Search Results (38)

This report presents the first method for simultaneous determination of the 2-S-lepidinium derivatives of total α-lipoic acid (LA), homocysteine (Hcy), cysteinylglycine (CysGly), and cysteine (Cys) in human saliva, using capillary electrophoresis with pH-mediated sample stacking and ultraviolet detection (CE-UV) at 355 nm. Electrophoretic separation is carried out at 20 kV and 25 °C using a standard fused silica capillary (effective length 91.5 cm, inner diameter 75 µm). The background electrolyte consists of 0.5 mol/L lithium acetate buffer, adjusted to pH 3.5 with 0.5 mol/L acetic acid. The limit of quantification was determined to be 1 µmol/L for LA and 0.17 µmol/L for Hcy, 0.11 µmol/L for CysGly, and 0.10 µmol/L for Cys in saliva samples. Calibration curves demonstrated linearity over the concentration range of 3 to 30 µmol/L for all analytes. Method precision did not exceed 4.7%, and accuracy ranged from 87.9% to 114.0%. The developed method was successfully applied to saliva samples from eleven apparently healthy volunteers to determine the content of LA, Hcy, CysGly, and Cys. The Hcy, CysGly, and Cys concentrations ranged from 0.55 to 13.76 µmol/L, 0.89 to 9.29 µmol/L, and 1.73 to 12.99 µmol/L, respectively. No LA-derived peaks were detected in the native saliva samples. Full article

To enhance the signal intensity of kynurenines, which are present at trace concentrations in biological fluids, a novel analytical approach was developed, combining pressure-assisted electrokinetic injection (PAEKI) with a mixed micelle system based on sodium dodecyl sulfate (SDS) and Brij-35. The method was applied to key compounds of the kynurenine pathway, including L-tryptophan, kynurenine, 3-hydroxykynurenine, and kynurenic acid, as well as to the aromatic amino acids (AAs) L-tyrosine and L-phenylalanine. PAEKI was performed by electrokinetic injection for 2 min at −6.5 kV (reversed polarity) and 0.5 psi (3.45 kPa) using a fused silica capillary (50 cm in length, 50 µm inner diameter). The background electrolyte (BGE) consisted of 20 mM Na₂B₄O₇ (pH 9.2), 2 mM Brij-35, 20 mM SDS, and 20% (v/v) methanol (MeOH). The limit of detection (LOD) using a diode array detector (DAD) was 1.2 ng/mL for kynurenine and ranged from 1.5 to 3.0 ng/mL for the other analytes. The application of PAEKI in conjunction with micellar electrokinetic capillary chromatography (MEKC) and solid-phase extraction (SPE) of artificial urine samples resulted in a 146-fold increase in signal intensity for kynurenines compared to that observed using the hydrodynamic injection (HDI) mode. The developed method demonstrates strong potential for determining kynurenine pathway metabolites in complex biological matrices. Full article

We present a corrosion-resistant quadrupole ion trap mass spectrometer (QIT-MS) for the direct detection of biosignature gasses in chemically reactive planetary atmospheres, such as Venusian clouds. The system employs a Paul trap with hyperbolic titanium alloy electrodes and alumina spacers for chemical durability and precise ion confinement. An yttria-coated iridium filament serves as the thermionic emitter within a modular electron gun capable of axial and radial ionization. Analytes are introduced through fused silica capillaries and crescent inlets into a miniature pressure cell. The testbed integrates high-voltage RF electronics, pressure-regulated sample delivery, and FPGA-based control for real-time tuning. Continuous operation in 98% sulfuric acid vapor for over three months demonstrated no degradation in emitter or sensor performance. Mass spectra revealed H₂SO₄ fragmentation and thermally induced decomposition up to 425 K. Spectral variations with filament current and electron energy highlight thermal and electron-induced dissociation dynamics. Operational modes include high-resolution scans and selective ion ejection (e.g., CO₂⁺, N₂⁺) to enhance the detection of PH₃⁺, H₂S⁺, and daughter ions. The compact QIT-MS platform is validated for future missions targeting corrosive atmospheres, enabling in situ astrobiological investigations through the detection of biosignature gasses such as phosphine and hydrogen sulfide. Full article

In this study, new monolithic poly(9-anthracenylmethyl methacrylate-co-trimethylolpropane trimethacrylate (TRIM) columns, referred as ANM monoliths were prepared, for the first time, and were used for the separation media for biomolecules and proteomics analysis by nano-liquid chromatography (nano-LC). Monolithic columns were prepared by in situ polymerization of 9-anthracenylmethyl methacrylate (ANM) and trimethylolpropane trimethacrylate (TRIM) in a fused silica capillary column of 100 µm ID. Polymerization solution was optimized in relation to monomer and porogenic solvent. Scanning electron microscopy (SEM) and chromatographic analyses were performed for the characterization studies of ANM monoliths. The ANM monolith produced more than 46.220 plates/m, and the chromatographic evaluation of the optimized ANM monolith was carried out using homologous alkylbenzenes (ABs) and polyaromatic hydrocarbons (PAHs), allowing both strong hydrophobic and π-π interactions. Run-to-run and column-to-column reproducibility values were found as <2.91% and 2.9–3.2%, respectively. The final monolith was used for biomolecule separation, including both three dipeptides, including Alanine-Tyrosine (Ala-Tyr), Glycine-Phenylalanine (Gly-Phe), and L-carnosine and five standard proteins, including ribonuclease A (RNase A), α-chymotrypsinogen (α-chym), lysozyme (Lys), cytochrome C (Cyt C), and myoglobin (Mb) in order to evaluate its potential. Both peptides and proteins were baseline separated using the developed ANM monolith in nano-LC. The ANM monolith was then applied to the protein and peptide profiling of MCF-7 cell line, which allowed a high-resolution analysis of peptides, providing a high peak capacity. Full article

The present work describes, for the first time, an eco-friendly capillary zone electrophoresis (CZE) methodology for determining apixaban (APX), an oral anticoagulant. Separation was carried out using a fused silica capillary with an applied voltage of 20 kV and hydrodynamic injection for 5 s at 50 mbar. The electrolyte system consisted of 50 mM sodium borate at pH 8.0. The method was validated as recommended by ICH, establishing selectivity, linearity, precision, accuracy, and robustness. The analytical procedure was linear in the range of 10–125 µg mL⁻¹ (r = 0.999). The limits of detection and quantification were determined to be 1.77 µg mL⁻¹ and 5.37 µg mL⁻¹, respectively. Precision was evaluated by relative standard deviation (RSD), with an intra-day RSD (n = 6) of 0.96% and an inter-day RSD (n = 18) of 4.42%. The average recovery rates for the pharmaceutical samples were excellent, ranging from 98.03% to 101.01%, with an RSD of 1.51%. Moreover, the green profile of the method was evaluated using the National Environmental Methods Index (NEMI), Analytical Eco-Scale, Green Analytical Procedure Index (GAPI), and Analytical GREEnness Metric (AGREE) assessment tools. The results suggest that the CZE method aligns with the principles of green chemistry, offering a greener alternative for the routine analysis of APX quality control. Also, the method presents a low-cost analysis, using fewer organic solvents and minimizing waste generation compared to techniques commonly used in routine analysis. Full article

Coal dust particles adhering to a camera lens reduce its light transmittance, which deteriorates the performance of the camera and may lead to serious problems with mining equipment that requires visual ability. Aiming at improving coal dust removal and cleaning technologies, the adhesion behavior of coal dust with fused silica is studied here. Experiments were conducted from microscopic and statistical points of view. The adhesion force between a single coal dust particle and fused silica is tested using atomic force microscopy (AFM), and the number and size distribution of large amounts of coal dust particles on fused silica are tested using a home-made adhesion experimental platform and image processing method. The results show that the adhesion force increases at high relative humidity (RH); it is dominated by van der Waals forces at low RH and capillary forces at high RH. The fused silica glass surface is predominantly covered by small-sized coal dust particles, and the total number of particles as well as the proportion of large-sized particles increases with RH. The theoretical values of van der Waals and capillary forces are significantly larger than the experimental values, owing to the irregular shape and roughness of the surface of the coal dust. Full article

In this study, we established a novel capillary electrophoresis method for monitoring the concentration of doripenem in human plasma. As a time-dependent antibiotic, doripenem maximizes its antibacterial effects and minimizes the potential for antibiotic resistance through careful therapeutic drug monitoring. Two online preconcentration techniques, field-enhanced sample stacking (FESS) and sweeping, were coupled to enhance the detection sensitivity. Briefly, an uncoated fused silica capillary (40 cm × 50 μm i.d) was rinsed with a high conductivity buffer (HCB) composed of 150 mM phosphate buffer (NaH₂PO₄, pH 2.5) and 20% methanol. A large sample plug prepared in a low-conductivity phosphate buffer (50 mM NaH₂PO₄, pH 2.5) was then hydrodynamically injected (5 psi, 80 s) into the capillary. Under an applied voltage of −30 kV, the analyte was accumulated at the FESS boundary and swept by the negatively charged micelles toward the UV detector. Plasma samples were pretreated by solid-phase extraction (SPE) to eliminate endogenous interferences. The validation results demonstrated a high coefficient of determination (r² > 0.9995) for the regression curve with impressive precision and accuracy: relative standard deviation (RSD) <5.86% and relative error <4.63%. The limit of detection (LOD, S/N = 3) for doripenem was determined to be 0.4 μg/mL. Compared to the conventional micellar electrokinetic chromatography method, our developed method achieved a sensitivity enhancement of up to 488-fold for doripenem. Furthermore, the newly developed method successfully quantified doripenem concentrations in plasma samples obtained from patients accepting doripenem regimens, proving its application potential in the clinical realm. Full article

Understanding the solubility of CO₂ is critical for implementing CO₂-enhanced oil recovery (CO₂-EOR). In this work, the solubility of CO₂ in n-decane in a temperature range between 303.15 K and 353.15 K and pressures up to 15 MPa was measured using a fused silica capillary cell with in situ Raman spectroscopy. A semi-empirical CO₂ solubility prediction model was obtained according to the experimental results. In order to improve the solubility of CO₂ in n-decane, the solubility of CO₂ in n-decane and co-solvent n-hexane (3% wt) mixture was also comparatively investigated. The results indicated that the solubility of CO₂ in n-decane was 1.6355~64.0084 mol/kg. The data from the prediction model were in good agreement with the experimental data, and the mean relative deviation was 3.65%, indicating that the prediction model could be used to predict the solubility of CO₂ in n-decane under different conditions. The solubility of CO₂ in n-decane + n-hexane system ranged from 1.0127 mol/kg to 65.7286 mol/kg. It was found that, under low-pressure conditions, the addition of co-solvent n-hexane did not enhance the solubility of CO₂, while it had a certain enhancement effect on the dissolution of CO₂ under high-pressure conditions. As the temperature increased from 303.15 K to 353.15 K, the enhancement efficiency of the solubility of CO₂ also increased from 1.34~2.05% to 8.17~9.82%, and the average enhancement efficiency increased from 1.74% to 9.00%. This study provides more CO₂ solubility data for CO₂-EOR. Full article

Temperature is a crucial factor for the safe operation of lithium-ion batteries. During operation, the internal temperature rises above the external temperature due to poor inner thermal conductivity. Various sensors have been proposed to detect the internal temperature, including fiber Bragg grating sensors. However, to the authors’ knowledge, there is no detailed description of the encapsulation of the fiber Bragg grating sensor in the literature to shield it from strain. In this study, different encapsulation methods for strain compensation were compared to find the encapsulation material most compatible with the electrolyte. For this, we stored the proposed sensors with different encapsulation methods in ethylene carbonate:ethyl methyl carbonate (EC:EMC) 3:7 with LiPF₆ (lithium hexafluorophosphate) electrolyte and applied temperature changes. After evaluating the sensor encapsulation methods in terms of handling, diameter, uncertainty, usability, and hysteresis behavior, the most suitable sensor encapsulation was found to be a fused silica capillary with polyimide coating. Full article

An ultra-fast method for the simultaneous determination of heavy metals in Passiflora incarnata tea by capillary electrophoresis (CE) using a short-end injection combined with multivariate analysis was proposed. Separation was conducted by hydrodynamic injection (5 s at 0.5 psi) using the short-end injection procedure in a fused uncoated silica capillary (50 cm total length, 10.2 cm effective length, 50 µm i.d.) with separation time less than 2 min. An indirect UV detection at 214 nm was employed by using imidazole as a chromophore. The buffer used was 6 mmol/L hydroxybutyric acid (HIBA). The optimum conditions by full factorial with a central point were achieved by 18-crown-6 concentration (23.3 mmol L⁻¹), voltage (+11.4 kV), methanol concentration (3.8%), and temperature (20 °C). The method showed good linearity (R² > 0.998) for both Cd and Pb, inter-day precision of less than 14.49%, and an adequate limit of quantification only for Cd (LOQ < 0.5 µg mL⁻¹ for Cd) based on the US Pharmacopeial Convention limit requirements for elemental impurities. After method validation, the method was applied to Passiflora incarnata tea samples from a local market. Furthermore, the developed method showed great potential for the determination of metals in other samples with proper sample preparation procedures. Full article

Capillary forces are shown to be extremely effective for micro-assembly and pick-and-place processes, especially for their ability to self-align the handled objects. However, in today’s machines, micro-objects are submitted to high loads, such as compressions for the electrical testing of the micro-components, or inertial forces coming from the high accelerations of the machines. There, capillary grippers may show some limits. These issues, as well as the difficulty to perform precise visual inspections (due to the tilt of the handled micro-object that can occur after a perturbation, such as the displacement of the gripper), can all be solved by temporarily removing the liquid meniscus. Therefore, we present a novel volume-tuning capillary gripper that provides a solution to these limitations without adding additional significant complexities or changes to the existing pick-and-place machines. A multi-scale prototype was dimensioned and produced by using fast prototyping methods, such as a femtosecond laser-assisted chemical etching process for fused silica. Models bringing a deeper understanding of the subsystems are presented. The proof of concept was extensively tested. Its picking capabilities and enhancements of the handling capabilities during horizontal motions, as well as the repeatability of the tuning of the volume of liquid, are presented. Full article

This article presents the first successful application of a capillary electrophoresis-microscale thermophoresis tandem technique (CE-MST) for determining the values of equilibrium constant, realized by connecting online the CE and MST instruments using a fused-silica capillary. The acid-base dissociation of fluorescein isothiocyanate, expressed by the acidity constant value (pK_a), was used as a model. The measurement procedure consisted of introducing a mixture containing the analyte and a deliberately added interferent into the CE capillary, electrophoretic separation of the analyte from the interferent, the detection of the analyte with a CE-integrated detector, detection with a MST detector, and then stopping the flow temporarily by turning off the voltage source to conduct the thermophoretic measurement. The analysis of migration times, peak areas and MST responses obtained concurrently for the same sample allowed us to determine the pK_a value using three independent methods integrated within one instrumentation. The analyte was effectively separated from the interferent, and the acidity values turned out to be consistent with each other. An attempt was also made to replace the standard commercial CE instrument with a home-made portable CE setup. As a result, the similar pK_a value was obtained, at the same time proving the possibility of increasing cost efficiency and reducing energy consumption. Overall, the CE-MST technique has a number of limitations, but its unique analytical capabilities may be beneficial for some applications, especially when sample separation is needed prior to the thermophoretic measurement. Full article

A capillary electrophoresis method was developed to detect and measure hydroxychloroquine (HCQ) and its active metabolite desethyl hydroxychloroquine (DHCQ) in whole blood in patients with rheumatoid arthritis. The best separation in terms of peak area reproducibility, migration time, peak shape, and resolution of adjacent peaks was obtained in a 60 cm, 75 µm i.d. uncoated fused-silica capillary using a background electrolyte mixture of an aqueous 55 mmol/L TRIS solution brought to pH 2.6 with phosphoric acid and methanol (85:15) and a voltage and a temperature of separation of 20 kV and 30 °C, respectively. Analytes were separated in less than 12 min, with excellent linearity (R² ≥ 0.999) in the concentration range of 0.5–8 µmol/L. The recovery of analytes spiked in whole blood was 99–101% for HCQ and 98–99% for DHCQ. Analysis of five samples from patients with rheumatoid arthritis receiving HCQ 400 mg daily yielded mean steady-state concentrations of 2.27 ± 1.61 and 1.54 ± 0.55 μmol/L for HCQ and DHCQ, respectively, with a HCQ to DHCQ ratio of 1.40 ± 0.77. Full article

We report an experimental study on the gain of the Raman signal of aqueous mixtures and liquid water when confined in aerogel-lined capillaries of various lengths of up to 20 cm and various internal diameters between 530 and 1000 µm. The lining was made of hydrophobised silica aerogel, and the carrier capillary body consisted of fused silica or borosilicate glass. Compared to the Raman signal detected from bulk liquid water with the same Raman probe, a Raman signal 27 times as large was detected when the liquid water was confined in a 20 cm-long capillary with an internal diameter of 700 µm. In comparison with silver-lined capillaries of the same length and same internal diameter, the aerogel-lined capillaries featured a superior Raman signal gain and a longer gain stability when exposed to mixtures of water, sugar, ethanol and acetic acid. Full article

The gas chromatography–mass spectrometry (GC-MS) approach is established for the simultaneous determination of fenchone (FCO) and trans-anethole (TOH) in the essential oils and methanolic extracts of fennel (Foeniculum vulgare Mill.) fruits obtained from India (IND), Pakistan (PAK), and Saudi Arabia (SA). The simultaneous determination of FCO and TOH was performed via Agilent 190914S HP–5MS fused-silica capillary column (30 m × 250 µm ID, 0.25 µm film thickness). The proposed GC-MS approach was linear in the range of 0.10–50 µg/g for FCO and TOH. FCO’s detection (LOD) and quantification (LOQ) limits were calculated to be 0.04 and 0.12 µg/g, respectively. The LOD and LOQ values for TOH, on the other hand, were calculated to be 0.05 and 0.15 µg/g, respectively. In addition, the proposed GC-MS approach was accurate and precise for the simultaneous determination of FCO and TOH. The amount of FCO in essential oils of F. vulgare was computed as 0.021, 0.034, and 0.029 mg/g in the samples obtained from IND, PAK, and SA, respectively. The amount of TOH in the essential oils of F. vulgare was computed as 7.40, 14.8, and 10.2 mg/g in the samples obtained from IND, PAK, and SA, respectively. However, the amount of FCO in the methanolic extract of F. vulgare was estimated as 0.031, 0.021, and 0.057 mg/g in the samples obtained from IND, PAK, and SA, respectively. On the other hand, the amount of TOH in the methanolic extract of F. vulgare was estimated as 0.440, 0.498, and 1.74 mg/g in the samples obtained from IND, PAK, and SA, respectively. These findings suggested that the proposed GC-MS approach might be used to simultaneously determine the FCO and TOH in a variety of essential oils and plant extracts. Full article