Review: Hydrothermal Synthesis Methods for Copper Nanoparticles: A Mini-Review

Paulo Cesar Rodrigues, Cristiane Renata Schmitt, Italo Odone Mazali, Marco Aurélio Zezzi Arruda

Abstract: This Mini-Review focus on the production of metallic copper nanoparticles trough hydrothermal synthesis, which represents the most applied method for metallic nanoparticles synthesis. These nanoparticles stand out for their diverse applications in various scientific and technological fields, and among these, copper nanoparticles (CuNPs) are particularly notable for their unique properties, including catalytic, optical and electronic characteristics. These properties are influenced by the size, shape and structure of the particles. Then, the influence of precursor salts, reducing agents, and stabilizers are discussed inside this Mini-Review on the size and shape of CuNPs. Additionally, in recent years, green synthesis methods have gained prominence due to their environmental compatibility and sustainability, but require more robust methods to be implemented. Routes using metal reducing agents such as extracts from plants, flowers, stems are already found in the literature, and some examples are presented in such Mini-Review. Furthermore, we explore the potential applications of CuNPs in areas such as catalysis, antibacterial agents, medical diagnostics, and bioanalytics.

Review: Analytical Techniques for the Determination of Elemental Composition of Coffee

Vilela, T. M.; Almeida, T. C. R.; de Souza, A. L. M.; Joca, J. F. S.; Oliveira, R. S.; Batista, B. L.; Baccaro, A. L. B.; Gaubeur, I.; Felix, F. S.

Abstract: According to the Coffee Market Report (2024) of the International Coffee Organization, the annual worldwide production of coffee increased 5.82% achieving 178 million bags between 2023 and 2024. South America is the coffee production leader accounting for 50.17% of the global production with Brazil playing a central role on it. To sustain the high quality standards under such a high demand, it is important to ensure the consumer health safety, while preserving the good flavor and aroma of coffee (terroir). Some key factors are required to allow the proper evaluation of crops and shipments using reliable parameters, which is the case of the determination of the elemental composition of coffee. Coffee organoleptic properties depend on several chemical elements of its composition, while accessing and monitoring their concentrations is challenging, since they might vary considerably according to some agronomical and climatic conditions that plantations are subjected. Yet, the analytes might not be homogeneously distributed throughout samples, demanding both refined solid sampling strategies and laborious sample preparation and pretreatment. Finally, several analytical techniques are available for researches and analysts to investigate the elemental composition of coffee samples, each one with their own advantages, limitations and particularities. Sometimes it is not a trivial task to choose a proper technique according to the aimed data. Therefore, an overview of the analysis of coffee elemental composition is herein presented, covering selected references from the last two decades. The selected works discuss the determination of elements affecting the quality of coffee in terms of terroir, toxicity, nutritional content, and geographical origin.

Article: Multivariate optimization of a HS-SPME+GC×GC-MS Procedure to Determine Fingerprints of the Volatile Fraction of Lager Beers

Isabela Cristina de Matos Cunha, Fabio Augusto

Abstract: In this work we describe the optimization and application of a HS-SPME-GC×GC-MS method to assess the volatile fraction of Lager beers. The method development was performed using a combination of univariate and simultaneous multivariate approaches. Before use, canned beer samples were decarbonated by a freeze+taw procedure designed to minimize loss of volatile compounds and ensure complete elimination of CO2 before extraction. The GC×GC cryogenic modulation conditions were optimized considering overall peak resolution and widths, where for the HS-SPME step parameters a multivariate approach using a Doehlert matrix was adopted, targetting the maximization of the total integrated peak area. The results of the multivariate optimization pointed that the extraction efficiency was maximum with 40 °C and 30 min as extraction temperature and time respectively. Using these optimized extraction conditions, it was possible to detect from 240 to 270 chromatographic peaks on the volatile fraction of the samples; among them 85 were identified. These results point out that careful optimization of operational parameters render HS-SPME combined to GC×GC-MS as a powerful tool to retrieve qualitative and quantitative information regarding the composition of beers.

Article: Simultaneous Determination of Tryptophan and 5-hydroxytryptophan in Dietary Supplements using Capillary Zone Electrophoresis and Capacitively Coupled Contactless Conductivity Detection

Brenda Maria de Castro Costa, Lucas Paines Bressan, Dosil Pereira de Jesus, José Alberto Fracassi da Silva

Abstract: Serotonin is a neurotransmitter that plays several roles in human health, mainly related to well-being sensation and physiological processes. It is a metabolite of tryptophan and 5-hydroxytryptophan, which are used as dietary supplementation. A simple method was developed to separate these three compounds using capillary electrophoresis equipped with capacitively coupled contactless conductivity detection, where the optimized conditions were background electrolyte consisting of a 3.0 mol L^-1 acetic acid solution pH 2.13, separation voltage at +27 kV, hydrodynamic injection at 11 kPa and 5.0 s, 40 cm (total) and 20 cm (effective) length fused-silica capillary (30 µm inner diameter). By using these conditions, complete resolution of these three compounds was achieved in less than 6 minutes with efficiencies higher than 8.6×10⁴ plates m^-1. The limits of quantification were 66 µmol L^-1 for serotonin and tryptophan and 132 µmol L^-1 for 5-hydroxytryptophan. The method was applied on the determination of tryptophan and 5-hydroxytryptophan in supplements, and on the evaluation of the stability of the formulations under forced degradation studies.

Article: Development of an Air-assisted Dispersive Liquid-Liquid Microextraction Method as a Valuable Biomonitoring Tool for Exposure Assessment of Phthalates

Bruno Alves Rocha, Matheus Gallimberti, Marília Cristina Oliveira Souza, João Paulo Bianchi Ximenez, Anderson Joel Martino-Andrade, José L. Domingo, Fernando Barbosa Jr.

Abstract: In recent years, the number of epidemiological studies on phthalates that can inform and help update health risk assessments has grown rapidly. Developing reliable and rapid analytical methods for determining phthalate monoesters (m-PAEs) is an important biomonitoring tool for assessing exposure. In this study, a fast and sensitive method was developed to determine 15 m-PAEs in human urine samples as effective biomarkers for exposure assessment. Air-assisted dispersive liquid-liquid microextraction and liquid chromatography coupled to mass spectrometry were used. In order to determine the optimal conditions and model the variables influencing the extraction efficiency, a central composite rotatable design coupled with response surface methodology was used. Under the optimized conditions, the method achieved good linearities (R > 0.99), satisfactory intra- and inter-day accuracies (97–111%), and intra- and inter-day precision (RSD < 14%). The proposed procedure allowed the detection of the m-PAEs with limit of detection values between 0.02 and 0.10 ng mL^-1, which makes the method sensitive and appropriate for assessing internal exposure to phthalates. The applicability of the proposed procedure was evaluated by screening fifty children’s urine from Brazil. High detection frequencies and urinary concentrations of several m-PAEs associated with using personal care products and diet were found.

Article: Cork-Activated Carbon as a Sorptive Phase for Microextraction of Emerging Contaminants in Water Samples

Valentina Rojas-Candia, Daniel Arismendi, Eduardo Carasek, Pablo Richter

Abstract: A novel strategy for microextraction of emerging contaminants was developed by using cork activated carbon (CAC) as the sorbent phase. Carbonization of the natural phase increased the surface area and the porosity of the material, thus improving the extraction efficiency. Moderately polar compounds, such as ibuprofen and its metabolites, were used as model analytes in water samples. Rotating disk sorptive extraction (RDSE) together with gas chromatography‒mass spectrometry (GC‒MS) were used for extraction and determination of the analytes, respectively. The optimum conditions for the material synthesis were 600 °C, K₂CO₃ as the activating agent and a mass ratio of 0.8:1 (activating agent:raw material). The optimum values for the RDSE were pH 2, a sample volume of 25 mL and an extraction time of 90 min. The absolute recovery rates for ibuprofen and its metabolites ranged from 19 to 55%, and the relative standard deviations were between 3 and 13%. The proposed method was used to measure the analytes in the influent and effluent from a wastewater treatment plant in Santiago, Chile. The concentrations found for ibuprofen and its metabolites were 0.98–9.8 µg L^-1 and
0.8–8.6 µg L^-1 in the influent and effluent, respectively. Activation of the cork material enabled the synthesis of a sorbent phase with sorption efficiencies similar to those obtained with the commercial octadecylsilane (C18) phase and superior to that observed for styrene-divinylbenzene (S-DVB). This process is simple and cost-effective.

Article: Simple and Fast Determination of Carbaryl Pesticide in Commercial Topical Formulations by Capillary Electrophoresis

Natalia Milaneze Cardoso, Bruna Kethelyn Pereira, José Alberto Fracassi da Silva, Dosil Pereira de Jesus

Abstract: A novel analytical method using capillary zone electrophoresis (CZE) for simple and fast determination of the pesticide carbaryl in commercial topical formulations was developed and validated. The carbaryl was previously hydrolyzed quantitatively under an alkaline medium (NaOH solution) to form 1-naphthol, which was separated and quantified by CZE with spectrophotometric detection at 214 nm. Optimization of the hydrolysis reaction regarding time and NaOH concentration was conducted. The CZE separation was achieved in less than 3 min using a bare silica capillary (60 cm total length) and a 10 mmol L^-1 sodium borate buffer (pH 9.3) as background electrolyte. The proposed CZE method was linear in the 0.25 to 70 mg L^-1 concentration range, as attested by a coefficient of determination (R²) higher than 0.999 and confirmed by the lack of fit test. Recovery tests at three concentration levels provided recovery percentages ranging from 80 to 115%, indicating acceptable accuracy. The limits of detection (LOD) and quantification (LOQ) were 0.08 and 0.25 mg L^-1, respectively. The proposed CZE method was successfully applied for carbaryl determination in commercial samples of topical formulations such as powders and dry bath gel.

Article: Impact of Nitrogen Fertilization on Nutrient Content of 'Paluma' Guavas During Fruit Development: A Target Metabolite Approach

Juliane Cristina Borba, Karina Fraige, Daniel Angelucci de Amorim, Luciana Teresa Dias Cappelini, Juliana Vieira Alberice, William Natale, Emanuel Carrilho

Abstract: Guava (Psidium guajava L.) is a tropical fruit with significant economic potential due to its in natura and industrialized consumption. This fruit has a high nutritional value due to bioactive substances, such as high levels of vitamins and carotenoids. Our study evaluated the impact of varying levels of nitrogen fertilization on the development of guava fruits over a set of targeted metabolites. For this purpose, guava plants were fertilized with 500, 1000, and 2000 g N₂/tree, and their fruits were evaluated at four stages of development. In all stages, the diameter of the fruits was measured, and the pH and soluble solids were analyzed. Capillary electrophoresis was used to determine the concentrations of neutral sugars and ascorbic acid. High-performance liquid chromatography was used for β-carotene analysis. The study observed that nitrogen fertilization did not change the size of the fruits, but the highest concentration of fertilizer (2000 g N₂/tree) reduced the concentrations of ascorbic acid and β-carotene. These results concluded that the intermediate fertilization level (1000 g N₂/ tree) produced most of the metabolite levels studied, in contrast to the highest nitrogen level applied, which showed similar behavior to the absence of fertilization. Correct nitrogen fertilization plays a fundamental role in producing high-quality fruits, influencing the content of various metabolites produced by the fruits. Therefore, adjusting fertilization practices according to the specific needs of their crops helps produce valuable fruits. Meanwhile, incorrect nitrogen fertilization generates direct costs for farmers regarding lost production and imposes significant costs on the environment and society.

Article: Incrustations Formed in Bioelectricity Turbogenerators: An Advanced Evaluation Using Energy Dispersive X-Ray Fluorescence (ED-XRF) and Exploratory Analysis

Érik Geraldo da Silva Souza, Fabiola Manhas Verbi Pereira

Abstract: This study aims to develop analytical methods that utilize advanced techniques, including x-ray fluorescence (XRF) in conjunction with data science, to monitor samples of incrustations formed in bioelectricity turbogenerators of power plants within the sugar-energy sector. By employing these cutting-edge technologies, valuable information can be generated to enhance bioenergy processes. The proposal to implement direct analysis for this specific type of analytical matrix is innovative as it enables the determination of the chemical composition of incrustations. By conducting analyses with higher frequency, this approach will facilitate informed decision-making regarding the chemical treatments of water used for steam generation, thereby safeguarding the equipment and optimizing the process of electrical energy cogeneration.

Article: Air-assisted Liquid-Liquid Microextraction Procedure to access Mono-Hydroxylated Polycyclic Aromatic Hydrocarbons Metabolites in Human Urine Samples

Marília Cristina Oliveira Souza, João Carlos Jacinto Souza, Jonas Carneiro Cruz, Bruno Alves Rocha, Fernando Barbosa Jr.

Abstract: In this study, the air-assisted liquid-liquid microextraction (AALLME) and the dispersive liquid-liquid microextraction (DLLME) techniques were compared in determining six mono-hydroxylated polycyclic aromatic hydrocarbons (OH-PAHs) in human urine samples by gas chromatography coupled to mass spectrometry (GC-MS). The parameters (type and volume of extraction and dispersive solvent, extraction cycles, sample pH, and ionic strength) that influence the extraction efficiency in the proposed procedures were investigated and optimized. After optimization, both methods were compared in terms of extraction efficiency. Although both AALLME (16-83%) and DLLME (15-92%) provided comparable extraction efficiencies, AALLME outperformed DLLME in determining four in six OH-HPAs. In addition, the technique used less organic solvent as it dismissed the dispersive solvent. Therefore, the developed AALLME method was chosen to analyze figures of merit, showing adequate linearity (r² > 0.99) ranging from 0.72-1.92 (LOQ) to 20 ng mL^-1. LODs ranging from 0.24 to 0.69 ng mL^-1 were obtained. Precision (3.1 to 14.9%) and accuracy (7.8 to 13.3%) were assessed at three concentration levels (3.0, 9.0 and 15.0 ng mL^-1). The new method was applied to 20 human urine samples, randomly collected from healthy Brazilian adults, to confirm its applicability. Finally, the proposed and validated AALLME method was considered simple, fast, and convenient, making it a straightforward strategy for large-scale biomonitoring studies.

Article: Diluted Acid and Microwave-Assisted Extraction for Trace Element Determination in Biochar by ICP OES and ICP-MS

Beatriz M. Fontoura, Nicholas Judd, Matthew Schmittling, Michael D. Gross, Bradley T. Jones, George L. Donati

Abstract: Determination of trace elements in biochar usually involves complex and inefficient sample preparation strategies due to the high carbon content and presence of silicates in the sample matrix, as well as to the variety of raw materials used in its production. Most methods are time-consuming, employ hazardous reagents (e.g. hydrofluoric acid), and are prone to analyte contamination and loss. Another issue is the lack of validation to ensure that these methods provide accurate results. In this study, we describe a sample preparation strategy to determine Al, As, Ba, Ca, Co, Cr, Cu, Fe, K, Mg, Mo, Mn, Na, Ni, P, Pb, S, Sr, Ti and Zn in biochar by inductively coupled plasma optical emission spectrometry (ICP OES) and inductively coupled plasma mass spectrometry (ICP-MS). The method includes a dry ashing step, followed by microwave-assisted extraction with diluted nitric acid, and hydrogen peroxide. Initially, it was evaluated for efficacy using a hog waste biochar and compared to a similar and commonly reported extraction with aqua regia. The method’s accuracy was assessed by addition and recovery experiments, with analyte recoveries in the 89.6%-114% range. Limits of detection were in the 0.02-3000 and 0.006-0.02 mg kg^-1 ranges for ICP OES and ICP-MS, respectively, with lower values for HNO₃ + H₂O₂ compared to aqua regia. Relative standard deviation (RSD) values using HNO₃ + H₂O₂ were below 10% for all analytes, except As (15%), Cr (12%), and Pb (11%), while aqua regia values were in the 15%-63% range. The method was then applied to the analysis of five commercially available biochar samples.

Article: Anticancer Drug Docetaxel in Hospital Effluent: Development of Chromatographic Method, Occurrence, and Degradation via Ozonation

Júlia Antunes de Oliveira, Nátalie de Paula, Jaqueline Fabiane Reichert, Ayrton Figueiredo Martins, Darliana Mello Souza

Abstract: Anticancer agents, specifically designed to induce cell death in neoplastic cells, have become increasingly prevalent contaminants in various environmental matrices. Their extensive use has resulted in their detection across multiple settings, including hospital and pharmaceutical factory effluents, domestic wastewater, and surface waters. This study aimed to develop an analytical method for determining docetaxel residues in hospital effluent using Solid-Phase Extraction (SPE) and HPLC-DAD. The SPE method demonstrated R² greater than 0.99, with recovery rates reaching 95% and an RSD of less than 2%. The LOQ was established at 10.0 μg L⁻¹, with no significant matrix effects observed for docetaxel. The validated SPE method was deemed suitable for its intended application, as all evaluated parameters met the specifications outlined in current regulatory guidelines. Docetaxel was quantified at 29.9 μg L⁻¹ (±1.3%) in one of the 14 effluent samples collected over a week from the Federal University of Santa Maria Hospital (HUSM). Given that the microbiological treatment system at HUSM does not effectively remove this drug, an advanced degradation process using ozonation was investigated. A Dispersive Liquid-Liquid Microextraction (DLLME) method was developed for bench-scale degradation studies and subsequently applied to assess the degradation of docetaxel via ozonation in real samples. The optimized extraction conditions for docetaxel involved a 10 mL hospital effluent sample at pH 9, with ionic strength adjusted using Na₂SO₄. Methanol served as the disperser solvent, while chloroform was the extracting solvent. The ozonation process achieved a removal efficiency exceeding 97% after 60 minutes of reaction, under optimal conditions of pH 7 and an average ozone production rate of 1.5 g O₃ h⁻¹. These findings indicate that ozonation is an effective treatment strategy, significantly reducing docetaxel concentrations in hospital effluent within a short reaction timeframe.

Article: Integrating an Extended-Gate Field Effect Transistor in Microfluidic Chips for Chloride and Thiocyanate Potentiometric Detection

Dhaniella Cristhina de Brito Oliveira, Fernando Henrique Marques Costa, Renato Massaroto Beraldo, José Alberto Fracassi da Silva

Abstract: In the last five years, the development of sensors based on Extended Gate Field Effect Transistors has grown by at least 223%. In this article we discuss the concepts involved behind the potentiometric response resulting from the use of EGFETs in recognizing chloride and thiocyanate ions. The results are discussed considering two ways of obtaining the response: current modulation between source-drain and the variation in threshold voltage caused by the different concentrations of the solutions. The current sensitivity for chloride was 0.0330 mA^0.5 mol^-1 L and 0.1762 mA^0.5 mol^-1 L for thiocyanate, the linear response ranged from 1.0 to 1.0x10^-5 mol L^-1 for both static and dynamic setups with R² of 0.9952 and 0.9992. The voltage sensitivity was 47.4 mV dec^-1 and 52.96 mV dec^-1 with R² of 0.9999 for chloride. For the thiocyanate detection, the linear range from 1.0 to 1.0x10^-5 mol L^-1 with 58.88 mV dec^-1 and 137.06 mV dec^-1 to voltage sensitivity, with R² of 0.9862. The voltage sensitivity obtained with the plug injection system was 170.78 mV dec^-1 ranging from 1.0 mol L^-1 to 1.0x10^-4 mol L^-1, with a R² of 0.9436. From our knowledge, this is the first demonstration of integration of EGFETs to a 3D-printed microfluidic device in recognizing chloride and thiocyanate ions.

Article: Combining Ultrasound-Assisted Extraction and ICP-MS for As, Cd, Cr, and Pb Determination in Atmospheric Particulate Matter

Felipe Almeida Silva, Rafael Francisco Santos, Gabriel Toneto Druzian, Cristian Rafael Andriolli, Érico Marlon Moraes Flores, Rochele Sogari Picoloto

Abstract: A simple, fast, and efficient ultrasound-assisted extraction (UAE) method for As, Cd, Cr, and Pb determination in atmospheric particulate matter (PM) by inductively coupled plasma mass spectrometry (ICP-MS) was developed. For the extraction procedure, the samples and the extraction solution were added directly into polypropylene vessels and placed in the ultrasound (US) bath. The following parameters were evaluated: i) sample mass: 50 to 500 mg, ii) extraction solutions: HNO₃, HCl, and HF, and iii) extraction time in the US bath: 10 to 30 min (80 °C). Accuracy was evaluated using certified reference materials (CRMs) of river sediment, (BCR 320, NIST 2704, and 8704) and by comparison with values obtained by using the method recommended by the United States Environmental Protection Agency (EPA 3052). The agreement with the CRMs and with the official method were better than 95% for all analytes when 100 mg of sample, 5 mL of an extraction solution containing 4.75 mL of 3:1 HNO₃:HCl (50%) + 0.25 mL of HF, and 20 min of heating (80 ºC) were used. Analytes were also determined by inductively coupled plasma optical emission spectrometry (ICP OES) and no statistical difference was observed (t-test, 95% confidence level) compared to ICP-MS results. The analyte concentration in the PM samples ranged from 6.60 ± 0.41 to 17.9 ± 0.9 µg g^-1 for As, from 0.839 ± 0.049 to 11.8 ± 0.6 µg g^-1 for Cd, from 31.3 ± 2.1 to 59.6 ± 3.5 µg g^-1 for Cr, and from 13.5 ± 0.5 to 123 ± 6 µg g^-1 for Pb. Low limits of detection (LODs) of 0.90, 0.015, 0.640, and 0.085 µg g^-1 were obtained for As, Cd, Cr, and Pb, respectively, which are important for the determination at low concentrations. Finally, the proposed method combined important advantages such as the use of a relatively low-cost sample preparation system (UAE method) with low reagent consumption, and a low volume of laboratory residues.

Article: Development of an Accurate Method based on MAD-SRC for the Determination of Metals and Sulfur in Crude Oil Atmospheric and Vacuum Residues by ICP OES

Gabriel Toneto Druzian, Mariele Samuel Nascimento, Ana Paula Fernandes Padilha, Rochele Sogari Picoloto, Paola Azevedo Mello, Fabio Andrei Duarte, Érico Marlon Moraes Flores

Abstract: The present study proposes for the first time a microwave-assisted digestion in an ultra-high pressure single reaction chamber (MAD-SRC) method for the digestion of atmospheric residue (AR) and vacuum residue (VR) from crude oil distillation. The determination of metals and sulfur was performed by inductively coupled plasma optical emission spectrometry (ICP OES). The type of digestion solution (HNO₃ or HNO₃ + H₂O₂), the volume of digestion solution (6 to 10 mL), maximum temperature (200 ºC and 270 ºC), and sample mass (up to 1000 mg) were evaluated. Using 1000 mg, 8 mL of HNO₃, and 270 °C the final digests presented carbon concentrations lower than 2500 mg L^-1 for both crude oil AR and VR. The accuracy of MAD-SRC was evaluated by using a certified reference material, recovery tests, and comparison with results obtained by using microwave-induced combustion (MIC). No statistical difference was observed between the results obtained after the proposed MAD-SRC method and the certified values and recoveries higher than 95% were obtained for all analytes. Comparing the results obtained by the MAD-SRC method with those obtained by MIC, an agreement higher than 95% was achieved for all analytes. The relative standard deviation was always lower than 7%. The quantification limits ranged from 0.06 µg g^-1 for Ba to 3.13 µg g^-1 for S enabling metals and sulfur determination in crude oil distillation residues virtually free of interferences. The main advantages of the proposed method is the possibility to digest up to 1000 mg of crude oil AR and VR without the use of relatively long processing time and with lower risks of contamination and volatilization of analytes when compared to an official method using open vessels (about 240 min). In addition, it was possible to obtain digests fully compatible with the determination technique making this method a suitable option for the routine quality control of crude oil AR and VR.

Article: Mercury Determination at Ultra-trace Level in Eye Shadow by a New Electrothermal Vaporization System Coupled to ICP-MS

Jussiane Souza Silva, Alessandra Schneider Henn, Geovana Mussato Mello, Valderi Luiz Dressler, Erico Marlon Moraes Flores

Abstract: Solid sampling-electrothermal vaporization inductively coupled plasma mass spectrometry (SS-ETV-ICP-MS) was proposed for ultra-trace determination of Hg in eye shadow samples. The ETV system was optimized using a heating program, consisting of drying at 80 °C for 20 s and vaporization at 800 °C for 10 s, followed by cooling for 120 s, without a pyrolysis step. The carrier gas flow rate was set to 1.10 L min^-1, and sample mass up to 4 mg was analyzed. An alternative external calibration strategy using a standard solution of Hg and magnesium silicate for matrix matching demonstrated good linearity (R² 0.9983) in the range of 5 to 100 pg of Hg. Magnesium silicate enhances analyte transport and acts as a modifier, enabling calibration with aqueous standard solutions and presenting an alternative to certified reference material (CRM). Despite the differences in signal profiles for Hg observed in the eye shadow samples, CRM MESS-3 (Marine Sediment), and the standard solution, the method has good accuracy when the signal was integrated using peak area. Compared to cold vapor inductively coupled plasma mass spectrometry, which needs acid digestion and a ten-fold dilution with a limit of quantification (LOQ) of 0.1 µg g^-1 Hg, the SS-ETV-ICP-MS provided a significantly lower LOQ (0.001 µg g^-1) and a simplified analytical approach for Hg determination. This approach presents a practical alternative for determining Hg in eye shadows at ultra-trace levels.

Technical Note: Fractionation and Spatial Distribution Analysis of Trace Elements in Wild and Farmed Shrimp from Northeast Brazil

Wladiana Oliveira Matos, Savarin Sinaviwat, Francisco Luan Fonsêca da Silva, Andrea Raab, Eva Maria Krupp, Joerg Feldmann

Abstract: Shrimp is an important commodity, and its production has been increased through aquaculture systems. This animal can bioaccumulate trace elements in their tissues, including toxic ones. The entire body of the animal can be used in culinary processes in food preparations. Thus, the distribution of trace elements in shrimps is a concern. The whole and fractionated (muscle tissue, carapace and viscera) samples of wild and farmed shrimps (Farfantepenaeus brasiliensis and Litopenaeus vannamei, respectively) from northeast of Brazil were analyzed. As, Cd, Co, Cu, Cr, Mn, Mo, Se and V were quantified by ICP-MS while for Al, Fe and Zn, MIP-OES was employed. Spatial distribution of the muscle tissue fraction cross-section of the shrimps was performed by LA-ICP-MS to assess the distribution of As, Cu, Fe, P, S and Se in both shrimp species. Wild and farmed shrimps show different content for almost all analytes, except Co and Mn. The levels of Cu, Mo, and Zn were higher in farmed shrimp. The vanadium content in wild shrimp was around one order of magnitude higher than that found in farmed shrimp. For Brazilian legislation, As (11.5 mg kg^-1) and Cd (1.94 mg kg^-1) in wild sample exceed around 10 times and 4 times, respectively, the limit established by Brazilian legislation. The trace elements distribution in fractions of shrimps are similar for both species, the majority of these elements are mainly found in carapace. Cd and Mn are almost completely present in the carapace. The most part of As, Se and Zn is in muscle tissue for both shrimp species, except As in farmed shrimp that is mostly in carapace. Similar spatial distribution was found for As, Se, P and S, probably due to the chemical similarity among them. Relevant information is obtained only through LA-ICP-MS analysis, which showed the correlation between the elements through their spatial distribution.

IBERO MS 2024 Conference – Science and Collaboration in Mass Spectrometry

The event brought together experts from around the world to discuss advancements in mass spectrometry. The congress featured a robust program, including keynote lectures, technical sessions, poster presentations, and workshops covering topics such as proteomics, metabolomics, environmental analysis, and clinical applications of mass spectrometry.

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Measurement of traces of heavy metals in cosmetic raw materials and finished products according to ISO/DIS 21392:2021 using triple quadrupole ICP-MS

Julie Moriceau, Laurent Naëls
EMEA Customer Solution Center, Thermo Fisher Scientific France

This application note highlights a complete and comprehensive workflow for the analysis of heavy metals in different types of cosmetic products, including raw materials, and will demonstrate the need to use triple quadrupole ICP-MS technology to achieve complete interference removal. As described in ISO/DIS 21392:2021, the samples were prepared using a microwave system prior to analysis.

Trace determination of Octyl&Nonyl-phenols, related Ethoxylates and Bisphenol A using on-line SPE and Orbitrap LCMSMS

James Thomas, Janine Elliott, Kenneth Burnside – SEPA, Glasgow, UK
Neville Llewellyn, Gary Woffendin, Olaf Scheibner, Ed George – Thermo Fisher Scientific

This study demonstrates the feasibility of using a Thermo Scientific Focus Hybrid Quadrupole-Orbitrap MS with a Thermo Scientific™ EQuan MAX Plus™ system to meet method detection limits for compliance with EU Water Frame Framework Environmental Quality Standards (EQS) for bisphenol A and key Alkylphenol and related Ethoxylates.

ISO 21392: A turning point in heavy metals analysis of cosmetic products

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