On-line reversed-phase liquid chromatography x supercritical fluid chromatography coupled to high-resolution mass spectrometry: A powerful tool for the characterization of advanced biofuels

Devaux, Jason; Mignot, Mélanie; Rouvière, Florent; François, Isabelle; Afonso, Carlos; Heinisch, Sabine

doi:10.1016/j.chroma.2023.463964

Cited by 10 publications

(2 citation statements)

References 42 publications

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“…Thus, the addition of water and the formation of carbonic acid could permit to reach this equilibrium, especially since carbonic acid is a stronger acid than methoxycarbonic acid 38 . Devaux et al 40 performed the RPLC x SFC analysis of biofuels and developed a 1D-SFC method using MeOH/ACN 50/50 (v/v) as a modifier with a similar MS interface. They also observed a significant improvement of ESI+ response when water was added in the methanolic make-up solution.…”

Section: Esi-ms Make-up Screeningmentioning

confidence: 99%

Comprehensive analysis of vitamin D₃ impurities in oily drug products using supercritical fluid chromatography–mass spectrometry

Jambo,

Dispas,

Pérez‐Mayán

et al. 2024

Drug Testing and Analysis

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Vitamin D3, an essential micronutrient, often requires supplementation via medicines or food supplements, which necessitate quality control (QC). This study presents the development of a method for detecting and quantifying seven impurities of vitamin D3 in oily drug products using supercritical fluid chromatography–mass spectrometry (SFC‐MS). Targeted impurities include two esters of vitamin D3 and five non‐esters including four that are isobaric to vitamin D3. Firstly, a screening study highlighted the Torus 1‐AA column and acetonitrile modifier as adequate for the separation, followed by optimization of the SFC conditions. Secondly, make‐up solvent composition and MS settings were optimized to reach high sensitivity. For both the separation and MS response, the screening design of experiments proved useful. Lastly, a fast saponification and liquid–liquid extraction method was developed, enabling efficient sample cleanup and impurities recovery from the complex oily matrix. The SFC‐MS method suitability was assessed in two validation studies. The first study employed the ICH Q2 guideline for impurity limit test to demonstrate method specificity and establish a limit of detection (LOD) and a limit of quantification (LOQ) at 0.2% and 0.5%, respectively, for ester impurities. The second study conducted a comprehensive quantitative assessment for three non‐ester impurities using a total error approach, determining method validity through accuracy profiles. The validated method exhibited reliable performance across impurity concentrations from 0.1% to 2.0%, with estimated LODs ranging from 2 to 7 ng/mL. This study further promotes SFC‐MS as a valuable, versatile, and green tool for routine pharmaceutical QC.

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Section: Esi-ms Make-up Screeningmentioning

confidence: 99%

Comprehensive analysis of vitamin D₃ impurities in oily drug products using supercritical fluid chromatography–mass spectrometry

Jambo,

Dispas,

Pérez‐Mayán

et al. 2024

Drug Testing and Analysis

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show abstract

“…Compared to LC, supercritical fluid chromatography (SFC) offers a number of advantages, such as high efficiency at high flow rates and environmentally friendly and economically advantageous solvents (mainly CO 2 ) . However, coupling LC with SFC can be challenging ,,− due to possible incompatibility of mobile phases and differences in pressure and flow rate between the two chromatographic systems. This typically causes broadening and distortion of the peaks.…”

Section: Introductionmentioning

confidence: 99%

Development of a Two-Dimensional Supercritical Fluid Chromatography System in Multiple Heart-Cutting Modes

Réset,

De Saint Jores,

François

et al. 2024

Anal. Chem.

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In this study, we present the development of a loopbased two-dimensional supercritical fluid system in multiple heartcutting modes (mSFC-SFC), with diode-array and mass spectrometric detection. The instrument design was developed to be as simple as possible, based on a single SFC instrument, with the sole addition of three external 2-port 6-position valves. The objective was to achieve the most complete transfer of a peak from the first to the second dimension, whatever the composition of the mobile phase, i.e., whatever the proportion of carbon dioxide and methanol cosolvent along a wide gradient elution. Thanks to fine adjustment of the valve switching times, the first-dimension peaks were parked in 50 μL or 100 μL loops and later discharged to the second dimension. The interest of this instrument was then demonstrated with a sample application on a natural product: an extract of Citrus aurantium L. bark was analyzed, with a particular focus on chiral flavonoids, neohesperidin, and naringin. In this system, the first dimension was an achiral separation of the flavonoids, based on a polar diethylamine-bonded silica stationary phase (ACQUITY Torus DEA), while the second dimension used a stereoselective polysaccharide stationary phase (CHIRALPAK IB-3) to resolve flavonoid diastereomers. Excellent repeatability was demonstrated, with relative standard deviation values on retention times and peak areas all below 2%, together with excellent peak capacity and peak shapes (no distortion observed), making it possible to quantify diastereomers in the second-dimension separation. This good repeatability was also shown for the transfer rate between the two dimensions, which reached a value of 83%. Finally, transferring a compressible sample from the first to the second dimension is demonstrated to yield excellent performance, despite the large loop volume.

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Development of an ultra-high-performance supercritical fluid chromatography method for the analysis of phenols in the pyrolysis aqueous fraction

dos S. Gois,

de S. Santos,

Santana

et al. 2023

Anal Bioanal Chem

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On-line reversed-phase liquid chromatography x supercritical fluid chromatography coupled to high-resolution mass spectrometry: A powerful tool for the characterization of advanced biofuels

Cited by 10 publications

References 42 publications

Comprehensive analysis of vitamin D₃ impurities in oily drug products using supercritical fluid chromatography–mass spectrometry

Comprehensive analysis of vitamin D₃ impurities in oily drug products using supercritical fluid chromatography–mass spectrometry

Development of a Two-Dimensional Supercritical Fluid Chromatography System in Multiple Heart-Cutting Modes

Development of an ultra-high-performance supercritical fluid chromatography method for the analysis of phenols in the pyrolysis aqueous fraction

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On-line reversed-phase liquid chromatography x supercritical fluid chromatography coupled to high-resolution mass spectrometry: A powerful tool for the characterization of advanced biofuels

Cited by 10 publications

References 42 publications

Comprehensive analysis of vitamin D3 impurities in oily drug products using supercritical fluid chromatography–mass spectrometry

Comprehensive analysis of vitamin D3 impurities in oily drug products using supercritical fluid chromatography–mass spectrometry

Development of a Two-Dimensional Supercritical Fluid Chromatography System in Multiple Heart-Cutting Modes

Development of an ultra-high-performance supercritical fluid chromatography method for the analysis of phenols in the pyrolysis aqueous fraction

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Comprehensive analysis of vitamin D₃ impurities in oily drug products using supercritical fluid chromatography–mass spectrometry

Comprehensive analysis of vitamin D₃ impurities in oily drug products using supercritical fluid chromatography–mass spectrometry