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Extraction Techniques in Sample Preparation
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Submitted by: Anurag Malik
All the research pertaining to the detection and identification of minute peptides (<4 amino acids) present in multifarious mixtures are in their early stages because of a lack of stringent peptide identification methodologies. Precise amendments like discerned censoring of ions against previously identified sequences of peptides can help overcome the aforementioned issues faced at times of optimization procedures during or after MS analysis. A state-of-the-art genesis in structure-informedpeptide identification and quantification methodologies can be guaranteed by added enrichment in the sensitivity and resolving capacity of MS, in conjunction with novel cutting edge ionization techniques. Modernization of the software for foodomics and peptidomics research and peptide identification is needed. Also, explicit and coherent structure identification in common and especially in synchronization with LC-MS requires significant attention. A continuous focus will be given to understanding of the biochemical functions of milk ingredients and their dietary implications by using a variety of powerful tools like -omics, cell models, gut microbiome research and imaging. The introduction of innovative facilities including is an absolute requirement for the development of approaches, such as proteomics, recombinant enzymes and microbial fermentation to study and improve the metabolic and health consequences of the various roles of bioactive peptides throughout the expression of genes. Consequently, the formulation of products incorporating bioactive peptides should examine the allergenicity, toxicity and stability of the a ected metabolic functions during gastrointestinal digestion. Despite considerable progress in the isolation, purification and assessment of bioactivities of BP from various natural sources, several hurdles still remain to be overcome, particularly technological advancements to produce them on a broad scale without losing activity. In conclusion, milk-derived bioactive peptides o er substantial future prospects for product development to support health, with their multifunctional assets.  
Submitted by: Michael Schoening
       Electrolyte-insulator-semiconductor (EIS) field-effect sensors belong to a new generation of electronic chips for biochemical sensing, enabling a direct electronic readout. The review gives an overview on recent advances and current trends in the research and development of chemical sensors and biosensors based on the capacitive field-effect EIS structure—the simplest field-effect device, which represents a biochemically sensitive capacitor. Fundamental concepts, physicochemical phenomena underlying the transduction mechanism and application of capacitive EIS sensors for the detection of pH, ion concentrations, and enzymatic reactions, as well as the label-free detection of charged molecules (nucleic acids, proteins, and polyelectrolytes) and nanoparticles, are presented and discussed.
Submitted by: Camila Xu
Sample preparation is and always will be the most important step in chemical analysis. Numerous techniques, methods, methodologies, and approaches are available in the literature, offering a wide range of analytical tools to the lab practitioner. Analytical scientists all over the world must deal with the development of protocols for a plethora of analytes in various sample matrices. Extraction techniques, either sorbent or solvent-based, provide the necessary tools to handle the sample in such a way that all its information can be revealed, exploiting all advantages of instrumentation to the fullest and prolonging the lifetime of the instrument for seamless operation. In the last decade, advances in sample pretreatment are following green chemistry and green analytical chemistry demands, focusing on miniaturization and automation as well as by using the least possible amount of organic solvents. The question, then, is how far have we come now and what are the future perspectives? This webinar provides a short introduction to sample preparation and include selective presentation of three state-of-the-art, representative extraction techniques: solid phase extraction, fabric phase sorptive extraction, and paper-based sorptive extraction.
Submitted by: Victoria Samanidou
Deep eutectic solvents (DESs), were introduced in 2001 as an alternative to ILs. These showed a stronger ecofriendly profile, with easier and cheaper production, while having similar properties. DESs contain large, asymmetrical ions that have low lattice energy and, thus, low melting points. They are often acquired by the complexation of a quaternary ammonium salt with a metal salt or hydrogen bond donor (HBD). The charge delocalization occurring through hydrogen bonding between, for instance a halide ion and the hydrogen-donor moiety, is responsible for the decrease in the melting point of the mixture, in relation to the melting points of the individual components. Since 2001, many scientists around the globe pursed the utilization of DESs and published a variety of studies. The use of DESs in analytical microextraction techniques is on the rise, due to the many benefits they provide, such as lower cost and easier synthesis than ILs and an environmentally friendly profile, because of the low toxicity reported, although they need further investigation. To this day, the number of HBAs and HBDs is quite limited, so more studies ought to be carried out to present a plethora of DESs available for use. Moreover, DESs are not commercially available yet, substantially affecting and further limiting their usage for routine analyses in industrial or certified laboratories. The extraordinary high relative recoveries, selectivity, low LODs and decent repeatability they offer, render them appropriate for the determination and quantification of lots of compounds in either simple or complex matrices. As seen, most applications regard liquid phase microextractions rather than solid phase microextractions, because of their liquid nature, as it is simpler to use them as supporting solid adsorbents. The fact that the sample preparation of complicated matrices is of high interest makes them ideal for the research. Hopefully, DESs will be available for purchase in the foreseeable future and will replace organic solvents in some analytical methods commonly used nowadays, while more studies are carried out about their properties. Our aim in this review will be towards the use of DESs in analytical extraction and microextraction techniques, while briefly presenting some frequently used DESs, their synthesis methods and their properties. The ever-increasing use of deep eutectic solvents (DES) in microextraction techniques will be discussed, focusing on the reasons needed to replace conventional extraction techniques with greener approaches that follow the principles of green analytical chemistry.
Submitted by: Marina Dobrovolskaia
This entry provides a comprehensive review of the current literature about biological properties and available methods for the detection of beta-glucans. It shares the experience of the Nanotechnology Characterization Laboratory with the detection of beta-glucans in nanotechnology-based drug products. This entry summarizes and discusses five different approaches currently applied for the data interpretation of beta-glucan tests with respect to the acceptability (or lack thereof) of the beta-glucan levels in pharmaceutical products.
Effervescence-assisted microextraction emerged in 2011 as a new alternative in this context. The technique uses in situ-generated carbon dioxide as the disperser, and it has been successfully applied in the solid-phase and liquid-phase microextraction fields. This minireview explains the main fundamentals of the technique, its potential and the main developments reported.
Submitted by: Victoria Samanidou
Sample preparation is the most crucial step in the analytical procedure designed for implementation in any analytical application (food analysis, bionalysis, forensics, toxicology, environmental monitoring etc). It is the limiting factor in chemical analysis since it is time consuming and it can potentially introduce errors. No one can doubt that the best approach would be the direct introduction of the sample to the instrument, however this is rarely feasible. Efficient sample pretreatment is inevitably required as the instrument technology has produced highly sophisticated and sensitive analytical equipment. Hence, the analytical scientists have to develop and apply a suitable sample preparation protocol that ensures that the composition of the sample remains unchanged, no impurities are introduced during handling, all interferences have been left back, the analytes’ concentration is not only at detectable levels, but it can also be quantified precisely and accurately and that the matrix of the sample is compatible with the analytical technique. Extraction techniques are the most powerful tool in hands of the analytical chemists and lab practitioners. Either sorbent based or solvent based, extraction techniques provide the necessary tool that can be used to handle the sample in a way that all information in it can be revealed, all advantages in instrumentation have been exploited to the fullest and the lifetime of the instrument is prolonged in a seamless operation mode.
Color additives are used extensively in several food products, as to enhance their appearance, and their nutritional properties. They can be defined as “any substance that its intentional addition of which to a food aiming for a technological (including organoleptic) purpose in the manufacture, processing, preparation treatment, packing, packaging, transport or holding of such food results, or may be reasonably expected to result, in it or its by-products becoming a component of the food or otherwise affecting the characteristics of such foods”. Thus, hereby they are presented all the late advancements related to existing analytical methods and sample preparation methodologies, for their determination and quantification in food matrices.Furthermore, all these advancements are connected to general information about the existing natural or synthetic food colorants, along with legislative information and toxicological aspects, in order to support the importance and the need of appropriate analytical methodologies.
Gas Chromatography-olfactometry (GC-O) is, by nature, the technique of choice for the screening of the molecules with odour (odorants) responsible for the aromatic sensory properties of any product. Ideally, the GC-O technique should provide an unbiased ranking of the odorants attending to the relevance of their contribution to those sensory properties. Such ranking is essential for further steps directed to the elucidation of the chemical nature of the odorants, for their quantification or for a basic understanding of the chemical bases of the aromatic perception in such product. The review discusses the different approaches for GC-O specifically applied to deciphering wine aroma. The critical difference between approaches is whether the ranking of odorants is carried out on an extract containing all the odorants present in the product or on an extract representative of the odorants contained in the vapour phases that cause the odour and flavor. Historically, most researchers have preferred techniques based on total extracts, because of sensitivity and operational issues. It is argued that the second alternative is more direct and can be more efficient, but it requires a good understanding of the factors affecting orthonasal olfaction, handling volatiles (purging, trapping, eluting, and separating) and about the sensory assessment of GC effluents.
Submitted by: Aristidis Anthemidis
A novel simple and sensitive, time-based flow injection solid phase extraction system was developed for the automated determination of metals at low concentration. The potential of the proposed scheme, coupled with flame atomic absorption spectrometry (FAAS), was demonstrated for trace lead and chromium(VI) determination in environmental water samples. The new sorptive extraction system, consisted of an online microcolumn packed with glass fiber coated with sol–gel poly (diphenylsiloxane) (sol–gel PDPS), which is presented here for the first time.
Submitted by: Victoria Samanidou
Graphene oxide (GO) is a chemical compound with a form similar to graphene that consists of one-atom-thick two-dimensional layers of sp2-bonded carbon. Graphene oxide exhibits high hydrophilicity and dispersibility. Thus, it is difficult to be separated from aqueous solutions. Therefore, functionalization with magnetic nanoparticles is performed in order to prepare a magnetic GO nanocomposite that combines the sufficient adsorption capacity of graphene oxide and the convenience of magnetic separation. Moreover, the magnetic material can be further functionalized with different groups to prevent aggregation and extends its potential application. Until today, a plethora of magnetic GO hybrid materials have been synthesized and successfully employed for the magnetic solid-phase extraction of organic compounds from environmental, agricultural, biological, and food samples. The developed GO nanocomposites exhibit satisfactory stability in aqueous solutions, as well as sufficient surface area. Thus, they are considered as an alternative to conventional sorbents by enriching the analytical toolbox for the analysis of trace organic compounds.
Submitted by: Sesha Srinivasan
In the field of energy storage, recently investigated nanocomposites show promise in terms of high hydrogen uptake and release with enhancement in the reaction kinetics. Among several, carbonaceous nanovariants like carbon nanotubes (CNTs), fullerenes, and graphitic nanofibers reveal reversible hydrogen sorption characteristics at 77 K, due to their van der Waals interaction. The spillover mechanism combining Pd nanoparticles on the host metal-organic framework (MOF) show at room temperature uptake of hydrogen. Metal or complex hydrides either in the nanocomposite form and its subset, nanocatalyst dispersed alloy phases illustrate the concept of nanoengineering and nanoconfinement of particles with tailor-made properties for reversible hydrogen storage. Another class of materials comprising polymeric nanostructures such as conducting polyaniline and their functionalized nanocomposites are versatile hydrogen storage materials because of their unique size, high specific surface-area, pore-volume, and bulk properties. The salient features of nanocomposite materials for reversible hydrogen storage are reviewed and discussed.
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