Download or read book Supercritical Fluid Extraction Supercritical Fluid Chromatography Mass Spectrometry SFE SFC MS Method Development for Online Extraction of Complex Biological and Environmental Matrices written by Blair Kristen Berger and published by . This book was released on 2022 with total page 582 pages. Available in PDF, EPUB and Kindle. Book excerpt: A systematic approach to the rapid development of hyphenated online methods for supercritical fluid extraction-supercritical fluid chromatography-mass spectrometry (SFE-SFC-MS) was established for the analysis of complex biological and environmental samples with limited sample sizes. Extensive sample preparation and cleanup is incompatible with small sample sizes. Hyphenated online extractions offer major advantages desirable where sample quantity is limited. By minimizing sample preparation and handling, online extractions provide higher throughput, and minimizes the opportunity for sample contamination or loss. However, hyphenated methods have been difficult to develop since each step has its own requirements, which has slowed penetration into many areas which it should be ideally suited. Recent instrument advances provide new opportunity in online extraction with hyphenated SFE-SFC-MS. The first step involved synergistically optimizing MS-detection, SFC-separation, and SFE extraction. Reference materials and quality controls (QCs) were developed using two separate complex matrices: A micro-dried blood spot (DBS) coring technique for antidoping analysis, and microplastics (μPs) reference materials from cryomilled plastic pellets, for environmental pollutants polycyclic aromatic hydrocarbons (PAHs). A micro-DBS coring technique was established for the for anti-doping analysis was established for direct applicability to with application to androgenic anabolic steroids (AAS) to reflect method validity for evaluation of real/field samples, For DBS: methods were optimized in a stepwise process for the separation and extraction of androgenic anabolic steroids (AAS) were applied to micro-DBS made with human and bovine blood and final method optimizations were performed with focus for Anti-doping analysis. μP Field samples: Pre-optimized methods for the online extraction and separation of environmentally persistent organic pollutants (ePOPs) were applied to marine-exposed μPs and final method optimizations were performed with focus for the targeted analysis of PAHs. The goal was to contribute alternative solutions for blood-based anti-doping testing to current techniques and broaden the accessibility of online SFE-SFC to the scientific community.
Download or read book Systematic Approach to On line Supercritical Fluid Extraction Supercritical Fluid Chromatography Tandem Mass Spectrometry Method Development written by Alison Paige Wicker and published by . This book was released on 2020 with total page 110 pages. Available in PDF, EPUB and Kindle. Book excerpt: Coupling supercritical fluid extraction (SFE) on-line with supercritical fluid chromatography (SFC) - tandem mass spectrometry (MS/MS) provides a platform for extraction, separation, and detection in a single analysis. Utilization of this technique simplifies sample preparation while limiting sample loss and/or contamination and significantly decreases total analysis time. SFE-SFC-MS/MS requires consideration of many extraction and chromatographic variables to not only provide the most efficient extraction, but to analytically transfer the extracted analytes to the column for separation. There is a fundamental lack of understanding of how the variables in SFE affect those in SFC. In the first study, on-line SFE-SFC-MS/MS was applied for the determination of polycyclic aromatic hydrocarbons (PAHs) in soil. The purpose of this study was to develop and validate the first on-line SFE-SFC-MS/MS method for the quantification of PAHs in various types of soil. Parameters for on-line extraction coupled to chromatographic analysis were optimized. The method was validated for concentrations of 10-1500 ng of PAHs per gram of soil in Certified Reference Material (CRM) sediment, clay, and sand with R2≥0.99. Limits of detection (LOD) were found in the range of 0.001-5 ng/g, and limits of quantification (LOQ) in the range of 5-15 ng/g. The method developed in this study can be effectively applied to the study of PAHs in the environment, and lays the foundation for further applications of on-line SFE-SFC-MS. Typically, a univariate approach is taken in on-line SFE-SFC-MS/MS method development which provides little insight into how the variables work together. In the second study, a multivariate approach was used to develop a better understanding of the synergistic relationship between the extraction and separation processes by focusing on the optimization of extraction parameters for target analytes with a wide range of physicochemical properties in matrices of variable retentivity. Optimal extraction parameters were determined for 18 analytes in three variable sample types. Compromise in optimal extraction parameters must be made when simultaneously extracting and analyzing a significantly wide range of analytes. Detection of drugs of abuse (DoA) in hair; being a convenient and noninvasive technique for the determination of controlled substances, is important in forensics and toxicology. SFE-SFC-MS/MS being ideal for DoA determination in complex matrices, provides a highly specific and sensitive chemical analysis while limiting the need for extensive manual sample preparation. Supercritical fluid extraction of seventeen DoAs from human hair was performed on-line using carbon dioxide (CO2) with 5 mM ammonium formate in methanol. Optimal conditions for simultaneously extracting 17 drugs of abuse were predicted using models developed by response surface methodology. Multivariate analysis was used to optimize extraction parameters, including time (static and dynamic), modifier concentration, flow rate and extraction pressure. It was determined that a compromise between flow rate and concentration was required. Optimal extraction occurred using 15% modifier at 5.00 mL/min for an 8 minute static extraction followed by 15 minutes of dynamic flow at 2 % modifier with a 30 °C extraction vessel temperature and dual backpressures of 10.0 MPa. Significant performance differences were observed between the extraction of standard analytes spiked onto blank hair samples and extraction of a known drug user's hair where the analytes of interest were incorporated into hair growth. The known drug user's hair required multiple extractions to liberate the illicit substance from the complex hair matrix. The amount of analyte extracted during a third round of extractions was observed at double the amount extracted in the first extraction. In samples with spiked on analytes, the amount of extracted analyte decreased with each consecutive extraction. More work is needed to address the matrix effects of drugs incorporated into hair. Most methods developed for hair analysis rely upon spiked samples; however, it appears that a spiked sample versus an incorporated sample may not be comparable. Determining a better method for incorporating standards into hair will provide the basis for an improved extraction and quantification.
Download or read book Analysis with Supercritical Fluids Extraction and Chromatography written by Bernd Wenclawiak and published by Springer Science & Business Media. This book was released on 2012-12-06 with total page 225 pages. Available in PDF, EPUB and Kindle. Book excerpt: The use of supercritical fluids in analytical chemistry is still grow ing. More and more analysts are discovering the favorable advan tages for a number of applications. Especially supercritical fluid extraction (SFE) has attracted a lot of interest in recent years due to its simplicity. Supercritical fluid chromatography (SFC) has become better established and the development of this technique has been accelerated by the many applications with capillary col umns which have been published in the literature. At first SFC equipment was based on instruments commonly used for liquid chromatography, and the first commercial in struments were derived from this technology. However, capillary columns can be much more easily interfaced to gas chromatogra phy equipment especially to the detectors commonly used for Oc. Many stationary phases both for packed micro columns and capillary columns have been designed for SFC purposes extending this technology to LC and OC. The most common fluid applied in SFC and SFE is carbon dioxide. The advantages of supercritical CO , such as having dif 2 fusivity like a gas and solvating power depending on temperature and pressure, are also valid for other fluids and modified fluids. Both properties are valuable for sample extraction and extraction selectivity.
Download or read book Practical Application of Supercritical Fluid Chromatography for Pharmaceutical Research and Development written by and published by Elsevier. This book was released on 2022-12-02 with total page 434 pages. Available in PDF, EPUB and Kindle. Book excerpt: Practical Application of Supercritical Fluid Chromatography for Pharmaceutical Research and Development provides a valuable “go-to reference for many difficult-to-solve challenges using pertinent chromatographic theory, first-hand case studies, and examples provided from academic and industry experts. This text also enables professors teaching an analytical instrumental course to introduce and instruct students about one of the most sustainable and powerful separation methods currently available. While the text has broad applicability across industrial sectors, it focuses primarily on application in the pharmaceutical industry. The book is designed to allow readers to align current HPLC/UHPLC capabilities with SFC as an orthogonal tool for project specific methods in the pharmaceutical industry. It highlights where SFC falls on the spectrum of useful chromatographic tools for routine and challenging separative methods. Experienced HPLC users who are interested in developing knowledge in orthogonal separation techniques, as well as newcomers to the field of separation science, will find this text particularly useful. Chapters address where SFC may fit the analytical needs of the pharmaceutical industry and alert the readers as to where the technique will not fit. Readers will gain an understanding of how and where SFC may be applied and adapted more routinely across the pharmaceutical industry as a ‘green’ way of undertaking separation opportunities and challenges. Areas within the pharmaceutical industry include early drug discovery, process chemistry, and late stage development and manufacturing. Describes approaches to SFC column and mobile phase selection for method development for both analytical and preparative tasks Gives practical examples of how analytical SFC enables the monitoring of synthetic reactions including unstable intermediates, chiral and achiral polar reactants and products across small and large modalities Provides need-focused case studies for pharmaceutical analysts, process chemists, and contract chemistry facilities that can benefit from monitoring or purifying polar intermediates, mutagenic impurities, nitrosamines and other reaction by-products including excipients and metabolites
Download or read book Supercritical Fluid Extraction and its Use in Chromatographic Sample Preparation written by S.A. Westwood and published by Springer Science & Business Media. This book was released on 2012-12-06 with total page 180 pages. Available in PDF, EPUB and Kindle. Book excerpt: by Professor D. E. Games, Mass Spectrometry Research Unit, University College of Swansea Sample preparation can be viewed as occupying a Cinderella role in analytical science. However, the quality of sample preparation plays a key role in high In the past decade, there has been quality analysis and deserves higher stature. considerable interest in the use of supercritical fluid extraction (SFE) as an alternative to conventional procedures for the preparation of samples for ana lysis. The driving force for this development is the need for automated, sim pler, faster, non-destructive and selective methods for extraction, preferably using non-toxic extraction media which are easily disposed of. Utilization of supercritical fluids for extraction fulfils these requirements because of their unique physical chemical properties and usually low toxicity. Selectivity can be achieved by suitable selection of pressure (density), temperature and modi fier conditions which enable solvating power to be varied. The high diffusivity of supercritical fluids provides rapid sample penetration and extraction. Use of fluids with low critical temperatures enables extraction to be conducted under mild thermal conditions ensuring that thermally labile compounds do not decompose. The technique can be used off-line, and the extracts analysed by appropriate techniques, or it can be used on-line, by coupling with a variety of chromatographic techniques. These can then, if necessary, be coupled fur ther with spectroscopic techniques, such as Fourier transform infrared, ultra violet or mass spectrometry, to provide specific identification or structural information.
Download or read book Supercritical Fluid Extraction and Chromatography written by Bonnie A. Charpentier and published by . This book was released on 1988 with total page 272 pages. Available in PDF, EPUB and Kindle. Book excerpt:
Download or read book Analytical Supercritical Fluid Extraction Techniques written by E.D. Ramsey and published by Springer Science & Business Media. This book was released on 2012-12-06 with total page 449 pages. Available in PDF, EPUB and Kindle. Book excerpt: During the past decade supercritical fluid extration (SFE) has attracted considerable attention as a sample preparation procedure in analytical chemistry. The successful implementation of this technique can lead to improved sample throughput, more efficient recovery of analytes, cleaner extracts, economic replacement of halogenated solvents and a high level of automation, compared to conventional sample preparation procedures. This book provides an overview of basic principles of SFE as well as in-depth reviews of both on- and off-line SFE methods. The on-line coupling of SFE with both chromatographic and spectroscopics techniques has been the subject of a great deal of research effort and is dealt with in detail. Newer developments, such as off-line SFE of solid and liquid matrices, are starting to attract a great deal of interest, and the coverage of these areas will prove of particular value to the analytical chemist. The international team of authors has illustrated these topics with many `state-of-the-art' applications, and each chapter provides a comprehensive list of references. For the convenience of the reader, an appendix which contains pressure conversion scales and supercritical fluid carbon dioxide density tables appears at the end of the book. The volume's extensive coverage of both on-line and off-line extraction will be particularly useful to analytical chemists, in a wide range of environments, seeking to develop high quality, simple and robust SFE methods.
Download or read book Hyphenated Techniques in Supercritical Fluid Chromatography and Extraction written by K. Jinno and published by Elsevier. This book was released on 1992-07-21 with total page 345 pages. Available in PDF, EPUB and Kindle. Book excerpt: This is the first book to focus on the latest developments in hyphenated techniques using supercritical fluids. The advantages of SFC in hyphenation with various detection modes, such as FTIR, MS, MPD and ICP and others are clearly featured throughout the book. Special attention is paid to coupling of SFE with GC or SFC. In this edited volume, chapters are written by leading experts in the field. The book will be of interest to professionals in academia, as well as to those researchers working in an industrial environment, such as analytical instrumentation, pharmaceuticals, agriculture, food, petrochemicals and environmental.
Download or read book Modern Supercritical Fluid Chromatography written by Larry M. Miller and published by John Wiley & Sons. This book was released on 2019-11-06 with total page 442 pages. Available in PDF, EPUB and Kindle. Book excerpt: Explains why modern supercritical fluid chromatography (SFC) is the leading "green" analytical and purification separations technology. Modern supercritical fluid chromatography (SFC) is the leading method used to analyze and purify chiral and achiral chemical compounds, many of which are pharmaceuticals, pharmaceutical candidates, and natural products including cannabis-related compounds. This book covers current SFC instrumentation as it relates to greater robustness, better reproducibility, and increased analytical sensitivity. Modern Supercritical Fluid Chromatography: Carbon Dioxide Containing Mobile Phases covers the history, instrumentation, method development and applications of SFC. The authors provided readers with an overview of analytical and preparative SFC equipment, stationary phases, and mobile phase choices. Topics covered include: Milestones of Supercritical Fluid Chromatography; Physical Properties of Supercritical Fluids; Instrumentation for SFC; Detection in SFC; Achiral SFC Method Development; Chiral SFC Method Development; and Preparative Scale SFC. The book also includes highlights of modern applications of SFC in the final chapters—namely pharmaceuticals, consumer products, foods, polymers, petroleum-related mixtures, and cannabis—and discusses the future of SFC. Provides a clear explanation of the physical and chemical properties of supercritical fluids, which gives the reader a better understanding of the basis for improved performance in SFC compared to HPLC and GC Describes the advantages of SFC as a green alternative to HPLC and GC for the analysis of both polar, water-soluble, and non-polar analytes Details both achiral and chiral SFC method development, including modifiers, additives, the impact of temperature and pressure, and stationary phase choices Details why SFC is the premier modern preparative chromatographic technique used to purify components of mixtures for subsequent uses, both from performance and economic perspectives Covers numerous detectors, with an emphasis on SFC-MS, SFC-UV, and SFC-ELSD (evaporative light scattering detection) Describes the application of SFC to numerous high-value application areas Modern Supercritical Fluid Chromatography: Carbon Dioxide Containing Mobile Phases will be of great interest to professionals, students, and professors involved in analytical, bioanalytical, separations science, medicinal, petroleum, and environmental chemistries. It will also appeal to pharmaceutical scientists, natural-product scientists, food and consumer-products scientists, chemical engineers, and managers in these areas.
Download or read book Unified Chromatography written by J. F. Parcher and published by . This book was released on 2000 with total page 272 pages. Available in PDF, EPUB and Kindle. Book excerpt: Here, authors specializing in different branches of chromatography--including gas chromatography, supercritical fluid chromatography, and high-pressure liquid chromatography--describe their fields while drawing out connections with other branches.
Download or read book Analytical Supercritical Fluid Extraction written by Maria D. Luque de Castro and published by Springer Science & Business Media. This book was released on 2012-12-06 with total page 332 pages. Available in PDF, EPUB and Kindle. Book excerpt: Recent advances in analytical chemistry have turned it into a virtually unrecognizable science compared to a few decades ago, when it lagged behind other sciences and techniques. However, advances in analytical science have been far from universal: while innovations in instrumentation and data acquisition and processing systems have reached unprecedented levels thanks to parallel breakthroughs in computer science and chemo metrics, progress in preliminary operations has been much slower despite their importance to analytical results. Thus, such clear trends in analytical process development as automation and miniaturization have not reached preliminary operations to the same extent, even though this area is pro bably in the greatest need. Improvement in preliminary operations is thus an urgent goal of analytical chemistry on the verge of the twenty first century. Increased R&D endeavours and manufacture of commercially available automatic equipment for implementation of the wide variety of operations that separate the uncollected, unmeasured, untreated sample from the signal measuring step are thus crucial on account of the wide variability of such operations, which precludes development of all-purpose equipment, and the complexity of some, particularly relating to solid samples. Supercritical fluid extraction opens up interesting prospects in this context and is no doubt an effective approach to automatioI1 and mini aturization in the preliminary steps of the analytical process. The dramatic developments achieved in its short life are atypical in many respects.
Download or read book Supercritical Fluid Extraction and Chromatography written by Bonnie A. Charpentier and published by . This book was released on 1988-01-01 with total page 264 pages. Available in PDF, EPUB and Kindle. Book excerpt:
Download or read book Supercritical Fluid Extraction written by Larry T. Taylor and published by Wiley-Interscience. This book was released on 1996-03-13 with total page 208 pages. Available in PDF, EPUB and Kindle. Book excerpt: By encouraging a deliberate, systematic approach to supercritical fluid extraction (SFE) methods and techniques, this book enables scientists and technicians to avoid disappointing results and erroneous conclusions and develop reliable guidelines for using this versatile technology.
Download or read book Handbook of Advanced Chromatography Mass Spectrometry Techniques written by Michal Holcapek and published by Elsevier. This book was released on 2017-09-07 with total page 522 pages. Available in PDF, EPUB and Kindle. Book excerpt: Handbook of Advanced Chromatography /Mass Spectrometry Techniques is a compendium of new and advanced analytical techniques that have been developed in recent years for analysis of all types of molecules in a variety of complex matrices, from foods to fuel to pharmaceuticals and more. Focusing on areas that are becoming widely used or growing rapidly, this is a comprehensive volume that describes both theoretical and practical aspects of advanced methods for analysis. Written by authors who have published the foundational works in the field, the chapters have an emphasis on lipids, but reach a broader audience by including advanced analytical techniques applied to a variety of fields. Handbook of Advanced Chromatography / Mass Spectrometry Techniques is the ideal reference for those just entering the analytical fields covered, but also for those experienced analysts who want a combination of an overview of the techniques plus specific and pragmatic details not often covered in journal reports. The authors provide, in one source, a synthesis of knowledge that is scattered across a multitude of literature articles. The combination of pragmatic hints and tips with theoretical concepts and demonstrated applications provides both breadth and depth to produce a valuable and enduring reference manual. It is well suited for advanced analytical instrumentation students as well as for analysts seeking additional knowledge or a deeper understanding of familiar techniques. Includes UHPLC, HILIC, nano-liquid chromatographic separations, two-dimensional LC-MS (LCxLC), multiple parallel MS, 2D-GC (GCxGC) methodologies for lipids analysis, and more Contains both practical and theoretical knowledge, providing core understanding for implementing modern chromatographic and mass spectrometric techniques Presents chapters on the most popular and fastest-growing new techniques being implemented in diverse areas of research
Download or read book Analysis with Supercritical Fluids written by Bernd Wenclawiak and published by . This book was released on 1992-11-03 with total page 232 pages. Available in PDF, EPUB and Kindle. Book excerpt: The editor has brought together in a compact and readable form the new methods of analytical chemistry using supercritical fluids. The volume provides comprehensive treatment of supercritical fluid chromatography (SFC) and supercritical fluid extraction (SFE); it discusses both theory and practice. The contributions are written by leading experts in their fields with exhaustive practical experience in SFC and SFE. Special attention is given to the description of applications and thus provides the experienced analyst with invaluable information widely scattered in the literature and helps the novice to adopt these new techniques quickly in his laboratory. An addendum includes brand new literature on SFC and SFE.
Download or read book Supercritical Fluids in Chromatography and Extraction written by R. M. Smith and published by Elsevier Science Limited. This book was released on 1997 with total page 404 pages. Available in PDF, EPUB and Kindle. Book excerpt: In the mid 1980s supercritical fluid chromatography (SFC) arose with considerable fanfare as the new technique which would shortly "displace HPLC" and become the "universal separation method". After the initial hype had passed, there has still remained a significant group of applications in both chromatography and extraction for which supercritical fluids are the most suitable solvents. These form the basis of this volume, which illustrates the present state of analytical supercritical technology by a collection of review and research papers. Many publications in this field have blurred the boundaries of supercritical fluids, claiming that they filled a gap between gases and liquids and "had the properties of both". This was never true and this book seeks a more rational view of the state of application of supercritical fluids as their position in the analytical laboratory becomes clearer. These papers emphasise that future chromatographers should not be compartmentalised into "gas chromatographers" or "liquid chromatographers" but should view the field as a series of merging separation techniques. The overall emphasis is on extraction methods, usually as a sample preparation method prior to HPLC or GC analysis, but in some cases the extract is examined directly as the analytical step. This bias on extraction methods reflects the impact of supercritical fluids in the working laboratory. It is therefore an area where advances can have the maximum benefit for the user. The papers on chromatography are diverse and adventurous, covering particularly chiral chromatography and metal complex analysis, where SFC offers particular advantages over existing methods. Rather than be a separate branch of chromatography or extractions it is clear that the use of solvents above their normal conditions of temperature and pressure, up to and including the supercritical state, will continue to expand the range of analytical methods as part of an overall spectrum of solubility, polarity and volatility properties of solvents and mobile phases. This volume is an important addition to this movement and will help to redress the lack of education in the theory and practice of sample preparation which has been a great limiting factor for SFC and SFE.
Download or read book 5th International Symposium on Supercritical Fluid Chromatography and Extraction written by and published by . This book was released on 1994 with total page 314 pages. Available in PDF, EPUB and Kindle. Book excerpt:
