons, the coupling of SFC with ESI/MS involves the use of a dedicated interface. Among the existing interfaces, some of them are more universal or user friendly, while others are more sensitive [7]. Today, the most advantageous interface seems to be the pre-back pressure regulator (BPR) splitting interface using a make-up pump, as it offers good flexibility in terms of applicable chromatographic conditions, extended robustness and ease of use [7]. Which analytes are compatible with SFC-MS?In the early days of SFC, the mobile phase was exclusively composed of supercritical CO 2 , possessing a polarity close to that of hexane. Therefore, SFC was only suitable for the analysis of highly lipophilic compounds such as petroleum fractions, and remained hardly compatible with drugs and other compounds of biological interest [1,2]. To increase the mobile phase polarity and extend the range of compounds compatible with SFC, an organic modifier (in average between 5 and 40% methanol) is generally added to the supercritical CO 2 . With such a mobile phase, and considering the wide range of stationary phase chemistries available for SFC operation (e.g., polar, nonpolar, aromatic and mixedmode), this sep...

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“…In the present approach a single quadrupole MS was used to assess the enzymatic behavior. Although selective MS/MS or sensitive Time of Flight (ToF) devices are widely used, the reliability of a single quadrupole MS has already been demonstrated for basic targeted CYP studies [45]. However, the discrimination of isomeric metabolites could provide further information regarding interpretation of the obtained results [46].…”

Section: Mass Spectrometric Measurementmentioning

confidence: 99%