Review
Chemistry, Analytical
Tatana Gazarkova, Katerina Plachka, Frantisek Svec, Lucie Novakova
Summary: Supercritical fluid chromatography-mass spectrometry (SFC-MS) is a commonly used analytical method that has wide applicability in various fields. However, there are challenges and principles in selecting suitable interfaces and mass analyzers. Additionally, differences arise when using SFC-MS compared to liquid chromatography with atmospheric pressure ionization sources.
TRAC-TRENDS IN ANALYTICAL CHEMISTRY
(2022)
Article
Chemistry, Analytical
Toshinobu Hondo, Chihiro Ota, Yumi Miyake, Hiroshi Furutani, Michisato Toyoda
Summary: PTR-MS is a real-time method used to detect trace VOCs in gaseous samples and is popular in various research fields. Supercritical fluid chromatography offers high separation efficiency and easy optimization. Combining PTR with SFC-MS interface allows for detection of nonvolatile organic compounds.
ANALYTICAL CHEMISTRY
(2021)
Article
Chemistry, Applied
Peilin Guo, Xiaokang An, Wuying Chen, Xinglu Pan, Runan Li, Jun Xu, Xiaohu Wu, Yongquan Zheng, Fengshou Dong
Summary: In this study, fluindapyr enantiomers were successfully separated by supercritical fluid chromatography-mass spectrometry, and it was found that the enantiomers exhibited different degradation behavior in different plants.
Article
Chemistry, Analytical
Fei Yang, Yusong Chen, Jun Liu, Yuan Ji, Kang Wang, Xingyi Jiang, Ying Wang, Shanshan Liu, Ziyan Fan, Zhaoyang Bian, Gangling Tang, Wei Xiong
Summary: Supercritical fluid chromatography tandem mass spectrometry (SFC-MS/MS) is an important tool for analyzing stereoisomers in complex matrices. This study investigated the influence of matrix effect on stereoselective analysis of mevinphos in tobacco by SFC-MS/MS. Experiments showed that a QuEChERS method combined with a dilution strategy effectively eliminated most of the matrix effects.
MICROCHEMICAL JOURNAL
(2022)
Review
Chemistry, Analytical
Laura Toribio, Jose Bernal, Maria Teresa Martin, Ana M. Ares
Summary: In recent years, there has been a growing interest in supercritical fluid chromatography (SFC) in food analysis due to the introduction of modern instruments with improved robustness and hyphenation to mass spectrometry (MS). This allows for high selectivity, sensitivity, and efficient analysis of trace compounds in complex samples.
TRAC-TRENDS IN ANALYTICAL CHEMISTRY
(2021)
Review
Chemistry, Analytical
Maria Kristina Parr, Francesco Botre
Summary: This article reviews the analysis methods of prohibited substances, their metabolites, and biomarkers in sports using SFC-MS(/MS). The current instrumental designs and method development, including sample preparation, are introduced, and selected examples are presented. Furthermore, the advantages of this method over others are evaluated, and potential areas of application and future perspectives are discussed.
TRAC-TRENDS IN ANALYTICAL CHEMISTRY
(2022)
Article
Biochemical Research Methods
Qing Fu, Wenwen Dong, Dandan Ge, Yanxiong Ke, Yu Jin
Summary: This study developed a method based on simultaneous supercritical fluid extraction-sample cleanup, followed by supercritical fluid chromatography/tandem mass spectrometry (SFE-SFC-MS/MS) for the extraction and analysis of alkaloids, specifically indole alkaloids of Uncaria rhynchophylla. By using a two-step SFE method with the addition of adsorbents, the specificity of extraction towards alkaloids was greatly improved. The SFE extract was then analyzed using SFC-MS/MS, and the results confirmed the presence of indole alkaloids. This method is important for the study of alkaline compounds in complex samples.
JOURNAL OF CHROMATOGRAPHY A
(2023)
Article
Chemistry, Analytical
Michael Zwerger, Judith Zelger, Markus Ganzera
Summary: The neophyte plant species S. inaequidens from South Africa has spread widely throughout Europe and the world. All species in this genus contain toxic pyrrolizidine alkaloids (PAs), which pose a potential health hazard to humans and livestock. Efficient and straightforward assays for their qualitative and quantitative analysis are in high demand due to their presence in the food chain and contaminants in herbal crops and phytopharmaceutical formulations.
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
(2023)
Article
Food Science & Technology
Giovanna Cafeo, Antonella Satira, Marina Russo, Monica Mondello, Paola Dugo
Summary: This research aimed to determine oxygen heterocyclic compounds in twenty-six Citrus- and cinnamon-flavoured foods using supercritical fluid chromatography in combination with triple-quadrupole mass spectrometry. The presence of these compounds in all samples analyzed confirmed the use of Citrus fruits in the preparation of the Citrus-flavoured foods. Mandarin juice was found to be the richest source of bioactive compounds, specifically polymethoxyflavones.
Article
Chemistry, Analytical
Peipei Qi, Jiao Wang, Zhenzhen Liu, Zhiwei Wang, Shanshan Di, Huiyu Zhao, Xinquan Wang
Summary: A rapid and accurate analytical method was developed for multiple pesticide residues in complex matrices using magnetic dispersive solid phase extraction (d-SPE) and supercritical fluid chromatography-tandem mass spectrometry (SFC-MS/MS). By using Fe3O4-MgO coupled with PSA and C18 as d-SPE purification adsorbents, efficient removal of interferences in complex matrix was achieved. The proposed method showed good linearity, satisfactory recovery, and wide applicability for pesticide residue analysis in complex samples.
ANALYTICA CHIMICA ACTA
(2023)
Article
Chemistry, Analytical
Yih Ling Saw, John R. Boughton, Faith L. Wroniuk, Mahmoud Elhusseiny Mostafa, Peter J. Pellegrinelli, Samantha A. Calvez, Alexander S. Kaplitz, Lark J. Perez, James L. Edwards, James P. Grinias
Summary: This report explores the use of a high proton affinity N-(4-aminophenyl)piperidine derivatization tag to improve the detection of organic acids by SFC-MS. By derivatizing four organic acids with varying carboxylate groups, detection limits as low as 0.5 ppb were achieved, with overall improvements in detection limit ranging from 25-to-2100-fold. The effect of derivatization on sensitivity, and the possibility of complete separation of these derivatized compounds using SFC, were also described.
JOURNAL OF SEPARATION SCIENCE
(2023)
Article
Chemistry, Analytical
Yingping Dai, Dasen Jiang, Xinhe Wang, Di Wu, Wenwen Dong, Qing Fu, Yu Jin, Xinmiao Liang
Summary: In this study, quality evaluations of Hedyotis diffusa (H. diffusa) batches were conducted using rapid fingerprint analysis based on supercritical fluid chromatography (SFC). The results showed that the SFC method is feasible for batch quality evaluation of H. diffitsa, as it allows for the effective extraction and separation of chemical components in H. diffusa. The fingerprint analysis revealed quality differences of H. diffusa based on origin and harvest year.
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
(2022)
Article
Chemistry, Analytical
Ivan Petr, Ales Pencik, Jakub Styskala, Lenka Tranova, Petra Amakorova, Miroslav Strnad, Ondrej Novak
Summary: The study introduces a novel approach using ultra-high performance supercritical fluid chromatography coupled with tandem mass spectrometry (UHPSFC-MS/MS) for the quantification of plant hormones. Compared to traditional UHPLC-MS/MS methods, this new approach offers a shorter total run time and lower matrix effect.
ANALYTICA CHIMICA ACTA
(2024)
Article
Medicine, Legal
Hiroki Segawa, Yuko T. Iwata, Yuki Okada, Tadashi Yamamuro, Kenji Kuwayama, Kenji Tsujikawa, Tatsuyuki Kanamori
Summary: A supercritical fluid chromatography (SFC) method was developed for the enantiomeric analysis of ZOP, a hypnotic drug. The SFC-MS/MS method achieved the baseline separation of S-ZOP and R-ZOP within 2 minutes, and showed good precision and recovery. The quick analysis ability of this method makes it a valid option for forensic drug analysis.
JOURNAL OF FORENSIC SCIENCES
(2023)
Article
Chemistry, Analytical
Tingting Sun, Jiaoyang Luo, Yuanyuan Xu, Xinqi Sun, Shihai Yang, Meihua Yang
Summary: A new method for separation and quantitation of saikosaponins using UHPSFC was established in this study, successfully separating the five saikosaponins and demonstrating good quantitation in Chaihu Dropping Pills.
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
(2021)
Article
Biochemical Research Methods
Davy Guillarme, Florent Rouviere, Sabine Heinisch
Summary: The objective of this study was to compare one-dimensional reversed-phase liquid chromatography (1D-RPLC) and comprehensive two-dimensional RPLC (RPLC x RPLC) by calculations and experiments. Various quality descriptors were evaluated, and it was found that short columns of 30 x 2.1 mm packed with sub-2-mu m particles should be selected in both dimensions of the 2D-LC setup to obtain the best compromise in terms of peak capacity and sensitivity. The peak capacity in RPLC x RPLC was significantly improved for analysis times beyond 5 min, but the extra-column volume after the second-dimension column was found to be critical for peptides. Higher dilution is not always observed in RPLC x RPLC, and with adequate analytical conditions, RPLC x RPLC can achieve better sensitivity compared to 1D-RPLC.
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
(2023)
Article
Biochemical Research Methods
Paul Thoueille, Ulrich Seybold, Laurent A. Decosterd, Vincent Desfontaine
Summary: Most people living with HIV now have access to highly effective and tolerable HIV treatment. However, drug-resistant viral strains have emerged in some patients due to continued virus replication in the presence of failing drug regimens. Therefore, new treatment options like RUKOBIA are needed for heavily treatment-experienced individuals. The LC-MS/MS method for quantifying temsavir in human plasma has been successfully developed and validated for routine analyses in a clinical pharmacology laboratory.
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
(2023)
Article
Biochemical Research Methods
Vincent Desfontaine, Sylvie Guinchard, Sara Marques, Anthony Vocat, Farizade Moulfi, Francois Versace, Jeff Huser-Pitteloud, Anton Ivanyuk, Carine Bardinet, Vadim Makarov, Olga Ryabova, Pascal Andre, Sylvain Prod'Home, Haithem Chtioui, Thierry Buclin, Stewart T. Cole, Laurent Descorted
Summary: Tuberculosis, especially multidrug-resistant tuberculosis, is a global health threat. Macozinone is a potential candidate for the treatment of drug-resistant Mycobacterium tuberculosis. A LC-MS/MS method was developed for the analysis of plasma samples to support clinical trials of macozinone. The optimization of the method allowed the identification of new metabolites, including H2PBTZ, and these methods were successfully applied in a clinical trial.
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
(2023)
Article
Biochemistry & Molecular Biology
Megane K. Aebischer, Thomas Bouvarel, Emmalyn Barrozo, Dominik Kochardt, Carsten Elger, Markus Haindl, Raphael Ruppert, Davy Guillarme, Valentina D'Atri
Summary: The purity of recombinant adeno-associated virus (rAAV), a gene therapy product, is important for its quality. Various electrophoretic and chromatographic methods were compared for characterizing the three viral proteins (VPs) in this study. Capillary electrophoresis-sodium dodecyl sulfate (CE-SDS) is considered the reference method but has limitations in post-translational modification characterization and species identification. Reversed phase liquid chromatography (RPLC) and hydrophilic interaction chromatography (HILIC) showed compatibility with mass spectrometry (MS) and sensitivity in detecting capsid protein variants, while hydrophobic interaction chromatography (HIC) performed poorly.
INTERNATIONAL JOURNAL OF MOLECULAR SCIENCES
(2023)
Article
Biochemical Research Methods
Sergey Girel, Davy Guillarme, Szabolcs Fekete, Serge Rudaz, Victor Gonzalez-Ruiz
Summary: Monitoring the central carbon metabolism network using LC-MS analysis is challenging due to the diverse chemical nature of analytes and non-specific adsorption on metal surfaces. In this study, different chromatographic methods were investigated for untargeted analysis of energy metabolism-related analytes in biological samples, and the best performance was achieved with sulfoalkylbetaine HILIC. Additionally, an extra hydrophilic modulation may be necessary for better resolution of carboxylic acids in zHILIC mode.
JOURNAL OF CHROMATOGRAPHY A
(2023)
Article
Chemistry, Analytical
Emmanuel Douez, Valentina D'Atri, Davy Guillarme, Daniel Antier, Mathieu Guerriaud, Alain Beck, Herve Watier, Laura Foucault-Fruchard
Summary: Monoclonal antibody (mAb)-based therapies have revolutionized oncology patient care, but their high cost prompted the development of biosimilars as more affordable alternatives. This article focuses on Erbitux® (cetuximab), a monoclonal antibody used for colorectal cancer and head and neck cancer. Despite its patent expiration and profitable sales, Erbitux® has not faced any biosimilar challenges in the US or Europe. The article discusses the complex structure of Erbitux® and the risks associated with demonstrating biosimilarity, as well as the potential of developing Erbitux® biobetters.
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
(2023)
Article
Biochemistry & Molecular Biology
Soraya Chapel, Florent Rouviere, Davy Guillarme, Sabine Heinisch
Summary: The aim of this study is to evaluate the possibilities and limitations of reversed hydrophilic interaction chromatography (revHILIC) mode in liquid chromatography (LC). It was found that the achievable selectivity can be ranked in the order RPLC > revHILIC > HILIC with representative mixtures of peptides and pharmaceutical compounds. Furthermore, the combination of revHILIC and RPLC in a comprehensive (LC x LC) mode showed impressive performance in peak capacity and sensitivity, as well as complementary selectivity compared to other combinations.
Article
Biochemistry & Molecular Biology
Thomas Bouvarel, Nadine Bremeyer, Mimi Gao, Wiebke Holkenjans, Terence Hetzel, Reinhard Pell, Valentina D'Atri, Davy Guillarme
Summary: Antibody-chelator conjugates (ACCs) are a promising class of tumor-targeted pharmaceuticals in targeted radionuclide therapy. A reliable method using liquid chromatography (LC) has been developed to monitor ACC samples and their small molecule impurities. This method addresses common analytical issues such as separation of impurities, interferences from formulation components, analysis of impurities in high concentration samples, and impurity recovery during the entire analytical procedure. This chromatographic method can also be potentially applied to the characterization of similar ACCs and other antibody-related drugs.
Article
Biochemistry & Molecular Biology
Claire I. Butre, Valentina D'Atri, Helene Diemer, Olivier Colas, Elsa Wagner, Alain Beck, Sarah Cianferani, Davy Guillarme, Arnaud Delobel
Summary: The concept of multi-attribute method (MAM) has been introduced to enhance the quality-by-design process development in biopharmaceutical companies. MAM strategies rely on LC-MS technology to identify and quantify critical quality attributes (CQA) in a single assay. This study evaluated the repeatability and robustness of a benchtop LC-MS platform and bioinformatics data treatment pipelines for peptide mapping-based MAM studies, benchmarking MAM methods across laboratories using nivolumab as a case study. The results demonstrated strong interlaboratory consistency in all CQAs and emphasized the importance of bioinformatics postprocessing in MAM studies.
Article
Biochemistry & Molecular Biology
Paulina Biniecka, Saki Matsumoto, Axel Belotti, Jessie Joussot, Jian Fei Bai, Somi Reddy Majjigapu, Paul Thoueille, Dany Spaggiari, Vincent Desfontaine, Francesco Piacente, Santina Bruzzone, Michele Cea, Laurent A. A. Decosterd, Pierre Vogel, Alessio Nencioni, Michel A. A. Duchosal, Aimable Nahimana
Summary: The newly synthesized NAMPT inhibitor JJ08 exhibits a broad anticancer activity in vitro by inhibiting NAD(+) and NADP(H), generating ROS, and inducing cell death. In a mouse xenograft model of human Burkitt lymphoma, JJ08 delays tumor growth and shows potential for further evaluation in hematological malignancies.
Article
Chemistry, Analytical
Honorine Lardeux, Szabolcs Fekete, Matthew Lauber, Valentina D'Atri, Davy Guillarme
Summary: Ion-pairing reversed-phase liquid chromatography (IP-RPLC) is the reference separation technique for characterizing oligonucleotides (ONs) and their related impurities. This study aimed to understand the retention mechanism of ONs, evaluate the applicability of the linear solvent strength (LSS) retention model, and explore ultra-short columns for ONs separation. It was found that 5-35 mm column lengths were appropriate for most gradient separation conditions. Baseline separation of three model ONs mixtures was achieved in as little as 30 seconds on the 5 mm column. This proof-of-concept work paves the way for future investigations using more complex therapeutic ONs and their related impurities.
ANALYTICAL CHEMISTRY
(2023)
Article
Chemistry, Multidisciplinary
Florentin Coppey, Cedric Schelling, Jean-Luc Veuthey, Pierre Esseiva
Summary: This article introduces an innovative technology or technology architecture that integrates a handheld device, Viavi MicroNIR, with a cloud-based system. By analyzing cannabis specimens, the transformative impact of this technology on field operators is demonstrated, with a particular focus on the system's ability to distinguish between CBD-type and THC-type cannabis. The near-infrared (NIR) spectra show remarkable congruence with the reference analytical method. The article highlights the advantages of this application in expediting routine illicit drug analysis and alleviating the burden on laboratories, providing laboratory personnel with additional time for more complex cases, thus enhancing overall efficiency.
HELVETICA CHIMICA ACTA
(2023)
Review
Chemistry, Analytical
Szabolcs Fekete, Megane K. Aebischer, Mateusz Imiolek, Tobias Graf, Raphael Ruppert, Matthew Lauber, Valentina D'Atri, Davy Guillarme
Summary: In recent years, there has been a significant increase in the biopharmaceutical industry's interest in gene therapy modalities. Fit-for-purpose analytical methods are crucial to ensure the quality of gene therapy products during manufacturing and upstream/downstream process. However, the characterization of these products remains challenging due to their large size, structural complexity, heterogeneity, potential instability, and limited sample availability. This review focuses on the use of liquid chromatography (LC) based methods for analyzing adeno-associated virus (AAV) vector-based gene therapy products, highlighting their advantages, drawbacks, and unique capabilities in the analysis of AAV gene transfer vehicles and their impurities.
TRAC-TRENDS IN ANALYTICAL CHEMISTRY
(2023)
Article
Biochemical Research Methods
Raquel Perez-Robles, Szabolcs Fekete, Robert Kormany, Natalia Navas, Davy Guillarme
Summary: There is a mismatch between the sample diluent and the mobile phase in HILIC analysis, leading to analyte breakthrough and peak distortion. Adding a weak solvent for pre-injection can effectively prevent these issues and improve sensitivity.
JOURNAL OF CHROMATOGRAPHY A
(2024)
Article
Biochemistry & Molecular Biology
Bastiaan Laurens Duivelshof, Thomas Bouvarel, Sebastian Pirner, Vincent Larraillet, Alexander Knaupp, Hans Koll, Valentina D'Atri, Davy Guillarme
Summary: Charge heterogeneity among therapeutic monoclonal antibodies is an important quality attribute that requires careful characterization. The use of solvent-enriched mobile phase composition can improve selectivity for the analysis of various antibody products.
INTERNATIONAL JOURNAL OF MOLECULAR SCIENCES
(2023)
