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Different manufacturers do not produce the same quality of children's Ca–Fe–Zn oral liquid due to different production materials and processes. To improve the phenomenon of counterfeit and imitation oral liquid on the market and effectively monitor its quality, laser-induced breakdown spectroscopy (LIBS) fingerprinting with sample preparation methods can provide a tool for real-time and rapid detection of oral liquids. The sample preparation methods include filter paper adsorption (FPA), filter paper adsorption with elemental Cu (FPA with Cu), adding dropwise to glass slides (ADS), adding dropwise to glass slides with elemental Cu (ADS with Cu), and gel preparation (GP). This work collected LIBS spectrum of oral liquids from eight manufacturers. The model for eXtreme Gradient Boosting (XGBoost) was constructed for classifying oral liquids based on five sample preparation methods. The accuracy was 91.25, 94.17, 55.42, 91.25, and 91.29%, respectively. The results show that the FPA method is more straightforward, efficient, and less affected by the specificity of the color of the sample. Both ADS and GP are susceptible to the color characteristics of the sample and are not well suited to the direct detection of transparent liquids. This work demonstrated that oral liquids could be discriminated by analyzing LIBS spectrum combined with the XGBoost model. Additionally, sample preparation, like the simple FPA method, can improve the accuracy of LIBS classification. [ABSTRACT FROM AUTHOR]

To explore the influence of sample preparation methods on the permeability and microstructure of remolded loess, remolded loess collected from Heifangtai was taken as the research object. A total of 40 sets of falling-head permeability tests were conducted using two commonly used sample preparation methods, and five different dry density and four initial water content conditions. Additionally, the electrical conductivity of the leachate and the microscopic structure of the samples were analyzed. The results demonstrate that compared to the transfer wetting method, the homogeneity of samples prepared using the pre-wetting method is inferior. This difference is particularly evident when the initial water content is high. Due to the long duration of the permeability test, the pore structure is prone to change, resulting in relatively higher permeability coefficients. Moreover, the total dissolved solids (TDS) of the leachate exhibit a significant decrease with increasing seepage time, indicating the loss of soluble salts. Microscopic structural analysis reveals that samples prepared using the pre-wetting method exhibit a greater number of large pores and aggregates, which are intrinsic factors contributing to the observed differences in permeability between the two sample preparation methods. Furthermore, it should be noted that the impact of the sample preparation method on the permeability of remolded loess is more significant when the dry density is relatively low (specifically, less than 1.45 g/cm3). Conversely, when the dry density is higher, the influence becomes less pronounced. [ABSTRACT FROM AUTHOR]

In the process of production, processing, transportation, and storage of edible oils, the oils inevitably come into contact with plastic products. As a result, plasticizers migrate into edible oils, are harmful to human health, and can exhibit reproductive toxicity. Therefore, the determination of plasticizers in edible oils is very important, and a series of sample preparation methods and determination techniques have been developed for the determination of plasticizers in edible oils. Phthalic acid ester (PAE) plasticizers are the most widely used among all plasticizers. This review aims to provide a comprehensive overview of the sample preparation methods and detection techniques reported for the determination of PAEs in edible oils since 2010, focusing on sample preparation methods of edible oils combined with various separation-based analytical techniques, such as gas chromatography (GC) and liquid chromatography (LC) with different detectors. Furthermore, the advantages, disadvantages, and limitations of these techniques as well as the prospective future developments are also discussed. [ABSTRACT FROM AUTHOR]

Sample preparation is the crucial and most challenging part of analytical chemistry for the speciation of environmental pollutants' traces. Along with the development of the sample preparation methods, the ionic liquid-based microextraction technique plays an important role. Due to the unequivocally unique "green" characteristic of ionic liquids (ILs), they owe their tunable properties, such as highly selective and high reaction efficiency, reusability, and good thermal stability, to present advancements in the sample preparation process. The ionic liquid-based microextraction techniques miniaturize the sample preparation process. Liquid phase microextraction intermediate solvents, desorption solvent extractants, and mediators have been used. They are quoting the benefits and limitations of each method. A few essential sample preparation methods covered the microextraction technique. In this context, miniaturized microextraction methods have been developed. They are generally used for their unlimited positive features, including easy, simple, and environmentally friendly; they also extract inorganic and organic species with low-cost instrumentation. This review advances the sample preparation process using ILs-based liquid phase microextraction as an intermediate solvent, extractant desorption, and mediator solvents. [ABSTRACT FROM AUTHOR]

• Review of sample preparation methods for halogen IC analysis in inorganic matrices. • Comparison of inorganic sample digestion methods. • Pros and cons of analytical techniques for nonmetals analysis. • The roles, limitations, and prospects of IC in inorganic sample analysis for environmental studies. The inorganic matrices such as metal concentrates, steel, cement, glass, clay, coal, graphite, rocks and sediments, ores etc. play a pivotal role in infrastructure development, transportation, and energy. The presence of non-metallic elements particularly halogens influence their quality, processing cost, and environment dynamics. The analysis of non-metals in such matrices is critically challenging due to their hardness, rigidity, and non-digestibility. This comprehensive review provides a critical comparison of various sample preparation methods in conjunction with pros and cons of advanced techniques for the detection of non-metals in complex matrices, particularly focusing on ion chromatography. Moreover, the review also addresses the challenges related to the enrichment and automation of non-metals analysis. In addition, the previous literature on non-metals determination in diverse range of inorganic matrices has been tabulated for the first time. These insights are intended to guide researchers, quality control analysts, environmental scientists, and policymakers in enhancing pollution monitoring and control strategies. [ABSTRACT FROM AUTHOR]

The aim of this study was to carry out a systematic investigation and analysis of different drug extraction methods, specifically non-steroidal anti-inflammatory drugs in biological fluid samples, for Liquid Chromatography in Mass Spectrometry assays (LC-MS/MS). A search was carried out in the main databases between 1999 and 2021, following the Preferred Reporting Items for Systematic reviews and Meta-Analyses extension for Scoping Reviews (PRISMA-ScR) checklist. Data were obtained through PubMed, Lilacs, Embase, Scopus, and Web of Science databases using the Boolean operators AND and OR. Studies were pre-selected by title and abstract by two independent reviewers. The selected texts were read in full, and only those that were complete and compatible with the inclusion and exclusion criteria were eligible for this research. A total of 248 references were obtained in the databases. After removing the duplicates and analyzing the titles and abstracts, 79 references were evaluated and passed to the next phase, which comprised the complete reading of the article. A total of 39 publications were eligible for this study. In 52% of the studies, the authors used the liquid–liquid extraction method (LLE), while in 41%, the solid-phase extraction method (SPE) was used. A total of 5% used microextraction methods and 2% used less-conventional techniques. The literature on the main methods used, the LLE and SPE methods, is extensive and consolidated; however, we found other studies that reported modifications of these traditional techniques, which were equally validated for use in LC-MS/MS. From this review, it is concluded that the diversity of techniques, reliability, and practical information about each analytical method used in this study can be adapted to advances in LC-MS/MS techniques; however, more ecological, economic, and sustainable approaches should be explored in the future. [ABSTRACT FROM AUTHOR]

The increasing food allergic cases have posed a great challenge to the human health worldwide. Avoiding the exposure to food allergens is still the only efficient method to prevent food allergic reactions for food allergic sufferers because there are no effective treatments for food allergy up to now. Therefore, it is crucial to develop analytical technologies for rapid and on-site detection of food allergens, helping allergy-prone groups make proper option when buying or eating foods. Recently, various detection technologies and portable analytical devices have been widely developed for rapid, accurate, and on-site screening of food allergens. In this review, first of all, the traditional detection methods were simply introduced and discussed. Then, the latest advances on emerging biosensing technologies (i.e., colorimetric biosensing, fluorescent biosensing, electrochemical biosensing, surface enhanced Raman spectroscopy (SERS) biosensing, surface plasmon resonance (SPR) biosensing, and dual-mode biosensing) and portable analytical devices (such as lateral flow assays (LFAs), microfluidic chips, and paper-based microfluidic devices) for the detection of food allergens were comprehensively summarized. Furthermore, the advantages and weaknesses of these analytical methods for food allergen detection were also compared and discussed. Most importantly, the remaining challenges and chances in this important field were also proposed. Emerging biosensing technologies have shown a great potential in the on-site detection of food allergens. Impressively, the integration of biosensing technologies and portable detection devices (e.g., LFAs, microfluidic chips, and paper-based microfluidic devices) is one of the most promising methods for reliable and on-site detection of food allergens. [Display omitted] • Emerging biosensors and portable analytical devices are promising for food allergen detection. • Food sample preparation methods before food allergen detection were discussed. • Advantages and disadvantages of existing food allergen detection technologies were discussed. • Remaining challenges and chances in this promising field were proposed. [ABSTRACT FROM AUTHOR]

The aim of this study was to carry out a systematic investigation and analysis of different drug extraction methods, specifically non-steroidal anti-inflammatory drugs in biological fluid samples, for Liquid Chromatography in Mass Spectrometry assays (LC-MS/MS). A search was carried out in the main databases between 1999 and 2021, following the Preferred Reporting Items for Systematic reviews and Meta-Analyses extension for Scoping Reviews (PRISMA-ScR) checklist. Data were obtained through PubMed, Lilacs, Embase, Scopus, and Web of Science databases using the Boolean operators AND and OR. Studies were pre-selected by title and abstract by two independent reviewers. The selected texts were read in full, and only those that were complete and compatible with the inclusion and exclusion criteria were eligible for this research. A total of 248 references were obtained in the databases. After removing the duplicates and analyzing the titles and abstracts, 79 references were evaluated and passed to the next phase, which comprised the complete reading of the article. A total of 39 publications were eligible for this study. In 52% of the studies, the authors used the liquid–liquid extraction method (LLE), while in 41%, the solid-phase extraction method (SPE) was used. A total of 5% used microextraction methods and 2% used less-conventional techniques. The literature on the main methods used, the LLE and SPE methods, is extensive and consolidated; however, we found other studies that reported modifications of these traditional techniques, which were equally validated for use in LC-MS/MS. From this review, it is concluded that the diversity of techniques, reliability, and practical information about each analytical method used in this study can be adapted to advances in LC-MS/MS techniques; however, more ecological, economic, and sustainable approaches should be explored in the future.

Reproductive cells are a very special kind of material for the analysis. Depending on the species, their dimensions allow for the application of mass spectrometry imaging-based techniques to receive a reasonable data for interpretation of their condition without any additional sample preparation steps, except for typical sample preparation characteristic for IMS protocols. A comparison between lipid profiles of oocytes could answer the question of the overall quality of the cells in the function of time or conditions of storage. Even tiny differences in the lipid profiles, but still detectable by bioinformatic analysis, could be crucial for the estimation of the conditions of the cells in various stages of development or aging. In our study, MALDI-TOF/TOF MSI was used to analyze and visualize the single oocytes. We deposited the cells on the transparent indium-tin-oxide (ITO) glass and marked their positions, which allowed for the fast localization of the cells and precise laser targeting in the ion source. We also optimized the usage of different MALDI matrices and different approaches. The proposed way of measurement allows analyzing quite a significant quantity of oocytes in a reasonably short time. During the analysis, the lipid composition of the single cell was successfully estimated in a conventional usage of the MALDI ion source, and the localization of lipids was confirmed by imaging mass spectrometry (IMS) analysis. The observed quantity of the lipids allowed for the application of the LIFT™ technique to obtain MS/MS spectra sufficient for lipids' unambiguous identification. We hope that our idea of the oocyte analysis will help to elucidate chemical changes that accompany different processes in which oocytes are involved. There could be such fascinating phenomena as the oocyte maturation, changes in the lipid components during their storage, and much more. [ABSTRACT FROM AUTHOR]

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There is no direct, less expensive, and practical method to measure the interconnectivity and parameters of air voids in asphalt mixtures other than the total air void volume calculated traditionally using bulk and maximum theoretical specific gravities. Unlike the conventional method, this paper proposes a method that is suitable for advanced applications and studies, such as for the evaluation of air void distribution and air void gradient to model and simulate long-term aging, predict top-down fatigue cracking, evaluate the effectiveness of compaction of thick lifts, and satisfy the representative volume element (RVE) requirements (a homogenous and representative specimen) for performance tests. Developing the proposed compact asphalt evaluation method included modifying the sample preparation methods and analysis from the American Society of Testing & Materials (ASTM), C457 Method C, and recently applied in the analyses of two independent studies at the Federal Highway Administration (FHWA). The first study was focused on checking the air void distribution within the small specimen for dynamic modulus and uniaxial cyclic fatigue tests using AASHTO TP 132 and TP 133, respectively. Results of air void analyses conducted on the interior and exterior sides of several slices sawn from different compacted asphalt mixtures consistently showed that the air void contents on the external sides are higher than on the interior. The second study was to evaluate whether the thicker-than-typical lift thickness to nominal maximum aggregate (NMAS) ratio was causing any top-to-bottom air void gradient in the pavement. Results showed that air void sizes and contents are consistently higher along the top ends of all the cores, and the total air void contents measured using the new method on several specimens from the field were comparable with the indirectly calculated air void percent with up to ± 0.4 percent random error. Overall, the new method is practical to apply to larger-size samples and is a tool that both agencies and contractors can use for confirming in situ void uniformity. Its application can support innovations and improve performance in asphalt pavement construction. • A reliable sample preparation procedure was developed that is applicable to compacted asphalt mixtures. • Results of air void contents measured using the quantitative petrographic method were comparable with the AASHTO Methods. • The method also provides information on void sizes, abundance, distribution, and air void gradients in asphalt pavement. [ABSTRACT FROM AUTHOR]

This paper describes the most significant achievements related to the creation and development of separation methods. Tswiett Nerst’s achievements and the role of such centers as Lublin, Warsaw, Gdańsk, Poznań, Łódź, Silesia, Kraków and Toruń are presented, as well as the role of leaders who created theories and methodological studies on chromatography and related techniques. The role of sample preparation methods is emphasized based on the same or similar theoretical foundations. The directions of developing these techniques in Poland today and in the future are presented.

As strategic emerging mineral resources supported by the state, niobium and tantalum are the functional and structural materials needed for the development of emerging industries. Therefore, conducting research on the determination of niobium and tantalum in related materials is of great significance. Unfortunately, niobium and tantalum have similar physical and chemical properties, making it difficult to separate them. However, they are easy to hydrate. Geological samples are difficult to be decomposed, thus the determination of niobium and tantalum has always been a difficult issue. Sample pre-treatment technology and modern analytical techniques are reviewed in this paper. Sample pre-treatment is the key step for niobium and tantalum analysis, therefore a suitable sample digestion and preconcentration method combined with analytical methods and sample characteristics is the premise of accurate determination of niobium and tantalum. Instrument analysis is the mainstream of modern analytical technology. Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) are the most widely used methods for the determination of niobium and tantalum, but it is necessary to solve problems such as coexisting component interference, matrix effects and salt influence. Laser Ablation (LA), X-ray Fluorescence Spectrometry (XRF), and Neutron Activation Analysis (NAA) are the development direction of tantalum and niobium analysis, due to the fact that they avoid the complicated sample pre-treatment and addition of impurities by solid sample introduction.

Background: Paraquat (N, N-dimethyl-4,4-bipyridinium dichloride) is a nonselective, fast-acting, and contact chemical herbicide used extensively for weed control. It has high acute oral toxicity, the ability to accumulate in the lungs, and a high potential for pulmonary fibrosis after its intoxication. The present systematic review focuses on evaluating diagnostic aspects of paraquat (PQ) in forensic toxicology., Methods: Evaluation of the literature according to the following criteria: only human studies published from February 1971 to March 2022 which are in English on the following databases: 1) Medline/PubMed/MeSH search words: ((Methyl viologen [Title/Abstract]) OR (paraquat [MeSH Terms])) AND (forensic [Title/Abstract]); 2) Scopus Keywords related to the study aim included forensic toxicology, paraquat, Methyl viologen; 3) Web of Science. Keywords related to the study aim included forensic toxicology, paraquat, and Methyl viologen., Results: Thirty full-text articles were included. The results of our review indicate plasma and urine are more used for identifying PQ, and liver, lung, and gastric fluid are important in postmortem cases. Preparation methods, including liquid-liquid extraction (LLE), solid-phase extraction, and acetonitrile-precipitated protein, are often required for removing interfering substances. Chromatographic methods, among other analytical techniques, are more sensitive, specific, and applicable., Conclusion: Our review suggests that plasma, urine, and lungs should be prioritized in sampling. Solid-phase extraction has better recovery than LLE in many samples. Colorimetric methods are not used much today, and radioimmunoassay (RIA) has limited application despite its high sensitivity. Gas and liquid chromatography methods appear to offer the best approach for the analysis of PQ., Competing Interests: All authors disclosed a financial and personal relationship with other people or organizations that could inappropriately influence (bias) their work., (© The Author(s) 2023.)

Arcellinida (testate lobose amoebae) are widely used as bio-indicators of lacustrine environmental change. Too much obscuring organic material in a gridded wet Petri dish preparation makes it difficult to observe all specimens present and slows quantification as the organic material has to be carefully worked through with a dissection probe. Chemical deflocculation using soda ash (Na2CO3·H2O), potassium hydroxide (KOH), or sodium hexametaphosphate ((NaPO3)6) has previously been shown to disaggregate and reduce organic content in lake sediments, but to date, no attempt has been made to comparatively evaluate the efficiency of these deflocculants in disaggregating organic content and their impact on Arcellinida analysis in lacustrine sediments. Here, we assess the effectiveness of soda ash, potassium hydroxide, and sodium hexametaphosphate treatments on removing organic content and the impact of those digestions on Arcellinida preservation in 126 sample aliquots subdivided from three sediment samples (YK-20, YK-25, and YK-57) collected from three lakes near Yellowknife, Northwest Territories, Canada. Following treatment, cluster analysis and Bray-Curtis dissimilarity matrix (BCDM) were utilized to determine whether treatments resulted in dissolution-driven changes in Arcellinida assemblage composition. Observed Arcellinida tests in aliquots increased drastically after treatment of organic-rich samples (47.5–452.7% in organic-rich aliquots and by 14.8% in aliquots with less organic matter). The BCDM results revealed that treatment with 5% KOH resulted in the highest reduction in observed organic content without significantly affecting Arcellinida assemblage structure, while soda ash and sodium hexametaphosphate treatments resulted in marginal organic matter reduction and caused severe damage to the arcellinidan tests. [ABSTRACT FROM AUTHOR]

The known approaches to sample preparation have been improved to achieve a more complete detection of microorganisms of the Black Sea bottom sediments using flow cytometry of SYBR Green I-stained cells. Total microbial abundance in the samples from the shelf and deep-sea sediments varied from 0.03 to 1.54 × 108 cells g–1 and from 0.002 to 1.24 × 108 cells g–1 dry weight, respectively. This is comparable to the data reported previously for various areas of the oceans, including the Black Sea. Application of sodium pyrophosphate was shown to be the most universal method for treating sediments of various types; along with this, using hydrofluoric acid is possible for the deep-sea reduced sediments, whereas treatment with methanol was preferable for the sediments of coastal waters with a normal degree of aeration of the bottom layer. For samples of various types, optimal sample preparation procedures were proposed (choice of chemical reagent, mode of ultrasonic processing and centrifugation, and additional washing procedures). These procedures resulted in significantly more efficient enumeration of bacterial cells, while application of flow cytometry ensured rapid determination of the total number of microorganisms in the bottom sediments. [ABSTRACT FROM AUTHOR]

The quality and safety of food is one of the most important issues in our life. In this work, four different sample preparation methods, i.e., rice powder pellet with boric acid (RPPBA), rice powder pellet (RPP), rice grain pellet (RGP) and rice grain (RG), were carried out to study the adulteration problem in food industry. 20 kinds of rice from different geographic origins were classified by laser-induced breakdown spectroscopy (LIBS) coupled with principal component analysis (PCA) and support vector machine (SVM). PCA was used to reduce the input variables of SVM, and the classification accuracies by PCA and SVM combination for the four sample preparation methods were 92.70%, 95.70%, 98.80%, and 99.20%, respectively. In addition, the sample preparation times were 15, 12, 10, and 1 min, respectively. These results show that RG was simpler and more efficient sample preparation method for distinguishing different geographical origin of agricultural products than the other preparing methods of RPPBA, RPP, and RG. Modeling efficiency of SVM could be improved by reducing its input variables using PCA. It can be concluded that the LIBS technique combined with chemometric method should be a promising tool to rapidly distinguish different rice geographic origins. [ABSTRACT FROM AUTHOR]

The sensitivity of complex analytical procedures depends not only on the sensitivity of the analytical instrument used, but also on the recovery degree of the examined analyte by the employed sample preparation method. The recovery degrees of individual cannabinoids reported in literature, estimated using the same sample preparation method, are unexpectedly divergent. Therefore, the aim of this study was a thorough assessment of the most commonly used sample preparation methods, such as protein precipitation, LLE, QuEChERS and SPE, in the context of the reliability of the obtained results. The presented report shows that the highest sensitivity, precision and reliability of the chromatographic analysis of CBG, CBD, ∆9-THC and CBN in human plasma can be obtained using SPE. The recovery degrees of these cannabinoids by SPE are highly repeatable and exceed 95 %, while they are significantly lower for such sample preparation methods as protein precipitation, LLE and QuEChERS (ca. 80, 65 and 87, respectively). Moreover, the supernatants obtained by the latter methods contain interferents evoking matrix-effect, which makes reliable quantification of the listed cannabinoids by GC difficult. To our knowledge, the paper is the first such extensive comparison of sample preparation procedures used for the determination of cannabinoids in plasma by GC-MS and HPLC-MS. The presented results and the discussion allow to understand why different recovery degrees for the same xenobiotic can be find in literature despite they have been estimated using the same or different sample preparation method or different chromatography types. [Display omitted] • Analyte recovery degree as a key factor in analytical procedure of complex mixtures. • SPE gives almost 100 % recovery of cannabinoids from blood plasma. • SPE allows for reliable analysis of cannabinoids in blood/plasma by GC and HPLC. • Plasma LLE and QuEChERS supernatants contain interferents evoking matrix effect in GC. [ABSTRACT FROM AUTHOR]

The exposome is the measure of total environmental exposures and has a significant impact on human health outcomes. Exposomics research typically examines complex biological samples and assesses 100s to 1,000s of small molecules associated with chemical exposure events. To acquire robust and comprehensive datasets encompassing a broad range of multi-class biomarkers of chemical exposures, high-resolution and tandem mass spectrometry have emerged as the preferred analytical tools in the field. Due to matrix effects and interferences associated with complex biological samples together with the presence of very low abundance analytes, sensitivity and reproducibility have plagued exposomic studies. This is especially true for large sample sets where adequate robustness is frequently lacking. A possible solution to this problem is the development of non-discriminatory sample preparation methods which can reduce interferences while increasing sensitivity and reproducibility. However, sample preparation techniques intrinsically result in a discrete loss of analytes leading to the outstanding analytical challenge of finding a proper balance. Therefore, approaches which decrease matrix interferences while preserving broad chemical coverage need to be developed. In this review, sample preparation procedures currently applied in exposome research and related fields are summarized and critically evaluated. This includes a comparison of advantages and limitations between different techniques such as solid-phase extraction, liquid extraction, QuEChERS, filters and dilute and shoot with a liquid chromatography-mass spectrometry analysis focus. Based on this evaluation, recommendations promoting balanced strategies for sample preparation in future exposome research applications are provided. • Current sample preparation techniques applied in mass spectrometry-based exposomics research are reviewed. • Challenges and advantages of available sample preparation methods are discussed. • Results from recent publications are compiled by analytical method, chemical coverage and performance. • Strategies are recommended for further research and application in future exposomics studies. [ABSTRACT FROM AUTHOR]

In this paper, analytical procedures are proposed for determination of inorganic constituents in honey samples from different regions of Brazil. Inductively coupled plasma with mass spectrometry detection (ICP-MS) was used to determine the analytes, using two different sample preparation methods: acid mineralization in block digester and microwave-assisted acid digestion. The methods were optimized in order to minimize the final acidity and the residual carbon content after the sample preparation. It was observed that mineralization using microwave radiation with 2 mol L HNO was the most suitable method for determination of minerals and trace elements by ICP-MS. Besides, Se, Mg, Ca, Al, P, Mn, Fe, Cu, Zn, Ba, and Pb were determined in 60 honey samples by ICP-MS. The appropriate instrumental conditions were also evaluated for this determination, as the need of the use of collision-reaction interface and internal standards. The accuracies were evaluated using two certified reference materials, and the recoveries ranged from 82 to 115 %. The results showed no evidence of contamination in the honey samples analyzed. [ABSTRACT FROM AUTHOR]

Fluorine, chlorine, bromine, and iodine have been studied in biological samples and other related matrices owing to the need to understand the biochemical effects in living organisms. In this review, the works published in last 20 years are covered, and the main topics related to sample preparation methods and analytical techniques commonly used for fluorine, chlorine, bromine, and iodine determination in biological samples, food, drugs, and plants used as food or with medical applications are discussed. The commonest sample preparation methods, as extraction and decomposition using combustion and pyrohydrolysis, are reviewed, as well as spectrometric and electroanalytical techniques, spectrophotometry, total reflection X-ray fluorescence, neutron activation analysis, and separation systems using chromatography and electrophoresis. On this aspect, the main analytical challenges and drawbacks are highlighted. A discussion related to the availability of certified reference materials for evaluation of accuracy is also included, as well as a discussion of the official methods used as references for the determination of halogens in the samples covered in this review. [Figure not available: see fulltext.] [ABSTRACT FROM AUTHOR]

Pretreatment methods for measuring stable sulphur (δ34S) and oxygen (δ18O) isotope ratios of dissolved sulphate from watersheds have evolved throughout the last few decades. The current study evaluated if there are differences in the measured stable S and O isotope values of dissolved sulphate from forested watersheds when pretreated using three different methods: Method 1 (M1): adsorb sulphate on anion exchange resins and send directly to isotope facility; Method 2 (M2): adsorb sulphate on anion exchange resins, extract sulphate from anion exchange resins, and send the produced BaSO4 to the isotope facility; and Method 3 (M3): directly precipitate BaSO4 without anion exchange resins with the precipitates being sent to the isotope facility. We found an excellent agreement of the δ34Ssulphate values among all the three methods. However, some differences were observed in the δ18Osulphate values (M1 versus M2:−1.5 ‰; M1 versus M3:−1.2 ‰) associated with possible O contamination before isotope measurement. Several approaches are recommended to improve the pretreatment procedures for δ18Osulphate analysis. [ABSTRACT FROM AUTHOR]

Abstract: Essential plants, due to their long presence in human history, their status in culinary arts, their use in medicine and perfume manufacture, belong to frequently examined stock materials in scientific and industrial laboratories. Because of a large number of freshly cut, dried or frozen plant samples requiring the determination of essential oil amount and composition, a fast, safe, simple, efficient and highly automatic sample preparation method is needed. Five sample preparation methods (steam distillation, extraction in the Soxhlet apparatus, supercritical fluid extraction, solid phase microextraction and pressurized liquid extraction) used for the isolation of aroma-active components from Thymus vulgaris L. are compared in the paper. The methods are mainly discussed with regard to the recovery of components which typically exist in essential oil isolated by steam distillation. According to the obtained data, PLE is the most efficient sample preparation method in determining the essential oil from the thyme herb. Although co-extraction of non-volatile ingredients is the main drawback of this method, it is characterized by the highest yield of essential oil components and the shortest extraction time required. Moreover, the relative peak amounts of essential components revealed by PLE are comparable with those obtained by steam distillation, which is recognized as standard sample preparation method for the analysis of essential oils in aromatic plants. [Copyright &y& Elsevier]

A sensitive and selective method for quantitation of glimepiride in human plasma was established using liquid chromatography-electrospray ionization tandem mass spectrometry. Three different methods for the sample preparation of glimepiride and an internal standard were investigated (liquid-liquid extraction, solid-phase extraction and protein precipitation). Glipizide was used as an internal standard. Compounds were separated on a C18 column with 80% acetonitrile and 20% deionized water (adjusted to pH 3.5 with acetic acid), as mobile phase at a flow rate of 200 μL min−1. By use of multiple reaction monitoring mode in MS-MS with liquid-liquid extraction and solid-phase extraction, glimepiride and glipizide were detected without severe interference from the human plasma matrix. Glimepiride produced a protonated precursor ion ([M+H]+) at m/z 491 and a corresponding product ion at m/z 352, and the internal standard produced a protonated precursor ion ([M+H]+) at m/z 446 and a corresponding product ion at m/z 321. The limit of quantitation was 0.1 ng mL−1, 0.5 ng mL−1 and 1.0 ng mL−1 when using liquid-liquid extraction, solid-phase extraction and protein precipitation, respectively. The validation, reproducibility, stability, and recovery of the different sample preparation methods were comparable and all the methods gave reliable results. The method has been successfully applied to pharmacokinetic study of glimepiride in human plasma. [ABSTRACT FROM AUTHOR]

The widespread use and questionable environmental acceptability of non-ionic surfactants make the alkylphenol ethoxylates (APEOs) and their neutral and acidic degradation products a focus of interest in environmental analytical chemistry. An overview of sample preparation methods used for the determination of alkylphenolic compounds in solid environmental samples is presented. Specific issues related to sample preparation, such as sample collection, preservation, advanced extraction and clean up techniques, are discussed. Levels found in sediment, sewage sludge and biota are reviewed briefly. [ABSTRACT FROM AUTHOR]

This paper describes the most significant achievements related to the creation and development of separation methods. Tswiett Nerst's achievements and the role of such centers as Lublin, Warsaw, Gdańsk, Poznań, Łódź, Silesia, Kraków and Toruń are presented, as well as the role of leaders who created theories and methodological studies on chromatography and related techniques. The role of sample preparation methods is emphasized based on the same or similar theoretical foundations. The directions of developing these techniques in Poland today and in the future are presented. [ABSTRACT FROM AUTHOR]

To carry the comparative analysis of sample preparation methods for the most effective identification of Candida yeast by mass spectrometric analysis. 265 strains of yeast and yeast-like fungi isolated from the sputum of patients with pneumonia were investigated. The selected strains were identified by conventional methods (cultural, morphological, tinctorial, enzymatic properties) and MALDI-ToF MS using the Autoflex speed III Bruker Daltonics mass spectrometer (Germany) and Flex Control software. To evaluate the effectiveness of fungi species determinination, the comparative analysis of sample preparation was performed using 4 methods: direct application to the target, an extended direct application method, protein extraction using ethanol/formic acid or trifluoroacetic acid. The accelerated scheme of identification of fungi by the culture method does not provide clear and unambiguous results. When using mass spectrometric analysis, the reliability of the results depended on the sample preparation. A comparative study of the effectiveness of fungi species determination by various methods of the sample preparation of 50 clinical isolates was carried out. It was revealed that the extraction of cells using TFC acid does not lead to the appearance of the recordable protein spectra. The use of direct and extended direct application methods made it possible to establish the species only in 32-44% of the strains. The most effective method of sample preparation was the method using formic acid and ethanol, which allowed us to determine the species affiliation in 100% of the studied fungi (Score 2.0). Depending on the yeast species, a high statistical indicator (Score≥2.3) was registered for 42-100% of samples. The results of present study show that the use of MALDI-ToF MS is the most reliable and informative method of Candida spp.identification., Competing Interests: The authors declare no conflict of interest.

For the first time the method DI-SPME/LC-TOFMS was used and developed in order to determine the large antidepressant drugs in real forensic cases. The aim of the study was to optimize the new DI-SPME/LC-TOFMS method for the quantification of the large group of psychotropic drugs such as benzodiazepines, selective serotonin reuptake inhibitors, selective serotonin and noradrenaline reuptake inhibitors, tricyclic antidepressants and sleeping pills "Z". The volume of the sample, adsorption time, post-adsorption purification and desorption time were precisely optimized. The validation parameters such as limit of detection and quantification, linearity, precision during and between days and the matrix effect were determined. All obtained values are within the acceptable range for toxicological analyses. The usefulness of the method was confirmed by analyzing the post-mortem samples. Drug concentrations were determined in real samples with high precision, which gives perspectives for the DI-SPME/LC-TOFMS routine application in toxicological and forensic analyses in the future. Image 1 • Blood and Bone marrow aspirate (BMA) as a usefully material in forensic analysis. • Psychotropic drugs determined in blood and bone marrow aspirate. • DI-SPME as a good solution in analytical and forensic analysis. • Postmortem analysis by using new DI-SPME/LC-TOFMS method. [ABSTRACT FROM AUTHOR]

The extracellular matrix is a key component of tissues, yet it is underrepresented in proteomic datasets. Identification and evaluation of proteins in the extracellular matrix (ECM) has proved challenging due to the insolubility of many ECM proteins in traditional protein extraction buffers. Here we separate the decellularization and ECM extraction steps of several prominent methods for evaluation under real-world conditions. The results are used to optimize a two-fraction ECM extraction method. Approximately one dozen additional parameters are tested, and recommendations for analysis based on overall ECM coverage or specific ECM classes are given. Compared with a standard in-solution digest, the optimized method yielded a fourfold improvement in unique ECM peptide identifications., Competing Interests: Conflict of interest The authors declare no competing interests., (Copyright © 2021. Published by Elsevier Inc.)

Based on the bioactive properties of certain compounds, such as antioxidant and anti-inflammatory activities, an interesting subject of research are natural substances present in various parts of plants. The choice of the most appropriate method for separation and quantification of biologically active compounds from plants and natural products is a crucial step of any analytical procedure. The aim of this review article is to present an overview of a comprehensive literature study from the last 10 years (2007-2017), where relevant articles exposed the latest trends and the most appropriate methods applicable for separation and quantification of biologically active compounds from plant material and natural products. Consequently, various extraction methods have been discussed, together with the available procedures for purification and pre-concentration and dedicated methods used for analysis., (© 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)