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Despite the recognized importance, the determination of halogens in Antarctic seaweeds remains understudied. Limited research exists due to challenges associated with sample preparation, and reliable analytical techniques for this type of analysis. Therefore, further investigations are necessary to bridge this knowledge gap and gain a comprehensive understanding of halogen metabolism in Antarctic seaweeds. In this study, seaweeds from the coast of the Antarctic continent were characterized concerning the total content of halogens and their species. For this purpose, different sample preparation methods, based on extraction and combustion, combining highly selective and sensitive chromatographic and spectrometric multi-technique approaches were used. By using optimized methods, it was possible to determine total halogens content, the distribution of bromine and iodine in different classes of species (lipids, water-soluble, proteins, carbohydrates, and residue), as well as the identification of iodinated amino acids (MIT and DIT) in ten brown and red seaweeds. Bromate and iodate were not detected in the samples, which presented only bromide and iodide species in their composition. Additionally, unknown bromine and iodine species were observed in different extracts evaluated. Furthermore, 25 halogenated polyphenols were identified in seaweeds, of which only four were already reported in the literature. The results obtained in this study comprise unprecedented data in the literature on species of halogens present in seaweeds from the Antarctic environment. [Display omitted] • First data in the literature on halogenated species in seaweed from the Antarctic. • A multi-technique approach was used to determine classes of halogenated compounds. • Sample preparation methods used were efficient to extract halogenated compounds. • Total halogen and its species were determined in ten Antarctic seaweed species. • Halogen distributions in lipid, water-soluble, protein, and carbohydrate fractions were showed. [ABSTRACT FROM AUTHOR]

Rationale: Bromine and iodine have important physiological functions; however, in inadequate concentration, they can also cause several physiological problems. Their mobility assessment in human organisms through biological sampling may help clarify some doubts related to metabolic routes, which are still not well elucidated. In this context, a suitable analytical method for this purpose should be developed. Methods: An analytical method for determining ultratrace levels of bromine and iodine in human nail samples was developed. Inductively coupled plasma mass spectrometry (ICP‐MS) using a conventional nebulization system was immediately chosen as the determination tool because of its powerful sensitivity and selectivity. Sample preparation methods including microwave‐induced combustion (MIC), microwave‐assisted extraction, and microwave‐assisted digestion were evaluated. The compatibility of the final solutions with ICP‐MS analysis was considered while the method was developed. Results: MIC was chosen as the most suitable method for the sample preparation for determining the levels of bromine and iodine in human nail samples using ICP‐MS. Unlike other sample preparation methods, this one fully eliminated interferences related to the carbon content and memory effects. Sample masses up to 100 mg were efficiently digested, and the analytes were quantitatively absorbed using only 50 mmol L−1 NH4OH solution. Recoveries ranged from 93% to 102%, and the relative standard deviation was < 8%. Conclusions: The proposed analytical method presents important characteristics for routine analysis. It allows ultratrace determination even when low sample masses are used because of the low blank values, reduced volume of reagents, and powerful detectability using ICP‐MS. [ABSTRACT FROM AUTHOR]

The daily use of cosmetics may expose consumers to localized skin problems and systemic effects caused by absorption of chemical elements. The requirements for suitable quality control and maximum limits for toxic and potentially toxic elements in cosmetics have attracted the attention of the scientific community and of the official institutions around the world. Maximum limits for chemical elements in some cosmetics have been set, but there are disagreements between them. In the same context, many analytical methods have been proposed in the literature, but several challenges during the sample preparation and determination steps related to the high complexity of cosmetics' matrices composition still remain. It is extremely difficulty to establish suitable methods, free of interference, even using modern technology. In this review, methods for determining toxic and potentially toxic elements in cosmetics used for make-up on the lips and on the eye area, covering the period since 2000, are presented. Techniques enabling direct analysis and those requiring a sample preparation step prior to the analysis are also discussed. This review focused on cosmetics for make-up on the lips and on the eye area because the risks of percutaneous absorption and oral ingestion of toxic and potentially toxic elements is higher than in other body regions. Image 1 • Trends and challenges for determination of elements in cosmetics used for make-up are discussed. • Cosmetics composition and problems associated with the presence of toxic elements are presented. • Sample preparation methods and techniques for analysis of cosmetics are detailed and discussed. • Advantages and disadvantages of analytical methods reported in literature are discussed. • Direct analysis methods used for cosmetics are covered. [ABSTRACT FROM AUTHOR]

The microwave-assisted digestion of dietary supplements using diluted nitric acid under oxygen pressure for subsequent indirect determination of phosphorus and sulfur by ion chromatography (IC) was proposed. Different concentrations of nitric acid (from 1 to 14.4 mol L−1) and oxygen pressures (from 5 to 20 bar) were evaluated. Dissolved organic carbon and residual acidity were used to choose the most suitable digestion condition. Using the proposed method, it was possible to digest up to 1350 mg of dietary supplements using only 5 mol L−1 HNO 3 under 5 bar of oxygen pressure. Comparing to conventional digestion procedure it was possible to digest up to 60% higher sample mass using HNO 3 around 30% more diluted. Recoveries ranging from 96 to 102% were obtained when recovery tests using a standard solution or a mixture with certificate reference material were carried out. The concentration of P and S indirectly determined by IC agreed with the results obtained by conventional microwave-assisted digestion using concentrated HNO 3 and subsequent determination by inductively coupled plasma optical emission spectrometry. [ABSTRACT FROM AUTHOR]

In this work, a method combining microwave-induced combustion (MIC) for sample preparation of commercial levothyroxine sodium (L-T 4 ) drugs (L-T 4 : 25−200 µg/tablet), and potentiometry with ion selective electrode (ISE) for iodine determination and subsequent indirect quantification of L-T 4 was proposed. The type and concentration of the absorbing solution were evaluated to select the most suitable conditions for this study. Using the MIC method, it was possible to use solutions as diluted as 150 mmol L −1 (NH 4 ) 2 CO 3 (for samples containing 25−200 µg of L-T 4 /tablet) for I absorption. In these conditions, recoveries for L-T 4 were between 99% and 101%, and relative standard deviations were lower than 10%. The limit of detection for L-T 4 was 11.2 µg/tablet, which is almost two times lower than the minimum concentration of L-T 4 in commercially available drugs. Thus, the MIC was suitable for the digestion of several L-T 4 drugs for subsequent I determination by ISE and indirect quantification of L-T 4 . Furthermore, the proposed method presents high throughput with low reagent consumption and consequently lower waste generation, making it suitable for routine determination of L-T 4 in drugs. From the obtained results, it was possible to observe that one of the analyzed samples is not in agreement with the limits established by the United States Pharmacopeia, indicating the importance of the drug quality control. The United States Pharmacopeia establishes that each tablet must contain between 90% and 110% of the amount of active substance declared by the manufacturer. [ABSTRACT FROM AUTHOR]

In this study, two methods based on the use of diluted acids were developed: microwave-assisted wet digestion (MAWD) and microwave-assisted ultraviolet digestion (MAWD-UV). These methods are evaluated for the digestion of oral pharmaceutical drugs and further determination of elemental impurities from classes 1 (As, Cd, Hg and Pb) and 2A (Co, Ni and V) by inductively coupled plasma optical emission spectrometry (ICP-OES). Commercial drugs for the treatment of type 2 diabetes are used. No prior comminution is performed. For MAWD, the optimized conditions were 2 mol L−1 or 3 mol L−1 HNO3, 1 mL of 50% H2O2 and a 45 min or 55 min irradiation program. For MAWD-UV, the condition using 1 mol L−1 HNO3, 1.6 mL of 50% H2O2 and a 55 min irradiation program enabled the digestion of all samples. In this way, efficient methods are proposed for the digestion of commercial pharmaceutical tablets for further determination of class 1 and 2A elemental impurities (ICH Q3D guidelines). [ABSTRACT FROM AUTHOR]

Abstract An effective analytical method for bromine and iodine determination in human hair using interference-free inductively coupled plasma mass spectrometry (ICP-MS) was developed. Human hair was digested based on combustion reaction to obtain compatible solutions with ICP-MS analysis. Using microwave-induced combustion (MIC), masses of human hair ranging from 50 to 300 mg were efficiently digested. Only a diluted alkaline solution (100 mmol L−1 NH 4 OH) was used for the absorption of both analytes, which was fully compatible with ICP-MS analysis. Using these conditions low limits of detection were obtained (LOD of 0.01 μg g−1 for Br and 0.004 μg g−1 for I). Recovery tests at two levels (50% and 100%) using a standard solution or mixtures of the sample with certified reference materials (CRMs) were carried out to evaluate the suitability of proposed method and recoveries between 94% and 102% were always obtained. Accuracy was evaluated by analysis of a human hair CRM, and the Br and I concentrations obtained by the proposed method did not differ significantly from those described in the certificate. Repeatability (RSDs ≤ 4%) and reproducibility (RSDs ≤ 7%) of the results using proposed method were always very suitable. The digests obtained using the MIC method were fully compatible with ICP-MS and the interferences currently found using conventional digestion methods were completely eliminated. Ultra-trace concentrations of Br and I were determined in human hair, demonstrating that the proposed method is a suitable strategy, and it presents several advantages compared to others published in the literature. Graphical abstract Image 1 Highlights • The MIC method provided suitable digests for Br and I determination in human hair using interference-free ICP-MS. • Low limits of detection were obtained for Br and I. • Blank values were negligible and additional dilution step was not required. • The drawbacks of analytical methods for human hair analysis proposed in the literature were overcome. • The proposed analytical method can be used accurately and reliably by researchers in a variety of fields. [ABSTRACT FROM AUTHOR]

Abstract Microwave-assisted digestion using diluted acid under oxygen pressure is proposed for sample preparation of sports supplements and subsequent determination of Ca, Cu, Fe, K, Mg, Mn, Na, Zn, P and S by inductively coupled plasma-optical emission spectrometry (ICP-OES). In this sense, 1350 mg of sport supplement were digested in a microwave oven using only 6 mL of 5 mol L−1 HNO 3 under 5 bar of oxygen pressure during 15 min. Accuracy of proposed method was evaluated by recovery tests using a standard solution and using a certified reference material. Suitable recoveries (ranging from 86% to 108%) were obtained in both evaluations for all analytes. Results were compared with those obtained by conventional microwave-assisted digestion (without oxygen pressure) for further analytes determination by ICP-OES, and no statistical differences were observed (Student's t -test, confidence level of 95%, p > 0.05). The precision of proposed method was evaluated in terms of repeatability (RSDs ≤3%) and intermediate precision (RSDs ≤7%), and suitable results were obtained for all analytes. In addition, the limits of detection for all analytes using proposed method were lower than those obtained using conventional digestion in view of use a high sample mass and a diluted acid solution for sample digestion. The use of diluted acid reduces risks to analyst – since it eliminates the concentrated acid handling; reduces the consumption of reagents and, consequently, the waste generation, in accordance with the principles of green chemistry. Using the proposed method was possible to perform the determination of ten elements in a single analysis with suitable precision and accuracy. Six sport supplements were analyzed and the results are alarming because in most cases they were in disagreement with those informed on the label. Thus, a suitable quality control of sports supplements should be performed and the proposed method is a green, safe, accurate, precise and sensitive alternative for this purpose. Graphical abstract Unlabelled Image Highlights • The proposed method is a green, safe, accurate, precise and sensitive alternative to quality control of sports supplements. • The use of diluted acid nitric provided digests compatible with multitechnique determination, including IC and ICP-OES. • Proposed method was suitable for determination of ten elements in a single analysis with suitable precision and accuracy. • It was possible to determine metals and non-metals in sport supplements at low concentration. • Six sport supplements were analyzed and the results were in disagreement with those informed on the label. [ABSTRACT FROM AUTHOR]

A method for arsenic speciation in shark, shrimp, squid, oyster and scallop using liquid chromatography coupled to inductively coupled plasma triple quadrupole mass spectrometry (LC-ICP-MS/MS) was proposed. Suitable sensitivity and selectivity by LC-ICP-MS/MS were obtained using 10 mmol L −1 (NH 4 ) 2 HPO 4 diluted in 1% methanol (pH 8.65) as mobile phase. Recoveries from 90 to 104% for arsenobetaine (AsB), arsenite [As(III)], dimethylarsinic acid (DMA), monomethylarsonic acid (MMA) and arsenate [As(V)] were obtained for all samples. A certificated reference material was also analyzed and the sum of As species was in agreement with the total As concentration. Limits of quantification (LOQ) for AsB, As(III), DMA, MMA, and As(V) were 6, 30, 6, 12 and 26 ng g −1 , respectively. Higher concentration of AsB was found in all seafood, while As(III) and DMA were found only in oyster. Arsenate was found in squid and scallops, and MMA was below the LOQ in all samples. [ABSTRACT FROM AUTHOR]

Responding to the need for green and efficient methods to determine catalyst residues with suitable precision and accuracy in samples with high fat content, the present work evaluates a microwave-assisted ultraviolet digestion (MW-UV) system for margarines and subsequent determination of Ni, Pd and Pt using inductively coupled plasma mass spectrometry (ICP-MS). It was possible to digest up to 500 mg of margarine using only 10 mL of 4 mol L −1 HNO 3 with a digestion efficiency higher than 98%. This allowed the determination of catalyst residues using the ICP-MS and free of interferences. For this purpose, the following experimental parameters were evaluated: concentration of digestion solution, sample mass and microwave irradiation program. The residual carbon content was used as a parameter to evaluate the efficiency of digestion and to select the most suitable experimental conditions. The accuracy evaluation was performed by recovery tests using a standard solution and certified reference material, and recoveries ranging from 94% to 99% were obtained for all analytes. The limits of detection for Ni, Pd and Pt using the proposed method were 35.6, 0.264 and 0.302 ng g −1 , respectively. When compared to microwave-assisted digestion (MW-AD) in closed vessels using concentrated HNO 3 (used as a reference method for sample digestion), the proposed MW-UV could be considered an excellent alternative for the digestion of margarine, as this method requires only a diluted nitric acid solution for efficient digestion. In addition, MW-UV provides appropriate solutions for further ICP-MS determination with suitable precision (relative standard deviation < 7%) and accuracy for all evaluated analytes. The proposed method was applied to margarines from different brands produced in Brazil, and the concentration of catalyst residues was in agreement with the current legislation or recommendations. [ABSTRACT FROM AUTHOR]

A method for Br and I determination in whole egg powder and its fractions (egg white and yolk) was developed by combining microwave-induced combustion (MIC) and inductively coupled plasma mass spectrometry (ICP-MS). Using the MIC method, 350 mg of whole egg powder and its fractions were efficiently digested using 50 mmol L −1 NH 4 OH as an absorbing solution. The limits of detection for Br and I using the MIC method followed by ICP-MS determination were 0.039 and 0.015 μg g −1 , respectively. Using the proposed method, agreements with the reference values between 97 and 104% for Br and I were obtained by analysis of reference material NIST 8435. Finally, it was possible to observe that Br concentration (4.59–5.29 μg g −1 ) was higher than I (0.150–2.28 μg g −1 ) for all the evaluated samples. [ABSTRACT FROM AUTHOR]