Metals, metallic compounds, and, recently, metallic nanoparticles appear in textiles due to impurities from raw materials, contamination during the manufacturing process, and/or their deliberate addition. However, the presence of lead, cadmium, chromium (VI), arsenic, mercury, and dioctyltin in textile products is regulated in Europe (Regulation 1907/2006). Metal determination in fabrics was performed by inductively coupled plasma-mass spectrometry (ICP-MS) after microwave-assisted acid digestion. The ICP-MS procedure has been successfully validated; relative standard deviations were up to 3% and analytical recoveries were within the 90–107% range. The developed method was applied to several commercial textiles, and special attention has been focused on textiles with nanofinishing (fabrics prepared with metallic nanoparticles for providing certain functionalities). Arsenic content (in textile T4) and lead content (in subsamples T1-1, T1-2, and T3-3) were found to exceed the maximum limits established by the European Regulation 1907/2006. Although impregnation of yarns with mercury compounds is not allowed, mercury was quantified in fabrics T1-2, T5, and T6. Further speciation studies for determining hexavalent chromium species in sample T9 are necessary (hexavalent chromium is the only species of chromium regulated). Some textile products commercialised in Europe included in this study do not comply with European regulation 1907/2006.
The accumulation of antimicrobial residues in edible animal products and aquaculture products could pose health concerns to unsuspecting consumers. Hence, this study aimed to develop a validated method for simultaneous quantification of chloramphenicol (CAP), thiamphenicol (TAP), florfenicol (FF), and florfenicol amine (FFA) in beef, pork, chicken, shrimp, eel, and flatfish using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction method coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS). Primary-secondary amine (PSA) and MgSO4 were used for sample purification. The analytes were separated on a reversed-phase analytical column. The coefficients of determination for the linear matrix-matched calibration curves were ≥0.9941. Recovery rates ranged between 64.26 and 116.51% for the four analytes with relative standard deviations (RSDs) ≤ 18.05%. The calculated limits of detection (LODs) and limits of quantification (LOQs) were 0.005–3.1 and 0.02–10.4 μg/kg, respectively. The developed method was successfully applied for monitoring samples obtained from local markets in Seoul, Republic of Korea. The target residues were not detected in any tested matrix. The designed method was versatile, sensitive, and proved suitable for quantifying residues in animal-derived products.
Considering the significance of its demand around the world, the accurate determination of fish freshness with a simple and rapid procedure has become an interesting issue for the fishing industry. Hence, we aimed to fabricate a new optical pH sensor based on a polyelectrolyte (PEC) membrane of pectin–chitosan and the active material chromoionophore ETH 5294. A trial-and-error investigation of the polymer compositions revealed that the optimum ratio of pectin to chitosan was 3:7. With an optimum wavelength region (λ) at 610 nm, the constructed sensor was capable of stable responses after 5 min exposure to phosphate-buffered solution. Furthermore, the obtained sensor achieved optimum sensitivity when the PBS concentration was 0.1 M, while the relative standard deviation values ranged from 2.07 to 2.34%, suggesting good reproducibility. Further investigation revealed that the sensor experienced decreased absorbance of 16.67–18.68% after 25 days of storage. Employing the optimum conditions stated previously, the sensor was tested to monitor fish freshness in samples that were stored at 4 °C and ambient temperature. The results suggested that the newly fabricated optical sensor could measure pH changes on fish skin after 25 h storage at room temperature (pH 6.37, 8.91 and 11.02, respectively) and 4 °C (pH 6.8, 7.31 and 7.92, respectively).
Purpose: To develop a reversed phase high performance liquid chromatography (HPLC) method for the determination of dehydroepiandrosterone (DHEA) in dietary supplements.
Methods: A reversed-phase high performance liquid chromatography (HPLC) method was developed for the determination of DHEA in dietary supplements. An isocratic system consisting of methanol and water (70:30 v/v) was run at a flow rate of 1 mL/min on a C18 HPLC column to achieve the separation. The method was validated with regard to linearity, intra-day and inter-day precision, and limits of both detection and quantification.
Results: The method achieved a retention time of 10.8 min, a resolution of 4.12, a detection limit (LOD) of 50 ng/μL, a quantification limit (LOQ) of 166.7 ng/μL and a label claim of 108.6 % with a relative standard deviation (RSD) of 0.38 % over a range of 0.0625 – 0.50 mg/mL with a correlation coefficient of 0.9997.
Conclusion: The method is simple, cost effective, time-saving and reliable for determining DHEA when compared to other reported methods in literature. Thus, it will be of benefit to manufacturers of this dietary supplement to adopt the method for quantitative laboratory analysis.
Short-chain fatty acids (SCFA, C2-C5) in milk and serum are derived from rumen bacterial fermentation and, thus, have the potential to be used as biomarkers for the health status of dairy cows. Currently, there is no comprehensive and validated method that can be used to analyse all SCFAs in both bovine serum and milk. This paper reports an optimised protocol, combining 3-nitrophenylhydrazine (3-NPH) derivatisation and liquid chromatography-mass spectrometry (LC-MS) analysis for quantification of SCFA and β-hydroxybutyric acid (BHBA) in both bovine milk and bovine serum. This method is sensitive (limit of detection (LOD) ≤ 0.1 µmol/L of bovine milk and serum), accurate (recovery 84–115% for most analytes) and reproducible (relative standard deviation (RSD) for repeated analyses below 7% for most measurements) with a short sample preparation step. The application of this method to samples collected from a small cohort of animals allowed us to reveal a large variation in SCFA concentration between serum and milk and across different animals as well as the strong correlation of some SCFAs between milk and serum samples.
The application of cardiovascular magnetic resonance angiography (CMRA) for the assessment of thoracic aortic disease is often associated with prolonged and unpredictable acquisition times and residual motion artefacts. To overcome these limitations, we have integrated undersampled acquisition with image-based navigators and inline non-rigid motion correction to enable a free-breathing, contrast-free Cartesian CMRA framework for the visualization of the thoracic aorta in a short and predictable scan of 3 min.
35 patients with thoracic aortic disease (36 ± 13y, 14 female) were prospectively enrolled in this single-center study. The proposed 3D T2-prepared balanced steady state free precession (bSSFP) sequence with image-based navigator (iNAV) was compared to the clinical 3D T2-prepared bSSFP with diaphragmatic-navigator gating (dNAV), in terms of image acquisition time. Three cardiologists blinded to iNAV vs. dNAV acquisition, recorded image quality scores across four aortic segments and their overall diagnostic confidence. Contrast ratio (CR) and relative standard deviation (RSD) of signal intensity (SI) in the corresponding segments were estimated. Co-axial aortic dimensions in six landmarks were measured by two readers to evaluate the agreement between the two methods, along with inter-observer and intra-observer agreement. Kolmogorov–Smirnov test, Mann–Whitney U (MWU), Bland–Altman analysis (BAA), intraclass correlation coefficient (ICC) were used for statistical analysis.
The scan time for the iNAV-based approach was significantly shorter (3.1 ± 0.5 min vs. 12.0 ± 3.0 min for dNAV, P = 0.005). Reconstruction was performed inline in 3.0 ± 0.3 min. Diagnostic confidence was similar for the proposed iNAV versus dNAV for all three reviewers (Reviewer 1: 3.9 ± 0.3 vs. 3.8 ± 0.4, P = 0.7; Reviewer 2: 4.0 ± 0.2 vs. 3.9 ± 0.3, P = 0.4; Reviewer 3: 3.8 ± 0.4 vs. 3.7 ± 0.6, P = 0.3). The proposed method yielded higher image quality scores in terms of artefacts from respiratory motion, and non-diagnostic images due to signal inhomogeneity were observed less frequently. While the dNAV approach outperformed the iNAV method in the CR assessment, the iNAV sequence showed improved signal homogeneity along the entire thoracic aorta [RSD SI 5.1 (4.4, 6.5) vs. 6.5 (4.6, 8.6), P = 0.002]. BAA showed a mean difference of < 0.05 cm across the 6 landmarks between the two datasets. ICC showed excellent inter- and intra-observer reproducibility.
Thoracic aortic iNAV-based CMRA with fast acquisition (~ 3 min) and inline reconstruction (3 min) is proposed, resulting in high diagnostic confidence and reproducible aortic measurements.
Regulatory bodies have started to recognise the value of in vitro screening and metabolomics as two types of new approach methodologies (NAMs) for chemical risk assessments, yet few high-throughput in vitro toxicometabolomics studies have been reported. A significant challenge is to implement automated sample preparation of the low biomass samples typically used for in vitro screening. Building on previous work, we have developed, characterised and demonstrated an automated sample preparation and analysis workflow for in vitro metabolomics of HepaRG cells in 96-well microplates using a Biomek i7 Hybrid Workstation (Beckman Coulter) and Orbitrap Elite (Thermo Scientific) high-resolution nanoelectrospray direct infusion mass spectrometry (nESI-DIMS), across polar metabolites and lipids. The experimental conditions evaluated included the day of metabolite extraction, order of extraction of samples in 96-well microplates, position of the 96-well microplate on the instrument’s deck and well location within a microplate. By using the median relative standard deviation (mRSD (%)) of spectral features, we have demonstrated good repeatability of the workflow (final mRSD < 30%) with a low percentage of features outside the threshold applied for statistical analysis. To improve the quality of the automated workflow further, small method modifications were made and then applied to a large cohort study (4860 sample infusions across three nESI-DIMS assays), which confirmed very high repeatability of the whole workflow from cell culturing to metabolite measurements, whilst providing a significant improvement in sample throughput. It is envisioned that the automated in vitro metabolomics workflow will help to advance the application of metabolomics (as a part of NAMs) in chemical safety, primarily as an approach for high throughput screening and prioritisation.
In recent years, there has been an increased uptake for surface functionalization through the means of laser surface processing. The constant evolution of low-cost, easily automatable, and highly repeatable nanosecond fibre lasers has significantly aided this. In this paper, we present a laser surface-texturing technique to manufacture a surface with a tailored high static friction coefficient for application within driveshafts of large marine engines. The requirement in this application is not only a high friction coefficient, but a friction coefficient kept within a narrow range. This is obtained by using nanosecond-pulsed fibre lasers to generate a hexagonal pattern of craters on the surface. To provide a suitable friction coefficient, after laser processing the surface was hardened using a chromium-based hardening process, so that the textured surface would embed into its counterpart when the normal force was applied in the engine application. Using the combination of the laser texturing and surface hardening, it is possible to tailor the surface properties to achieve a static friction coefficient of ≥0.7 with ~3–4% relative standard deviation. The laser-textured and hardened parts were installed in driveshafts for ship testing. After successfully performing in 1500 h of operation, it is planned to adopt the solution into production.
Purpose: A simple, specific, precise, and accurate reversed phase liquid chromatographic (RP-LC) method has been developed for the determination of Escitalopram in tablet dosage form.
Methods: The chromatographic separation was achieved on a LiChrosorb C18, 250 mm x 4.6 mm, 5 μm column at a detector wavelength of 270 nm and a flow rate of 1.0 ml/min. The mobile phase was composed of methanol, acetonitrile (70:30 v/v). The retention time of Escitalopram was 5.49 min. The method was validated for the parameters like specificity, linearity, precision, accuracy, limit of quantitation and limit of detection.
Results: The method was found to be specific as no other peaks of impurities and excipients were observed. The square of correlation coefficient (R2) was 0.9999 while relative standard deviations were found to be <2.0%.
Conclusion: The proposed RP-LC method can be applied for the routine analysis of commercially available formulations of Escitalopram.
A sensitive, selective, and stable sensor for the simultaneous determination of Cd2+ and Pb2+ in aqueous solution has been developed based on the carbon dots (CDs) and Nafion-modified bismuth film glassy carbon electrode (GCE). High graphitized CDs prepared by the sulfuric acid-assisted hydrothermal synthesis were directly electrodeposited on the GCE surface by cyclic voltammetry. Compared with the conventional bismuth film electrodes, CDs greatly improved the electrochemical activity of the bismuth film electrode for the detection of Cd2+ and Pb2+. After decorating CDs, the surface impedance of the GCE was decreased from 10.9 kΩ to 4.84 kΩ. Meanwhile, the corresponding response currents of the Bi/GCE were increased over 7.4 and 2.4 times for Cd2+ and Pb2+ with a wide linear range of 0.05-0.50 mg/L, respectively. High sensitivity was obtained with the detection limits of 3.1 μg L-1 (Cd2+) and 2.3 μg L-1 (Pb2+). Moreover, good stability was obtained for the simultaneous determination of Cd2+ and Pb2+ in the practical underground water with the relative standard deviations less than 10%. The results indicated that the CDs-modified bismuth film electrode could potentially be applied to detect the heavy metal ion concentrations in practical environment.