Journal of chromatography open最新文献

Since the introduction of Quality by Design for production of biopharmaceuticals, the global biopharma industry has been advancing towards developing highly efficient and sensitive platforms for monitoring product quality attributes. Incorporating mass-spectrometry-based multi-attribute monitoring (MAM) as a novel tool for identifying and characterizing post-translational modifications in biotherapeutics has gained increasing traction. The ability of MAM to monitor multiple critical quality attributes coupled with new peak detection functions in a single workflow is highly desirable to the biopharmaceutical industry. This review examines and discusses the evolution and adaptation of MAM for routine product quality assessment. MAM applications in biotherapeutic characterization, comparability, and chemometrics have also been discussed, along with the gaps and future perspectives of the MAM implementation in biopharmaceutical drug development. Primary focus has been kept on major developments in last 6 years (2018–2024).

Rice husk ash is an important waste of agricultural industry that, within the framework of the circular economy, has been easily converted into a sustainable sorbent material. This was tested in this work for the pre-concentration of perfluorooctanoic acid (PFOA) and perfluorooctane sulfonic acid (PFOS), representative perfluoroalkyl substances as probe environmental pollutants of waters, with HPLC-MS/MS quantification. The preparation involves a rapid microwave-assisted oxidation followed by a hydrothermal treatment, which was studied using a 2² design of experiments. The final material was thoroughly characterized and tested for its affinity to the target analytes by solid-phase extraction in environmental waters and wastewaters. Recoveries in the range 67–113 % (RSD < 11 %, n = 3) were achieved at environmentally relevant concentrations (10, 50, and 100 ng L^-1) and the sorbent was reusable for at least ten consecutive extractions. Good linearity (R² = 0.9997) was observed, with a method quantification limit in the water sample of 10 ng L^-1 that allows the analysis of PFOA and PFOS below the established limits. The method was evaluated for greenness using AGREEprep and SPMS metrics, and it was then applied to the analysis of actual water samples from Northern Italy.

Olive oil is the most used vegetable oil for human consumption and its production represents an important economic sector, especially in Mediterranean countries. Olive trees are grown in more than 40 countries around the world on over 10 million hectares. The milling industry generates large quantities of liquid and solid residues, the disposal of which requires sophisticated and rather expensive procedures, given the polluting characteristics of the processing products. Since a considerable measure of olive-derived biomass is generated each year, it could be used as a potential source of bioactive compounds. This work evaluates the possibility of recovering natural antioxidants from by-products of the olive oil mill, through the optimization of extraction processes with green approaches. In the present work, through HPLC-PDA analysis with a validated method, it was possible to characterize a chemical profile of the extracts obtained through an optimized (DoE) and green approach. The waste products of the olive oil companies represent the samples considered in this work, and are derived from the pomace and the washing water of 2-phases, 2.5-phases, and 3-phase extra virgin olive oil (EVO) production plants. The optimized extraction methodology, starting from the 2.5-phase olive pomace, proved to be satisfactory in terms of efficiency by evaluating the effect of parameters such as extraction time and process temperature. The application of this methodology to other types of pomace and agro-industrial by-products has highlighted excellent results in terms of extraction yield, demonstrating the validity of this procedure as also suitable for other solid residues coming from the olive oil mill. Regarding the treatment in vegetation water, the developed protocol allowed the chromatographic profile of the analytes extracted from this matrix to be evaluated, leading to satisfactory results in terms of quantitative yields. Samples of these extracts are also subjected to biological tests in order to evaluate their antioxidant and enzyme inhibition activities.

The main trends in the use of liposomes or lipid aggregates as pseudostationary phases in capillary electrokinetic chromatography (EKC) over the past 15 years are reviewed. Due to the ability of liposomes to mimic cell membranes, they have found wide applications in analytical chemistry and especially in the field of biomedical sciences. Various liposomes, lipid aggregates, and liposomal formulations have been adopted as background electrolytes in EKC and ultraviolet detection is by far the most commonly used detection mode. The possibility to vary the type of lipids and their content in the lipid aggregates has increasingly expanded the usage of liposome EKC for solving specific tasks. The presented data shows that there is great potential of liposome EKC in investigations of interactions between lipid membranes and compounds and the applications are typically related to biomedical and pharmaceutical issues, but not limited to these.

In a recent untargeted clinical lipidomics study of platelets of coronary artery disease (CAD) patients, medium-chain phosphatidylcholines (MCPCs) with C8 and C10 fatty acyl residues were found significantly upregulated in the patient group with acute coronary syndrome (ACS) as compared to chronic coronary syndrome (CCS) and healthy controls. To support this finding, this work presents the development and optimization of a targeted UHPLC-QTrap-MS/MS method with multiple reaction monitoring acquisition for the quantitative analysis of MCPCs (PC 10:0/8:0, PC 16:0/8:0, PC 10:0/20:4 and PC 10:0/10:0) in platelets for biomarker validation. A systematic optimization of chromatographic and mass spectrometric parameters was performed. A charged surface hybrid CSH C18 (1.7 µm, 130 Å) column and fine-tuned gradient elution with 2-propanol/acetonitrile and ammonium acetate as additive to the mobile phase was employed in the final method in ESI negative mode. Four selected PC standards (PC 6:0/6:0, PC 8:0/8:0, PC 10:0/10:0 and PC 12:0/12:0), which cover well the carbon and retention rime range of the target analytes, were used for the optimization process and calibration. Quantification was based on matrix-matched calibration with these four selected commercially available MCPC standards as surrogate calibrants and PC 6:0/6:0(d22) as internal standard. Furthermore, an organic solvent and fatty acyl carbon number-corrected response factor approach gave also accuracies within acceptance limits of bioanalytical validation guidelines and has more generic applicability. Compared to the previous untargeted RPLC-ESI-QTOF-MS/MS method, the optimized targeted UHPLC-QTrap-MS/MS assay showed increased sensitivity and selectivity for the detection of medium-chain PCs in platelet samples of CAD (LOQs in the range of 0.5–5 nmol/L). The method performance parameters indicated its suitability for a future biomarker validation study of MCPCs in platelets.

The chemoselective probe technique combines the benefits of chemical derivatization and solid-phase extraction, allowing for simultaneous enhancement of analyte ionization efficiency, reduction of matrix interference, and improvement in chromatographic separation. This innovative technique holds great promise for applications in metabolomics research, metabolic tracking, and natural product isolation and purification. This review provides a comprehensive overview of the advancements in chemoselective probes from 2007 to 2024, focusing on the progress in probe design, particularly cleavable linkers. Additionally, it discusses the application of chemoselective probes in LC-MS analysis of small-molecular-weight compounds.

With the growing demand for rapid processing of laboratory samples, great efforts have been dedicated to improving the speed and throughput of solid phase extraction (SPE), a widely used sample pretreatment technique. This review comprehensively summarizes the latest advancements in accelerating SPE within the last five years, with a focus on three crucial aspects: novel extraction materials, field-assisted technology, and online coupling. It provides an update of the remarkable features and applications of advanced and novel sorbents, as well as novel devices used in SPE. The mainstream approach for accelerating SPE continues to be the development of novel sorbents with large surface area and high porosity. Additionally, promising results have been achieved through the design of novel devices for field-assisted SPE or highly integrated online SPE systems. This review also addresses current limitations and presents future prospects for the acceleration of SPE. By consolidating recent developments and discussing potential directions, this review endeavors to shed light on the path towards faster and more efficient SPE, imparting substantial benefits to various analytical applications.

The Abraham's solvation parameter model is an important tool to model and predict distribution properties of compounds in numerous partitioning systems in chemistry, environmental chemistry, medicine, and biology. The evaluation of the distribution properties in extractables and leachables (E&L) studies in pharmaceutical and medical device industries is another major application of this model. This tutorial is aimed at illustrating the applications of the model in E&L studies. Specific examples of the application illustrated in this tutorial include: (a) establishment of equivalent or similar solvents; (b) determination of polarity of solvents, biological tissues, and materials; (c) development of drug product simulating solvents; (d) understanding solvent extraction power for a material; (e) selection of solvent and standards in pretreatment of extraction samples; and (f) chromatography retention prediction for E&L.

Solid-phase analytical derivatization is a versatile sample preparation technique that enhances analysis accuracy, efficiency, reproducibility, and sensitivity. The technique combines the advantages of analytical derivatization and solid-phase extraction, providing a versatile approach for analysing analytes with various functional groups in complex matrices. Analytical derivatization is a technique used for functional group analysis that involves modifying the structure of an analyte to enhance sensitivity and specificity. Solid-phase analytical derivatization is a one-pot procedure that combines analytical derivatization and extraction. In the presence of acids, it can derivatize phenols, carboxylic acids, and other analytes. Furthermore, solid-phase analytical derivatization increases the reaction rate of carbonyl compounds, making it easier to extract aldehydes and ketones rapidly. This technique utilises electrophoresis, chromophores, fluorophores, and functional groups for detection and extraction. It initially began as a batch procedure but has now developed into an automated, microextraction, and derivatization method. Solid-phase analytical derivatization is highly efficient due to the significant excess of the derivatizing reagent relative to the analyte, along with the pre-impregnation of derivatizing reagents, which can speed up the process compared to traditional solution-based derivatization. This tutorial aims to provide detailed insights into the practical aspects of implementing solid-phase analytical derivatization in analytical method development and discuss the prospects and future trends.

This paper discusses a novel method for improving resolution in protein separation obtained by membrane chromatography. The method is based on a bipolar membrane system involving the synergistic combination of a modulating membrane and a binding membrane for improving peak sharpness, and resolution in bind-and-elute protein separation. In this study, an anion exchange membrane served as the binding membrane while a cation exchange membrane served as the modulating membrane. Significantly sharper peaks were obtained in single-protein bind-and-elute experiments using modulated bipolar membrane chromatography compared to normal anion exchange membrane chromatography, which served as the control. Significantly greater resolution in binary protein separation was also obtained with modulated bipolar membrane chromatography. The working principles of the method are hypothesized in this paper. Modulated bipolar membrane chromatography could potentially be used for high-resolution analytical separation of proteins and other biological macromolecules.