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Analytical Methods : Advancing Methods... Jul 2020Polypyrrole (PPy) is a polymer widely used as an extraction phase due to its ability to perform intermolecular interactions with the analyte, such as acid-base, π-π,...
Polypyrrole (PPy) is a polymer widely used as an extraction phase due to its ability to perform intermolecular interactions with the analyte, such as acid-base, π-π, dipole-dipole, hydrophobic, and hydrogen bonding. In this manuscript, we report the coating of a stainless steel needle with a PPy film for analyte extraction and subsequent analysis by electrospray ionization mass spectrometry (ESI-MS) under ambient and open-air conditions. The method, named PPy-ESI-MS, was optimized for analysis of 3,4-methylenedioxyamphetamine (MDA) and 3,4-methylenedioxymethamphetamine (MDMA) in synthetic urine. Seven cycles of electrodeposition of the PPy film onto the needle surface, sample at pH 8, and 40 min of extraction of analytes were determined as the best analysis conditions. The analytical performance of PPy-ESI-MS was evaluated for MDA and MDMA compounds. Analytical curves were obtained with R2 > 0.98. Limits of detection (LODs) and limits of quantification (LOQs) were determined as 20 μg L-1 and 70 μg L-1 for MDA and as 25 μg L-1 and 80 μg L-1 for MDMA, respectively. Values of precision were below 17%, and values of accuracy below 5%. The apparent recoveries ranged between 84.5% and 111.3%. In addition, the PPy-ESI-MS method was applied for the analysis of sarcosine in synthetic urine in order to evaluate the performance of the method for another class of compounds. The calibration curve was obtained with R2 > 0.98, along with LOD and LOQ of 30 μg L-1 and 100 μg L-1, respectively. The precision and accuracy values were below 5% and 8%, respectively, and the apparent recoveries close to 100%. This work demonstrates the usefulness of combining an extraction phase with ESI-MS analysis under ambient conditions to determine different classes of small molecules in a complex sample.
PubMed: 32930186
DOI: 10.1039/d0ay00652a -
EJIFCC Apr 2024A business intelligence (BI) tool in a laboratory workflow offers various benefits, including data consolidation, real-time monitoring, process optimization, cost... (Review)
Review
A business intelligence (BI) tool in a laboratory workflow offers various benefits, including data consolidation, real-time monitoring, process optimization, cost analysis, performance benchmarking (quality indicators), predictive analytics, compliance reporting, and decision support. These tools improve operational efficiency, quality control, inventory management, cost analysis, and clinical decision-making. This write up reveals the workflow process and implementation of BI in a private hospital laboratory. By identifying challenges and overcoming them, laboratories can utilize the power of BI and analytics solutions to accelerate healthcare performance, lower costs, and improve care quality. We used navify (Viewics) as a BI platform which relies on an infinity data warehouse for analytics and dashboards. We applied it for pre-analytic, analytic and post-analytic phases in laboratory. We conclude, digitalization is crucial for innovation and competitiveness, enhancing productivity, efficiency, and flexibility in future laboratories.
PubMed: 38706734
DOI: No ID Found -
Analytical and Bioanalytical Chemistry Jan 2024The development and expansion of analytical methods for per- and polyfluoroalkyl substances (PFAS) in food are essential for the continued monitoring of the United...
The development and expansion of analytical methods for per- and polyfluoroalkyl substances (PFAS) in food are essential for the continued monitoring of the United States (US) food supply and assessments of dietary exposure. In March 2022, the European Union Reference Laboratory for Halogenated Persistent Organic Pollutants in Feed and Food (EURL POPs) released a guidance document covering priority PFAS of interest, including analytical method parameters and limits of quantification (LOQs). As a result, the Food and Drug Administration (FDA) began method extension work to incorporate ten new additional analytes to method C-010.02 including long-chain perfluorosulfonic acids, fluorotelomer sulfonates, and perfluorooctane sulfonamide. Four long-chain carboxylic acids were also validated across all foods, which were previously added to C-010.02 but only validated in seafood. In December 2022, the European Union published Commission Regulation 2022/2388, establishing maximum levels for perfluorooctane sulfonic acid (PFOS), perfluorooctanoic acid (PFOA), perfluorononanoic acid (PFNA), and perfluorohexane sulfonic acid (PFHxS) in certain foodstuffs, primarily fish, molluscs, crustaceans, and eggs. As a result, the FDA method was evaluated for performance in reaching LOQs defined in Commission Regulation (EU) 2022/1431. The FDA method was found to be able to reach all required LOQs for analytes in matrices with established maximum levels. Currently, method detection limits (MDLs), which are used by the FDA as the lower limit for reporting PFAS in surveillance samples, were in the same range as defined indicative levels. With further method modifications, required LOQs could be met in fruits, vegetables, and milk. Reaching the lower targeted LOQs for these food matrices will require moving the method to an instrument that can provide increased signal:noise gains at the lower limits of quantification.
Topics: Animals; United States; Alkanesulfonic Acids; Fluorocarbons; Vegetables; Dietary Exposure; Environmental Pollutants
PubMed: 37528269
DOI: 10.1007/s00216-023-04833-1 -
ACS Omega Jul 2022The use of immunodetection assays including the widely used enzyme-linked immunosorbent assay (ELISA) in applications such as point-of-care detection is often limited by...
The use of immunodetection assays including the widely used enzyme-linked immunosorbent assay (ELISA) in applications such as point-of-care detection is often limited by the need for protein immobilization and multiple binding and washing steps. Here, we describe an experimental and analytical framework for the development of simple and modular "mix-and-read" enzymatic complementation assays based on split luciferase that enable sensitive detection and quantification of analytes in solution. In this assay, two engineered protein binders targeting nonoverlapping epitopes on the target analyte were each fused to nonactive fragments of luciferase to create biosensor probes. Binding proteins to two model targets, lysozyme and Sso6904, were isolated from a combinatorial library of Sso7d mutants using yeast surface display. In the presence of the analyte, probes were brought into close proximity, reconstituting enzymatic activity of luciferase and enabling detection of low picomolar concentrations of the analyte by chemiluminescence. Subsequently, we constructed an equilibrium binding model that relates binding affinities of the binding proteins for the target, assay parameters such as the concentrations of probes used, and assay performance (limit of detection and concentration range over which the target can be quantified). Overall, our experimental and analytical framework provides the foundation for the development of split luciferase assays for detection and quantification of various targets.
PubMed: 35874239
DOI: 10.1021/acsomega.2c02319 -
Journal of Materials Chemistry. B Nov 2022In the last few decades, nanomaterials have made great advances in the biosensor field, thanks to their ability to enhance several key issues of biosensing analytical... (Review)
Review
In the last few decades, nanomaterials have made great advances in the biosensor field, thanks to their ability to enhance several key issues of biosensing analytical tools, namely, sensitivity, selectivity, robustness, and reproducibility. The recent trend of sustainability has boosted the progress of novel and eco-designed electrochemical paper-based devices to detect easily the target analyte(s) with high sensitivity in complex matrices. The huge attention given by the scientific community and industrial sectors to paper-based devices is ascribed to the numerous advantages of these cost-effective analytical tools, including the absence of external equipment for solution flow, thanks to the capillary force of paper, the fabrication of reagent-free devices, because of the loading of reagents on the paper, and the easy multistep analyses by using the origami approach. Besides these features, herein we highlight the multifarious aspects of the nanomaterials such as (i) the significant enlargement of the electroactive surface area as well as the area available for the desired chemical interactions, (ii) the capability of anchoring biorecognition elements on the electrode surface on the paper matrix, (iii) the improvement of the conductivity of the cellulose matrix, (iv) the functionality of photoelectrochemical properties within the cellulose matrix, and (v) the improvement of electrochemical capabilities of conductive inks commonly used for electrode printing on the paper support, for the development of a new generation of paper-based electrochemical biosensors applied in the biomedical field. The state of the art over the last ten years has been analyzed highlighting the various functionalities that arise from the integration of nanomaterials with paper-based electrochemical biosensors for the detection of biomarkers.
Topics: Reproducibility of Results; Nanostructures; Biosensing Techniques; Biomarkers; Cellulose
PubMed: 35899594
DOI: 10.1039/d2tb00387b -
Cells Nov 2022Gaining structural information is a must to allow the unequivocal structural characterization of analytes from natural sources. In liquid state, NMR spectroscopy is... (Review)
Review
Gaining structural information is a must to allow the unequivocal structural characterization of analytes from natural sources. In liquid state, NMR spectroscopy is almost the only possible alternative to HPLC-MS and hyphenating the effluent of an analyte separation device to the probe head of an NMR spectrometer has therefore been pursued for more than three decades. The purpose of this review article was to demonstrate that, while it is possible to use mass spectrometry and similar methods to differentiate, group, and often assign the differentiating variables to entities that can be recognized as single molecules, the structural characterization of these putative biomarkers usually requires the use of NMR spectroscopy.
Topics: Molecular Structure; Magnetic Resonance Spectroscopy; Chromatography, High Pressure Liquid; Mass Spectrometry
PubMed: 36359922
DOI: 10.3390/cells11213526 -
Frontiers in Chemistry 2021Anodic stripping voltammetry (ASV) is a powerful electrochemical analytical technique that allows for the detection and quantification of a variety of metal ion species... (Review)
Review
Anodic stripping voltammetry (ASV) is a powerful electrochemical analytical technique that allows for the detection and quantification of a variety of metal ion species at very low concentrations in aqueous media. While early, traditional ASV measurements relied on macroscopic electrodes like Hg drop electrodes to provide surfaces suitable for plating/stripping, more recent work on the technique has replaced these electrodes with thin film metal electrodes generated . Such electrodes are plated alongside the analyte species onto the surface of a primary electrode, producing a composite metal electrode from which the analyte(s) can then be stripped, identified, and quantified. In this minireview, we will explore the development and use of these unique electrodes in a variety of different applications. A number of metals (e.g., Hg, Bi, Sn, etc.) have shown promise as thin film ASV electrodes in both acidic and alkaline media, and frequently multiple metals in addition to the analyte of interest are deposited together to optimize the plating/stripping behavior, improving sensitivity. Due to the relatively simple nature of the measurement and its suitability for a wide range of pH, it has been used broadly: To measure toxic metals in the environment, characterize battery materials, and enable biological assays, among other applications. We will discuss these applications in greater detail, as well as provide perspective on future development and uses of these thin film electrodes in ASV measurements.
PubMed: 35186893
DOI: 10.3389/fchem.2021.809535 -
Foods (Basel, Switzerland) Oct 2023Multi-analyte methods based on QuEChERS sample preparation and chromatography/mass spectrometry determination are indispensable in monitoring pesticide residues in the...
Multi-analyte methods based on QuEChERS sample preparation and chromatography/mass spectrometry determination are indispensable in monitoring pesticide residues in the feed and food chain. QuEChERS method, even though perceived as convenient and generic, can contribute to sample matrix constituents' introduction to the measuring system and possibly affect analytical results. In this study, matrix effects (ME) were investigated in four food matrices of plant origin (apples, grapes, spelt kernels, and sunflower seeds) during GC-MS/MS analysis of >200 pesticide residues using QuEChERS sample preparation. Data analysis revealed considerable analyte signal enhancement and suppression: strong enhancement was observed for the majority of analytes in two matrices within the commodity groups with high water content-apples, and high acid and water content-grapes (73.9% ME and 72.5% ME, and 77.7% ME and 74.9% ME, respectively), while strong suppression was observed for matrices within the commodity groups with high starch/protein content and low water and fat content-spelt kernels, and high oil content and very low water content-sunflower seeds (82.1% ME and 82.6% ME, and 65.2% ME and 70.0% ME, respectively). Although strong matrix effects were the most common for all investigated matrices, the use of matrix-matched calibration for each sample type enabled satisfactory method performance, i.e., recoveries for the majority of analytes (up to roughly 90%, depending on the fortification level and matrix type), which was also externally confirmed through participation in proficiency testing schemes for relevant food commodity groups with the achieved z-scores within acceptable range ≤ |2|.
PubMed: 37959112
DOI: 10.3390/foods12213991 -
ACS Sensors Oct 2021Potentiometric sensors induce a spontaneous voltage that indicates ion activity in real time. We present here an advanced self-powered potentiometric sensor with memory....
Potentiometric sensors induce a spontaneous voltage that indicates ion activity in real time. We present here an advanced self-powered potentiometric sensor with memory. Specifically, the approach allows for one to record a deviation from the analyte's original concentration or determine whether the analyte concentration has surpassed a threshold in a predefined time interval. The sensor achieves this by harvesting energy in a capacitor and preserving it with the help of a diode. While the analyte concentration is allowed to return to an original value following a perturbation over time, this may not influence the sensor readout. To achieve the diode function, the sensor utilizes an additional pair of driving electrodes to move the potentiometric signal to a sufficiently high base voltage that is required for operating the diode placed in series with the capacitor and between the sensing probes. A single voltage measurement across the capacitor at the end of a chosen time interval is sufficient to reveal any altered ion activity occurring during that period. We demonstrate the applicability of the sensor to identify incurred pH changes in a river water sample during an interval of 2 h. This approach is promising for achieving deployable sensors to monitor ion activity relative to a defined threshold during a time interval with minimal electronic components in a self-powered design.
Topics: Electrodes; Electronics; Potentiometry
PubMed: 34582164
DOI: 10.1021/acssensors.1c01273 -
The Journal of Physical Chemistry. C,... Aug 2022Diagnostic advancements require continuous developments of reliable analytical sensors, which can simultaneously fulfill many criteria, including high sensitivity and...
Diagnostic advancements require continuous developments of reliable analytical sensors, which can simultaneously fulfill many criteria, including high sensitivity and specificity for a broad range of target analytes. Incorporating the highly sensitive attributes of surface-enhanced Raman spectroscopy (SERS) combined with highly specific analyte recognition capabilities via molecular surface functionalization could address major challenges in molecular diagnostics and analytical spectroscopy fields. Herein, we have established a controllable molecular surface functionalization process for a series of textured gold surfaces. To create the molecularly surface-functionalized SERS platforms, self-assembled benzyl-terminated and benzoboroxole-terminated monolayers were used to compare which thicknesses and root-mean-square (RMS) roughness of planar gold produced the most sensitive and specific surfaces. Optimal functionalization was identified at 80 ± 8 nm thickness and 7.2 ± 1.0 nm RMS. These exhibited a considerably higher SERS signal (70-fold) and improved sensitivity for polysaccharides when analyzed using principal component analysis (PCA) and self-organizing maps (SOM). These findings lay the procedure for establishing the optimal substrate specifications as an essential prerequisite for future studies aiming at developing the feasibility of molecular imprinting for SERS diagnostic applications and the subsequent delivery of advanced, highly selective, and sensitive sensing devices and analytical platforms.
PubMed: 36017358
DOI: 10.1021/acs.jpcc.2c03524