Development of a Dispersive Liquid-Liquid Aerosol Phase Extraction Method for the Quantification of Ag, Cd, Cu, Ni, and Pb in Seawater by Inductively Coupled Plasma Optical Emission Spectroscopy.

The dispersive liquid-liquid aerosol phase extraction (DLLAPE) method was applied for the determination of Ag, Cd, Cu, Ni, and Pb in seawater samples by inductively coupled plasma optical emission spectroscopy (ICP-OES). Key parameters such as sample pH and extractant concentration were systematically evaluated, with ammonium ,'-diethyldithiophosphate (DDTP) identified as the optimal chelating agent. Optimal extraction conditions were achieved at pH 2.

EXPRESS: Landmark Publications in Analytical Atomic Spectrometry: Fundamentals and Instrumentation Development.

The almost-two-centuries history of spectrochemical analysis has generated a body of literature so vast that it has become nearly intractable for experts, much less for those wishing to enter the field. Authoritative, focused reviews help to address this problem but become so granular that the overall directions of the field are lost. This broader perspective can be provided partially by general overviews but then the thinking, experimental details, theoretical underpinnings and instrumental innovations of the original work must be sacrificed.

Evaluation of highly adsorptive Guefoams (multifunctional guest-containing foams) as a potential sorbent for determination of volatile organic compounds (VOCs) by means of thermal desorption.

The present work delves into the feasibility of employing a novel structured sorbent referred to as GFAD (Guefoam Adsorption Device) for the determination of volatile organic compounds (VOCs) in liquid samples. The chosen method has been static headspace sorptive extraction-thermal desorption gas chromatography mass spectrometry (HSSE-TD-GC-MS). The GFAD comprises an aluminum cellular material with a distinct replication structure and a solid guest phase consisting of activated carbon particles dispersed within the cavities of the cellular aluminum.

Application of Dispersive Liquid-Liquid Aerosol Phase Extraction to the Analysis of Total and Individual Phenolic Compounds in Fried Extra Virgin Olive Oils.

Seventeen extra virgin olive oil samples from Valencian Community (Spain) were submitted to a domestic-frying process (180 °C) during different degradation times (5, 10, 30, 60, 120 min). A dispersive liquid-liquid aerosol phase extraction by using a methanol/water (50:50) extracting solution was used to isolate the polyphenol fraction. Total phenolic content (TPC) was determined, whereas the determination of seven individual target polyphenolic compounds (hydroxytyrosol, tyrosol, oleuropein, vanillic acid, -coumaric acid, ferulic acid, and vanillin) was carried out by using ultrahigh-performance liquid chromatography coupled to a tandem mass spectrometer.

Efficacy and Safety of Anakinra Plus Standard of Care for Patients With Severe COVID-19: A Randomized Phase 2/3 Clinical Trial.

Importance: COVID-19 pneumonia is often associated with hyperinflammation. The efficacy and safety of anakinra in treating patients with severe COVID-19 pneumonia and hyperinflammation are still unclear.

Objective: To assess the efficacy and safety of anakinra vs standard of care alone for patients with severe COVID-19 pneumonia and hyperinflammation.

High temperature total consumption sample introduction system coupled to microwave plasma optical emission spectrometry (MIP-OES) for the analysis of aqueous samples.

The high temperature torch integrated sample introduction system (hTISIS) is coupled to microwave plasma optical emission spectrometry (MIP-OES) for the first time. The goal of this work is to develop an accurate analysis of digested samples under continuous sample aspiration mode by coupling the hTISIS to a MIP-OES instrument. To achieve this, different operating conditions such as, nebulization flow rate, liquid flow rate and the spray chamber temperature were optimized in terms of sensitivity, limits of quantification (LOQs) and background equivalent concentration (BECs) for the determination of Ca, Cr, Cu Fe, K, Mg, Mn, Na, Pb and Zn, and these values were compared with those reported with a conventional sample introduction system.

Localized Quantitative Analysis of Polymeric Films through Laser Ablation-Inductively Coupled Plasma Mass Spectrometry.

The present work shows, for the first time, the application of laser ablation connected to inductively coupled plasma mass spectrometry (LA-ICP-MS) to the localized quantitative analysis of inclusions in polymeric industrial films. The multielemental mapping capabilities of LA-ICP-MS has allowed to chemically examine unique defects appeared during the plastic processing. This analytical tool is perfectly suited to detect elements such as Al, Mg, Zr, Ti, Cr, P, Pb, Sb, Zn, and Si in those inclusions.

Prospect on Rare Earth Elements and Metals Fingerprint for the Geographical Discrimination of Commercial Spanish Wines.

This paper presents a novel tool for Spanish commercial wine discrimination according to their designation of origin (PDO). A total of 65 commercial wines from different Spanish designation of origin (Alicante, Bullas, Campo de Borja, Jumilla, Castilla la Mancha, Ribeiro, Ribera de Duero, Rioja, Rueda, Utiel-Requena, Valdepeñas and Valencia) were characterized. The rare earth elements (REEs) content was determined by a high-temperature torch integrated sample introduction system (hTISIS) coupled to inductively coupled plasma mass spectrometry (ICP-MS).

Profiling of Organic Compounds in Bioethanol Samples of Different Nature and the Related Fractions.

Forty-one bioethanol real samples and related fractions, together with a biobutanol sample, have been analyzed with gas chromatography coupled to either mass spectrometry (GC-MS) or flame ionization detection (GC-FID). Bioethanol with different water contents, samples originated from several sources of biomass, first- as well as second-generation specimens, distillation fractions, samples stocked in containers made of four different materials, and, finally, a biobutanol sample have been analyzed. The number of the compounds found through GC-MS has been 130, including alcohols, aldehydes, ketones, esters, ethers, nitrogen compounds, organic acids, furane derivates as well as other species (e.

Evolution of the Multielemental Content along the Red Wine Production Process from and Grape Varieties.

In the present work, 38 elements were quantified in the different fractions generated by applying amateur winemaking methods. Inductively Coupled Plasma Mass Spectrometry was used as detection technique. Grapes were analyzed and separate metal profiles were also obtained for the skin and seeds.

Total polyphenol content and metals determination in Spanish virgin olive oils by means of a dispersive liquid-liquid aerosol phase extraction method and ICP-MS.

This report presents a study on the determination of total polyphenols together with metals in several samples of olive oil produced in Spain. The results provided by applying a conventional extraction method were compared against those encountered by means of the so-called Dispersive Liquid-Liquid Aerosol Phase Extraction method. The novel method is based on the dispersion of the extracting solution in the sample.

Comparative evaluation of ICP sample introduction systems to be used in the metabolite profiling of chlorine-containing pharmaceuticals via HPLC-ICP-MS.

A systematic evaluation of four different ICP sample introduction systems to be used in the context of metabolite profiling of chlorine-containing pharmaceuticals via HPLC-ICP-MS was carried out using diclofenac and its major metabolite, 4'-hydroxy-diclofenac, as model compounds. The strict requirements for GMP validation of chromatographic methods in the pharmaceutical industry were adhered to in this context. The final aim of this investigation is an extension of the applicability and validatability of HPLC-ICP-MS in the field of pharmaceutical R&D.

Tocilizumab as first treatment option in optic neuropathy secondary to Graves' orbitopathy.

Dysthyroid optic neuropathy (DON) is one of the complications that can affect Graves' orbitopathy (GO) patients. Its prevalence is estimated at less than 5%. It is usually treated with intravenous steroids, radiotherapy or orbital decompression.

First clinical symptom as a prognostic factor in systemic sclerosis: results of a retrospective nationwide cohort study.

The objective of the study is to determine the importance of the mode of onset as prognostic factor in systemic sclerosis (SSc). Data were collected from the Spanish Scleroderma Registry (RESCLE), a nationwide retrospective multicenter database created in 2006. As first symptom, we included Raynaud's phenomenon (RP), cutaneous sclerosis, arthralgia/arthritis, puffy hands, interstitial lung disease (ILD), pulmonary arterial hypertension (PAH), and digestive hypomotility.

Aerosol-Phase Extraction Method for Determination of Ca, K, Mg, and Na in Biodiesel through Inductively Coupled Plasma Optical Emission Spectrometry.

A novel extraction method was developed, optimized, and validated for the elemental analysis of organic samples. The method, called aerosol-phase extraction (APE), is based on nebulization of the extracting aqueous solution (0.1 mol·L nitric acid) on the sample.

Fully Automatic In-Syringe Magnetic Stirring-Assisted Dispersive Liquid-Liquid Microextraction Hyphenated to High-Temperature Torch Integrated Sample Introduction System-Inductively Coupled Plasma Spectrometer with Direct Injection of the Organic Phase.

A proof of concept study involving the online coupling of automatic dispersive liquid-liquid microextraction (DLLME) to inductively coupled plasma optical emission spectrometry (ICP OES) with direct introduction and analysis of the organic extract is herein reported for the first time. The flow-based analyzer features a lab-in-syringe (LIS) setup with an integrated stirring system, a Meinhard nebulizer in combination with a heated single-pass spray chamber, and a rotary injection valve, used as an online interface between the microextraction system and the detection instrument. Air-segmented flow was used for delivery of a fraction of the nonwater miscible extraction phase, 12 μL of xylene, to the nebulizer.

Determination of fat-soluble vitamins in vegetable oils through microwave-assisted high-performance liquid chromatography.

In this manuscript, a study of the effect of microwave radiation on the high-performance liquid chromatography separation of tocopherols and vitamin K1 was conducted. The novelty of the application was the use of a relatively low polarity mobile phase in which the dielectric heating effect was minimized to evaluate the nonthermal effect of the microwave radiation over the separation process. Results obtained show that microwave-assisted high-performance liquid chromatography had a shorter analysis time from 31.

Increased circulating endothelial cells and microparticles in patients with psoriasis.

Introduction: Psoriasis is a chronic pathology characterized by increased inflammation that can be associated with changes in the vascular endothelium. We quantified the levels of circulating endothelial cells (CECs) and microparticles (MPs) in patients with psoriasis in order to analyze their relationship with endothelial and inflammation markers, subclinical atherosclerosis and microcirculation.

Methods: We studied 20 patients and 20 controls.

Haematological, biochemical and inflammatory parameters in inactive Behçet's disease. Its association with red blood cell distribution width.

Red blood cell distribution width (RDW) has been shown to be associated with disease activity in several inflammatory disorders. However only one study to show this has been conducted in patients with Behçet's disease (BD). The aim of the present study was to analyse the association of RDW with BD and its main complications; i.

Hemorheological profile in primary and secondary Raynaud's phenomenon. Influence of microangiopathy.

Raynaud's phenomenon (RP) is an episodic peripheral circulatory disorder characterized by local artery spams in subjects exposed to cold or emotional stress. It is not well-established whether RP patients show an altered rheological profile, mostly due to patient classification and clinical severity. We aimed to compare the hemorheological profile in patients with primary and secondary RP with a healthy control group.

Total introduction of microsamples in inductively coupled plasma mass spectrometry by high-temperature evaporation chamber with a sheathing gas stream.

A systematic study on the high-temperature Torch Integrated Sample Introduction System (TISIS) for use in Inductively Coupled Plasma Mass Spectrometry (ICP-MS) has been performed. The investigation included the optimization of the relevant parameters (chamber temperature, sheathing gas flow rate, nebulizer gas flow rate, sample uptake rate), the evaluation of its performance characteristics (sensitivity, limits of detection, stability, memory effects, use with the dynamic reaction cell) and representative applications to environmental, biological and clinical samples. Under the optimal conditions (T=150°C; nebulizer gas flow rate of 0.

Homocysteine levels in patients with primary and secondary Raynaud's phenomenon. Its association with microangiopathy severity.

The association between hyperhomocysteinemia (HHcy) and Raynaud's phenomenon (RP) remains a matter of debate. In 18 primary RP, 23 secondary RP and 41 controls, we investigated homocysteine (Hcy) levels along with biochemical and inflammatory parameters. The Hcy levels in both primary and secondary RP were elevated when compared with controls (p < 0.

Psoriasis and hemorheology. Influence of the metabolic syndrome.

Psoriasis is a systemic inflammatory disorder with increased cardiovascular risk which has been partly attributed to the increased prevalence of the metabolic syndrome (MS). However, the contribution of rheological alterations to cardiovascular risk has been scarcely investigated. In 91 psoriasis patients and in 101 healthy volunteers, we determined the rheological profile (fibrinogen, blood viscosity and erythrocyte aggregation), along with lipidic and inflammatory parameters.