Mass Scanning Research Articles

Paralytic Shellfish Poisoning (PSP) Toxins in Bivalve Molluscs from Southern Italy Analysed by Liquid Chromatography Coupled with High-Resolution Mass Spectrometry (UHPLC-HRMS/MS).

A new method for simultaneous determination by liquid chromatography coupled with high resolution mass spectrometry (UHPLC-HRMS/MS) of 14 paralytic shellfish poisoning toxins (PSP), that is, Saxitoxin, Neosaxitoxin, Gonyautoxins and their respective variants, in bivalve molluscs, is herein described. The samples were extracted by acetic acid solution, then analysed by UHPLC coupled with a Q-Exactive Orbitrap Plus high resolution mass spectrometer, by electrospray ionization mode (ESI) with no further clean up step. The analysis was carried out by monitoring both the exact mass of the molecular precursor ion of each compound (in mass scan mode, resolution at 70,000 FWHM) and its respective fragmentation patterns (two product ions) with mass accuracy greater than 5 ppm. The analytical performance of the method was evaluated calculating trueness, as mean recoveries of each biotoxin, between 77.8% and 111.9%, a within-laboratory reproducibility (RSDR) between 3.6% and 12.2%, the specificity, the linearity of detector response, and the ruggedness for slight changes The results of the validation study demonstrate this method fits for the purposes of the official control of PSP toxins in molluscs. The results of two years of monitoring in local mussel farms are also reported, showing that no significant concerns for food safety in the monitored productions.

Effect of thermal annealing on the luminescent and structural properties of the SiOxCy thin films by organic catalytic chemical vapor deposition

Photoluminescent silicon oxycarbide (SiOxCy) thin films were deposited on n-type (100) silicon substrates using the organic catalytic chemical vapor deposition (O-Cat-CVD) technique employing tetra-ethyl orthosilicate (TEOS) as an organic-based precursor. These films were annealed at a temperature of 500, 800 and 1000°C for 30 minutes in a nitrogen (N2) environment. The as-deposited and annealed SiOxCy films were analyzed using optical and structural characterizations, such as photoluminescence (PL), Fourier transform infrared (FTIR), X-ray photoelectron spectroscopy (XPS), Secondary ion mass spectrometry (SIMS) and scanning electron microscopy (SEM). The PL spectrum of the as-deposited film showed emission in the blue-green region, while the annealed SiOxCy films showed strong emission from blue to near-infrared. The PL in all the films was attributed to different structural defects related to oxygen and carbon that act as radiative centers in the SiOxCy network. The annealed films showed an increase in the emission intensity, where the annealed film at 800°C displayed the highest emission intensity. This is related to an increase in the amount of radiative defects in the films due to structural and compositional changes after the thermal annealing (TA). XPS and SIMS measurements showed an oxygen incorporation with the TA, increasing from 54.59 at. % to 63.5 at. % for the as-deposited and annealed at 1000°C films, respectively. FTIR spectra showed an increase in the Si-O-C and Si-O-Si bonds and the hydrogen and other radicals desorption. These results support the creation of radiative centers due to structural changes in the films after the thermal annealing.

High Specificity and Sensitivity Method for Quantitation of Anthocyanins by Precursor Ion Scan Using Liquid Chromatography‐Tandem Mass Spectrometry Technique

ABSTRACTAnthocyanins, primarily found in flowers, vegetables, and fruits, play a critical role in human and plant health. These polyphenolic pigments are predominantly found in plants in the form of glucosides linked to one or more sugar units and exhibit a broad range of structural diversity. This creates a complex spectrum of anthocyanins making it challenging to perform its absolute quantification in different plant matrices due to the lack of availability of all reference standards. More commonly today, anthocyanins are quantified by spectrophotometric methods, which is non‐specific quantification due to a lack of information on the anthocyanin classes present. In this study, a systematic approach has been proposed to address this challenge, utilizing liquid chromatography‐tandem mass spectrometry using precursor ion scan mode for high‐specificity identification and subsequent quantification of the anthocyanin classes. A method was developed for six anthocyanin classes and it was used to quantify anthocyanins in black carrot extract. The initial scan was conducted for all anthocyanin classes, followed by the quantification of the anthocyanin classes detected using the reference standard specific to that class. This approach has demonstrated that precursor ion scan mass spectrometry can serve as a valuable tool for the rapid identification and specific quantification of anthocyanin classes in plants.

Hygrothermal Effect on Glass Fiber Reinforced Plastic (GFRP) Under Seawater Immersion

Glass Fiber Reinforced Plastic (GFRP) is extensively used for corrugated roofing sheets and gutters in Indonesia, especially in corrosive environments, due to its superior corrosion resistancecompared to steel. Despite its widespread application in coastal areas, limited studies have examined the durability of GFRP when exposed to seawater and heat. This research investigates the influence of hygrothermal conditions on the physical and mechanical properties of GFRP. Samples were immersed in seawater at temperatures of 30°C, 40°C, and 60°C for 3 and 6 months. Results show that hygrothermal exposure leads to degradation in physical but notmechanical properties. Physical properties were evaluated using mass gain measurements, hardness testing, and Scanning Electron Microscopy (SEM), while mechanical properties were assessed via tensile testing.The result shown all specimen have increased mass up to 3,8% and decrease in hardnessup to 56%. SEM also shown several dark spot which indicatevoid. SEM analysis revealed the presence of dark spots, indicating void formation. These findings underscore the vulnerability of GFRP to hygrothermal conditions, raising concerns about its long-term durability in coastal applications.

B-159 Fast Cleanup for 19 Steroid Analytes in Serum Using Supported Liquid Extraction (SLE)

Abstract Background Liquid chromatography-tandem mass spectrometry (LC-MS/MS) is a powerful tool that holds promise in designing the future of steroid analysis in the clinical laboratory. It is already widely used in steroid analysis in endocrinology and is being utilized increasingly in newer applications for individual steroids and panels relevant in clinical research. LC-MS/MS is gaining user base owing to greater sensitivity and specificity and gradually even replacing some of the legacy test methods. Improved sample preparation, modern chromatography methods, and sensitive, faster scanning mass spectrometers have all played a role in improving LC-MS/MS. Steroid analysis for clinical research can require very low limits of detection which demand high recoveries and very clean extracted samples. Supported Liquid Extraction (SLE) can provide very clean extracted samples with less method development and a streamlined workflow compared to solid phase extraction (SPE). Laboratories desire high-throughput methods which consolidate analytes into one panel with fast chromatographic run times. Chromatographic separation of steroid isomers with the same m/z is necessary for accurate quantitation by LCMS/MS. Meeting these criteria can be challenging in a single LC-MS/MS method. Methods Each 200 µL serum sample was pretreated with 200 µL of pH 6 Ammonium Acetate buffer (aq) before being loaded onto a Novum™ PRO SLE, MAX 96-well plate, following the standard SLE protocol. Samples were eluted using 2 × 900 µL of Dichloromethane or Ethyl Acetate. After evaporation of the elution solvent, samples were reconstituted in 100 µL of 0.5 mM Ammonium Fluoride / Methanol (60:40, v/v). A Kinetex™ 2.6 μm C18, 50 x 3.0 mm column using a gradient of 0.5 mM Ammonium Fluoride (aq) and Methanol on an Agilent® 1290 Infinity UHPLC and SCIEX® 7500 Triple Quad™ were used for quantitation. Results Here, we present an effective sample extraction method and LC-MS/MS analysis method for the quantitation of a 19-analyte steroid panel from serum. The Kinetex 2.6 μm C18 column provided a fast 8-minute chromatographic separation and good selectivity for steroid analytes in both positive ion mode and negative ion mode. Calibration curves with a linear fit and 1/x weighting, showed good linearity with R2 of >0.99 for all analytes except 17-OH-Pregnenolone and DHEAS when using Dichloromethane as the elution solvent, and R2 of >0.980 for all analytes when using Ethyl Acetate as the elution the solvent. Accuracy of samples using Dichloromethane as the elution solvent were 80-112 %, except for 17-OH-Pregnenolone and DHEAS. Accuracy of all samples using the Ethyl Acetate elution solvent were 91-118 %. Conclusions The-96 well plate extraction method was robust, reproducible, and can be automated. SLE using Novum Pro MAX combined with a fast LC method provides a simple, rapid, high-throughput workflow for identification and quantitation of 19 steroids from serum.

Study of the mechanisms of change in hydride phases in zirconium beryllide during its linear heating

Abstract Beryllides have a number of unique properties that make them promising for use in various fields of industry and energy. Since some of the beryllides have the potential to dissolve large amounts of hydrogen (in some cases forming hydride phases), there is some interest in evaluating their possible applications in hydrogen technologies. This paper presents the results of studies of changes in the phase composition of the zirconium beryllide deuteride compound during its linear heating. The studies were carried out using a complex method including thermal gravimetrical analysis (TGA), differential scanning calorimetry (DSC) and mass spectrometry. Based on the results of the experiments, a number of parameters were obtained characterizing the transitions of deuteride from the phase of the Orthorhombic I mma crystal structure of deuteride ZrBe2D into the Orthorhombic C mcm crystal structure of deuteride ZrBe2D0.67, as well as the decomposition parameters of Orthorhombic C mcm crystal structure of ZrBe2D0.67. The energies of endothermic reactions of the corresponding transitions and decompositions of deuteride phases were estimated, and the activation energy of the interaction of water vapor with the surface of zirconium beryllide samples was also estimated.

Composition and micromorphological determination of blue honeysuckle fruit (Lonicera caerulea L.) cuticular wax and its effects on fruit post-harvest quality

The chemical composition and structure of the cuticular wax in blue honeysuckle fruit were investigated using gas chromatography–mass spectrometry (GC–MS) and scanning electron microscopy (SEM). The results revealed that the cuticular wax was dense and uniform, taking on a tubular form. A total of 158 wax components were identified, including alkanes, terpenes, ketones, alcohols, fatty acids, and esters. The wax was found to be particularly rich in alkanes. After storage, the wax content decreased, whereas an increase in 1-undecanol. The destruction or reduction of cuticular wax resulted in a more rapid decline in storage quality, loss of nutrients, and a decrease in antioxidant phytochemicals. Meanwhile, wax metabolizing enzyme activity and gene expression increased. This study presents a deeper understanding of blue honeysuckle fruit cuticular wax composition and aids to developing effective measures to delay its postharvest fruit quality deterioration.

The Surface Deterioration of Prefabricated Zirconia Crowns on Exposure to Acidulated Phosphate Fluoride Gel: An In Vitro Study.

Introduction Zirconia is a widely used restorative material in dentistry due to its superior aesthetic and mechanical properties. The oral cavity is a complex ecosystem with various components, which affect the teeth, as well as artificial restorative materials. Various personal and professional interventions carried out can severely affect the properties of restorative materials, thus altering the longevity of the prosthesis; 1.23% acidulated phosphate fluoride (APF) gel is one such professionally applied topical fluoride agent used to prevent caries. The interaction of this APF gel with highly aesthetic restorative material such as zirconia crowns is unknown. Objective The objective of this study is the evaluation of the surface deterioration of prefabricated zirconia crowns on exposure to deionised water and 1.23% acidulated phosphate fluoride (APF) gel with field emission scanning electron microscope (FE-SEM) and mass loss analysis. Material and method Sixty prefabricated paediatric zirconia crowns were taken, 10 samples were immersed in deionised water, 40 samples were immersed in 1.23% APF gel and 10 samples were used ascontrol. Surface morphology and mass loss analysis were carried out at time intervals of four minutes, 24 hours, 48 hours and 72 hours using FE-SEM and digital weighing machine. Results No visual change was observed in the samples immersed in deionised water at the time interval of 72 hours. There was a marked visual change in samples immersed in 1.23% APF gel at the time interval of four minutes to 72 hours; this change involved a loss of gloss to the appearance of chalkiness. FE-SEM analysis for the control group and samples immersed in deionised water showed a smooth, continuous, undisrupted top layer, while samples immersed in 1.23% APF gel showed changes ranging from surface etching, to pinhole porosities, to crack formation and disruption of the surface depending upon the exposure time. Conclusions On the immersion of zirconia crowns in an aqueous acidic medium of 1.23% APF gel, the crowns showed flaws, imperfectionsand uneven superficial layers. It has been observed that surface grains are disrupted and micropores have been formed. This degraded superficial surface when undergoes cyclic mechanical loading can accelerate the ageing phenomenon of zirconia. Mechanical forces along with a dynamic electrochemical environment can degrade the material properties of zirconia.

Peculiarities of rearing poultry by floor method on deep bedding

In poultry rearing on deep bedding systems, microorganisms that cause infectious diseases develop within the bedding. This study aimed to determine the physical properties and microbial accumulation capacity of different types of bedding. Methods used included thermo-programmed desorption mass spectrometry, microbiological methods, and scanning electron microscopy. The hygroscopic properties of straw bedding deteriorated by 269.90% from the seventh to the fortysecond day. In the experimental room, where a dry disinfectant was added to the straw bedding, the hygroscopic capacity was 86.70% at the end of the experiment, a difference of 183.2%. Wood shavings bedding, with the addition of disinfectant, exhibited a water absorption capacity 102.82% higher than the control on the forty-second day. Granulated bedding with disinfectant retained moisture 150.33% better compared to the control. At the end of the experiment, the pH of straw bedding was 8.13 in the control group compared to 7.56 in the treated group; for wood shavings was 7.95 versus 7.16; and for granule was 7.35 versus 6.35, due to the use of the disinfectant. At the conclusion of the experiment, granulated bedding exhibited the lowest pH compared to straw and wood shavings, affecting the growth and reproduction of microorganisms. Monitoring of microorganisms in the bedding revealed the presence of bacteria: Escherichia coli, Salmonella typhimurium, Salmonella pullorum, Clostridium perfringens, Staphylococcus aureus, Klebsiella pneumonia, Listeria monocytogenes, as well as microscopic fungi: Fusarium sporotrichioides, Aspergillus niger, and Eimeria oocysts. The use of disinfectant reduced bacterial contamination of straw bedding by 12.35-199.19%, fungal contamination by 633.91-1959.14%, and Eimeria by 676.50%. In the wood shavings bedding, bacterial contamination was reduced by 32.84-257.93%, fungal contamination by 487.08-1098.4%, and Eimeria by 570.21%. Granulated bedding showed reduced bacterial accumulation by 50.93-228.87%, fungal accumulation by 169.89-500.9%, and Eimeria by 301.56%. The practical significance of this study lies in the improved physical properties of poultry bedding and the reduction in bacterial, fungal, and Eimeria oocyst accumulation

Experimental Evaluation of Higher Order Stability Zones Using a Digitally Operated Quadrupole Mass Filter.

Recent improvements to the comparison-based method of digital waveform generation increased the reproducibility of the waveforms so that the higher-order Mathieu stability zones can be accessed reliably. Digitally driven quadrupole mass filters access these zones using a fixed AC voltage and rectangular waveforms that are defined by a duty cycle. In this context, the duty cycle is the fraction of the waveform period where the waveform remains in the high state. Because digitally driven quadrupoles navigate stability using a duty cycle, there is no need to apply a resolving DC offset between electrode pairs. Accessing the higher stability zones using a conventional resonantly tuned RF requires the use of thousands of AC and DC voltages making the mode of operation less accessible with these devices. Stability zones higher than (1,1) and (2,1) have theoretical resolving powers that are on the order 1,140 and 3,447 at fwhm which drives efforts to practically access these operational conditions. Accessing these zones digitally requires the use of extremely precise waveforms. In a previous effort, waveform generation produced waveforms to reliably access the (1,1) and (2,1) zones without impacting performance. However, recent work found more improvement was needed to reliably access neighboring higher stability zones. Derived from that work, it was determined that a waveform resolution of ∼10 ppm or less was needed to reliably access the (3,1) and (3,2) zones. The present work utilized digital waveforms that achieve this level of precision to experimentally access and characterize attributes of the (3,1) and (3,2) zones. This work dives into the investigation of different beam energies to overcome the destabilizing fringing fields, improve transmission, and their overall effect on the experimental resolving power and signal-to-noise. In addition, the AC voltage of the driving RF was varied to understand the effects on the initial ion beam energy that is needed to achieve balanced separation and how the overall signal-to-noise is affected. Lastly, an assessment was made on the effects of the temporal parameters of a digital mass scan on peak sensitivity, peak fidelity, and overall duration for a scan.

Enrichment of Phosphates, Lead, and Mixed Soil‐Organic Particles in INPs at the Southern Great Plains Site

AbstractIce nucleating particles (INPs) are rare particles that initiate primary ice formation, a critical step required for subsequent important cloud microphysical processes that ultimately govern cloud phase and cloud radiative properties. Laboratory studies have found that organic‐rich dusts, such as those found in soils, are more efficient INPs compared to mineral dust. However, the atmospheric relevance of these organic‐rich dusts are not well understood, particularly in regions with significant agricultural activity. The Agricultural Ice nuclei at the Southern Great Plains field campaign (AGINSGP) was conducted in rural Oklahoma to investigate how soil dusts contribute to INP populations in the Great Plains. We present chemical characterization of ambient and ice crystal residual particles from a single day of sampling, using single particle mass spectrometry (SPMS) and scanning microscopy. Ambient particles were primarily carbonaceous or secondary aerosol, while the fraction of dust particles was higher in the residual particles. We also observed an unusual particle type consisting of a carbonaceous core mixed with dust fragments on the surface, which was found in higher proportion in residuals. Dust particles measured during residual sampling contained greater proportions of phosphate (63 and 79) and lead (206Pb+). Strong sulfate signals were not seen in the residual dust particles measured by the SPMS, while nitrate was slightly depleted relative to ambient dust. This study shows that organic‐rich soils may be important contributors to the ambient INP population in agricultural regions.

The Reduction Reaction Behavior of Steelmaking Dusts with Lignin under Different Atmospheres.

This study investigated lignin as a reducing agent instead of fossil carbon for the reduction of zinc oxide and zinc ferrite contained in steelmaking dusts. Three types of dusts from different steelmaking processes were considered: ferrochrome converter (CRC), electric arc furnace stainless steel (EAFSS) and electric arc furnace carbon steel (EAFCS). Zinc is primarily found in zincite phases within CRC dust, while EAFSS and EAFCS dusts contain franklinite and zincite phases as Zn-bearing minerals. The proximate analysis of lignin showed that the fixed carbon content is 28.9%. Thermogravimetric (TG) analysis coupled with differential scanning calorimetry (DSC) and mass spectrometry (MS) was used to study the reduction behavior of different mixtures of lignin and steel dusts under inert and air atmospheres. Simultaneously, the minimum ratio of lignin out of three different proportions required to achieve a complete reduction of franklinite and zincite phases into metallic zinc was identified. The results indicated that a 1.1 stoichiometric amount of lignin is sufficient for the complete reduction of zinc-bearing minerals into metallic zinc. In conclusion, lignin can be used efficiently for processing steelmaking dusts.

Angiectatic Polyp-An Unusual Nasal Mass in a Young Adult.

Angiectatic nasal polyps (ANP) are rare pseudo-neoplastic lesions that might raise intriguing pathophysiological issues and present a significant diagnostic challenge. They are also referred to as inflammatory granuloma telangiectaticum, vascular granuloma, pseudo-angioma, and angiomatous/angiectatic polyp. However, the name angiectatic polyp refers to the fact that the lesion is not a true tumour and is clinically distinguished by ectatic vasculature, haemorrhage, and persistent proliferation. The most confusing aspect of this polyp is its clinical appearance, which resembles a juvenile nasal angiofibroma. Despite its typical imaging characteristics, this lesion is difficult to differentiate radiologically. Hence, histopathology is paramount for establishing diagnosis. We report a rare case of a young adult who presented with complaints of nasal block and epistaxis. Examination revealed a vascular nasal mass and CT scan demonstrated the lesion to be epicentred in right nasal cavity extending to multiple sinuses with adjacent bone erosion. Patient underwent endoscopic excision of the mass with JNA as the predominant differential and only following histopathological examination, the final diagnosis was confirmed.

Modeling of a linear ion trap with driving rectangular waveforms.

We consider the operation of a digital linear ion trap with resonant radial ejection. A sequence of rectangular voltage pulses with a dipole resonance signal is applied to the trap electrodes. The periodic waveform is piecewise constant, has zero mean, and is determined by an asymmetry parameter : one value is taken on interval and another on , where is the RF period. Ion mass scanning is performed by varying the asymmetry parameter and amplitude of the negative pulse part with time. The ion oscillation frequencies and acceptance of the linear trap are calculated. The dependence of the ion mass to charge ratio on the parameter is . The maximum value is about kDa for typical parameters of the linear trap: frequency 0.5 MHz, rod radius 4 mm, and negative pulse amplitude 1 kV. The dipolar excitation frequency is 0.125 MHz at which the LIT acceptance is maximal.

Utilizing a novel MRI technique to identify adverse muscle composition in end-stage liver disease: A pilot study

Introduction and ObjectivesSarcopenia is a common complication of end-stage liver disease (ESLD), but its exact relationship to myosteatosis and frailty remains unclear. In this pilot study, we tested the feasibility of a specialized MRI protocol and automated image analysis in patients with ESLD. Materials and MethodsIn a single-center prospective study, adult liver transplant candidates with ESLD underwent assessment of muscle composition between 3/2022 and 6/2022 using the AMRA® MAsS Scan. The primary outcome of interest was feasibility of the novel MRI technique in patients with ESLD. We also tested if thigh muscle composition correlated with validated measures of frailty and sarcopenia. ResultsEighteen subjects (71 % male, mean age 59 years) were enrolled. The most common etiologies of cirrhosis were alcohol-related liver disease (44 %) and non-alcohol-associated fatty liver disease (33 %), with a mean MELD-Na of 13 (± 4). The mean time needed to complete the MRI protocol was 14.9 min and only one patient could not complete it due to metal hardware in both knees. Forty-one percent of patients had adverse muscle composition (high thigh fat infiltration and low-fat free muscle volume) and these patients were more likely to have undergone a recent large volume paracentesis (43 % vs. 0 %, p < 0.02). The adverse muscle composition group performed significantly worse on the 6-minute walk test compared to the remainder of the cohort (379 vs 470 m, p < 0.01). ConclusionsThe AMRA® MAsS Scan is feasible to perform in patients with ESLD and can be used to quantify myosteatosis, a marker of muscle quality and potentially muscle functionality in ESLD.

The Influence of Freezing-thawing on the Properties of Sludge from Water Treatment Facilities and the Prospects for its Disposal

It has been shown that the freezing-thawing method allows a sharp increase in the water-yielding capacity of water treatment sludge (WTS sludge) and leads to an increase in the median particle size of the dispersed phase of sludge. The distribution of bound water types in WTP sludge was studied using thermogravimetry (TG), differential thermal thermogravimetry (DTG), differential scanning calorimetry (DSC) and mass spectrometry of gaseous thermolysis products (MS). It has been established that the release of water and carbon dioxide is completely completed at a temperature of 600°C. The specific surface area of the solid phase of WTP sludge before and after freezing-thawing was determined. The pore size distribution was studied. The BET isotherm of WTP sludge corresponds to mesoporous sorbents.

Graphene oxide functionalized organosilanes for electrochemical detection of uric acid in urine and water

The development of a sensitive molecular probe for recognition of uric acid is imperative because of diseases caused from change in its normal level. In the present article, new nanocomposites are developed based on graphene oxide (GO) functionalized organosilanes and applied for electrochemical detection of uric acid using GO-Silane/Glassy Carbon Electrode (GCE). Firstly, Isoindolone tethered organosilanes are synthesized by inserting amino phenol into pthallic anhydride followed by azide-alkyne click reaction catalyzed by [CuBr (PPh3)3]. The presence of silane unit helped in the extension of this molecular system in the material field and the prepared organosilanes have been grafted over the graphene oxide surface to get the desired probe for uric acid. The newly synthesized compounds have been well characterized by Infrared Spectroscopy (IR), Nuclear Magnetic Resonance (1H and 13C NMR), X-ray Diffraction (XRD), Field Emission Scanning Electron Microscope (FE-SEM) and mass spectral analysis. Cyclic Voltammetry (CV) and Differential Pulse Voltammetry (DPV) are used to evaluate the electrochemical signal of the prepared GO-Silane/GCE electrode. The results obtained shows excellent selectivity for uric acid against different species with a low detection limit of 65.7 nM in the linear range 2.5 μM–80.0 μM. Further, the outcome of the work suggests high specificity of the current GO-silane based receptor for uric acid in the presence of different interfering ions. Moreover, the real sample analysis of the present organosilane-based receptor in urine and water pave the way for its practical applicability.

Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry Analysis of Urinary Oligosaccharides and Glycoamino Acids for the Diagnosis of Mucopolysaccharidosis and Glycoproteinosis.

Mucopolysaccharidosis (MPS) and glycoproteinosis are 2 groups of heterogenous lysosomal storage disorders (LSDs) caused by defective degradation of glycosaminoglycans (GAGs) and glycoproteins, respectively. Oligosaccharides and glycoamino acids have been recognized as biomarkers for MPS and glycoproteinosis. Given that both groups of LSDs have overlapping clinical features, a multiplexed assay capable of unambiguous subtyping is desired for accurate diagnosis, and potentially for severity stratification and treatment monitoring. Urinary oligosaccharides were derivatized with 3-methyl-1-phenyl-2-pyrazoline-5-one (PMP) and analyzed by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) together with the underivatized glycoamino acids. Novel biomarkers were identified with a semi-targeted approach with precursor mass scanning, the fragmentation pattern (if applicable), and the biochemical basis of the condition. A UPLC-MS/MS analysis with improved chromatographic separation was developed. Novel biomarkers for MPS-IIIA, IIIB, IIIC, and VII were identified and validated. A total of 28 oligosaccharides, 2 glycoamino acids, and 2 ratios were selected as key diagnostic biomarkers. Validation studies including linearity, lower limit of quantitation (LLOQ), and precision were carried out with the assay performance meeting the required criteria. Age-specific reference ranges were collected. In the 76 untreated patients, unambiguous diagnosis was achieved with 100% sensitivity and specificity. Additionally, the levels of disease-specific biomarkers were substantially reduced in the treated patients. A multiplexed UPLC-MS/MS assay for urinary oligosaccharides and glycoamino acids measurement was developed and validated. The assay is suitable for the accurate diagnosis and subtyping of MPS and glycoproteinosis, and potentially for severity stratification and monitoring response to treatment.

Comprehensive characterization of modern industrial Argentinian paints for improved chronological painting attribution

Throughout the twentieth century, the paint industry developed a multitude of new binding media, pigments and additives that improved the appearance, ease of application, and performance of modern industrial paints. Depending on when and where they were first manufactured, and when they were introduced into paint formulations, some of these new paint components could conceivably be chronological markers useful in assigning attribution to specific artists or in the study of forgeries. The aim of this study was to develop a systematic methodology for characterizing organic and inorganic materials in modern paints, and search for potential chronological markers. Colored reference paints manufactured by local companies in Argentina from the 1940s and 1950s were studied with a multi-analytical approach that included Fourier-transform infrared spectroscopy, gas chromatography coupled with mass spectrometry, Raman spectroscopy, X-ray diffraction, X-ray fluorescence and scanning electron microscopy with energy dispersive X-ray analysis. A wide range of compounds was identified due to the complementarity use of the analytical techniques. Historical references, patents, books, and scientific publications about the materials used in that time period provided invaluable information in establishing tentative timelines for modern paint components. This investigation was part of a broader interdisciplinary investigation of Concrete Art, an international art movement of the beginning of the twentieth century, which took place in Argentina and other nearby countries during the 1940s and 1950s. To prove the concept, a micro-sample from “Obra N° 171” by Raúl Lozza was analyzed. Organic and inorganic fractions were studied and the information collected was correlated with developed timelines to support the authentication process. Ultimately, the information from this study may also have a direct impact on the key areas of material characterization, aging behavior, and conservation of works of art made from these products.

In-Line Co-Processing of Stainless Steel Pickling Sludge Using Argon Oxygen Decarburization Slag Bath: Behavior and Mechanism

Stainless steel pickling sludge (SSPS) is classified as hazardous solid waste, while Argon Oxygen Decarburization (AOD) slag is challenging to utilize due to the leaching toxicity of Cr. This study introduces a novel in-line co-processing technique for AOD slag and SSPS, parallel to the steelmaking process, aimed at metal recovery, sulfur fixation, and slag detoxification: pre-treatment-AOD slag bath approach. The transformations and migrations of sulfur and metal elements, such as Fe and Cr, in the co-processed mixture were analyzed using thermogravimetric–mass spectrometry (TG-MS) and scanning electron microscopy–energy dispersive spectroscopy (SEM-EDS). The results indicated that sulfur in SSPS could be transformed from CaSO4 to CaS under controlled low pre-reduction temperatures (below 800 °C), facilitating its stabilization in the slag and achieving a sulfur fixation rate of over 99%. Metal elements, including iron and chromium, first formed a small portion of spinel (FeCr2O4) during the pre-reduction phase, then Fe-Cr or Fe-Cr-C-based alloy particles were rapidly formed at high temperatures and in the presence of reducers in the slag bath (1550 °C), aggregating and growing spontaneously, ultimately achieving a metal recovery rate of over 95%. Furthermore, a reaction model for SSPS briquettes in the AOD slag bath was established to further reveal the mechanisms of sulfur, iron, and chromium stabilization and migration, thereby providing a basis for the harmless disposal of both materials. The product alloys are expected to be used as additives in stainless steel production, while the harmless slag could be safely utilized in the preparation of cementitious auxiliary materials.