Trends In Sample Preparation Research Articles

Reflecting on the Influence of the Current State of Sample Preparation on GC, Part 2: Techniques

Recently, we examined major trends in sample preparation and how they relate to gas chromatography (GC), based on a 2023 user survey by LCGC International. In Part 2 of LCGC’s survey of sample preparation users, the prevalence of sample preparation techniques, from the most common, such as weighing, to the most complex, such as online extractions, was discussed. In this installment, we examine trends in the use of sample preparation techniques through the lens of instrumental analysis by gas chromatography (GC) and GC–mass spectrometry (GC–MS). We see that, although common and classical techniques, such as filtration and centrifugation, are still generally the most widely used, newer techniques that allow automation, simplification of analysis steps, and green analysis are gaining traction.

Trends in Sample Preparation, Part II: Sample Considerations and Techniques

In the October 2023 installment of “Sample Prep Perspectives,” we reported results obtained from a survey on sample preparation techniques, and compared those to results from previous surveys. The results uncovered trends in the field over the last generation and their impact in areas such as which technologies are currently being used, sample types, and sample load. This installment will continue our look at the sample preparation survey, focusing on sample sizes, laboratory techniques used, automation, the use of solid-phase extraction (SPE) devices (cartridges, disks, plates, tips), SPE chemistries and selection criteria, and problems encountered in SPE.

Chemical Trends in Sample Preparation for Nucleic Acid Amplification Testing (NAAT): A Review.

Nucleic acid amplification testing facilitates the detection of disease through specific genomic sequences and is attractive for point-of-need testing (PONT); in particular, the early detection of microorganisms can alert early response systems to protect the public and ecosystems from widespread outbreaks of biological threats, including infectious diseases. Prior to nucleic acid amplification and detection, extensive sample preparation techniques are required to free nucleic acids and extract them from the sample matrix. Sample preparation is critical to maximize the sensitivity and reliability of testing. As the enzymatic amplification reactions can be sensitive to inhibitors from the sample, as well as from chemicals used for lysis and extraction, avoiding inhibition is a significant challenge, particularly when minimising liquid handling steps is also desirable for the translation of the assay to a portable format for PONT. The reagents used in sample preparation for nucleic acid testing, covering lysis and NA extraction (binding, washing, and elution), are reviewed with a focus on their suitability for use in PONT.

Trends in Sample Preparation, Part I: Current State of the Field

This installment of “Sample Prep Perspectives” reports the results obtained from a new survey on sample preparation techniques. This is our first survey since 2016 and its findings are compared with the results of previous surveys dating from 1991. Results involve undercover trends in the field over the last generation and their impact. The survey investigated trends in areas such as which technologies are currently being used, sample loads, sample sizes, automation, the use of solid-phase extraction (SPE) devices (cartridges, disks, plates, tips), SPE chemistries, selection criteria, and problems encountered. Respondents were also asked about sample preparation technologies on the horizon.

Application of Single Particle ICP-MS for the Determination of Inorganic Nanoparticles in Food Additives and Food: A Short Review.

Due to enhanced properties at the nanoscale, nanomaterials (NMs) have been incorporated into foods, food additives, and food packaging materials. Knowledge gaps related to (but not limited to) fate, transport, bioaccumulation, and toxicity of nanomaterials have led to an expedient need to expand research efforts in the food research field. While classical techniques can provide information on dilute suspensions, these techniques sample a low throughput of nanoparticles (NPs) in the suspension and are limited in the range of the measurement metrics so orthogonal techniques must be used in tandem to fill in measurement gaps. New and innovative characterization techniques have been developed and optimized for employment in food nano-characterization. Single particle inductively coupled plasma mass spectrometry, a high-throughput nanoparticle characterization technique capable of providing vital measurands of NP-containing samples such as size distribution, number concentration, and NP evolution has been employed as a characterization technique in food research since its inception. Here, we offer a short, critical review highlighting existing studies that employ spICP-MS in food research with a particular focus on method validation and trends in sample preparation and spICP-MS methodology. Importantly, we identify and address areas in research as well as offer insights into yet to be addressed knowledge gaps in methodology.

Exploring the Versatility of LC-ESI-MS/MS: Fundamentals, Applications, and Advancements at the Forefront of Analytical Science

Abstract: This comprehensive review paper focuses on LC-ESI-MS/MS, a powerful analytical technique widely used in various scientific disciplines. It begins by explaining the working mechanisms and components of LC-ESI-MS/MS highlighting advancements in sensitivity, resolution, speed and data analysis. This paper explores the diverse applications of LC-ESI-MS/MS in pharmaceutical analysis, environmental analysis, metabolomics, and proteomics, discussing its advantages and limitations in each area. The review also emphasizes the integration of LC-ESI-MS/MS with other techniques like GC-MS, CE-MS, and MALDI-MS, showcasing their combined effects and enhanced capabilities. It presents recent developments and innovations in LC-ESI-MS/MS technology including improvements in sensitivity, resolution and data analysis. This paper discusses emerging trends in sample preparation, ionization methods, chromatographic columns, and mass spectrometry detectors. Addressing the challenges and limitations, the review identifies potential areas for improvement and future research directions. It emphasizes the untapped potential of LC-ESI-MS/MS in advancing scientific knowledge and solving complex analytical problems, calling for further collaboration and research in the field. In conclusion, this review paper provides a comprehensive overview of LCESI-MS/MS, emphasizing its fundamental principles, applications, recent innovations, and future perspectives. The findings underscore the significance of LC-ESI-MS/MS in modern science and its potential for further advancements.

Enhanced multi-stir bar sorptive extraction for wine analysis: Alteration in headspace mode

Multi-stir bar sorptive extraction (multi-SBSE) represents a viable alternative for recent trends in sample preparation based on a combination of extraction techniques. In this case, increased amount of sorbent and its extended polarity range could advance quality of experimental data obtained in foodomics or metabolomics investigations. With this in mind, it was developed multi-SBSE procedure suitable for authentication of botrytized wine produced in different countries of Tokaj wine region. A design of headspace mode of multi-SBSE was modified to provide additional agitation of a stir bar. An expanded profile of wine samples was obtained with the application of EG-Silicone and PDMS coated stir bars in headspace and direction immersion mode, respectively. Multivariate optimization based on central composite design was selected to determine the influence of various experimental parameters, including extraction temperature enhancing headspace extraction. In our case, proper description of the optimization results required application of a third-order polynomial model, which highlighted dominant influence of salt addition for extraction in both modes. Due to a large number of extracted compounds, comprehensive two-dimensional gas chromatography (GC × GC) was used for assessment of wine samples. Such approach allows reveleaing the presence of sulphur containing compounds, diols, ketone derivatives and methoxybenzenes linking a specific geographical origin. At the same time, the results obtained for compounds common for all the samples were processed with principal component analysis (PCA). Considerable progress for discrimination of the botrytized wines was mainly achieved with combined data from EG-Silicone and PDMS extraction.

Recent advances and trends in sample preparation and chemical modification for glycan analysis

Growing significance of glycosylation in protein functions has accelerated the development of methodologies for detection, identification, and characterization of protein glycosylation. In the past decade, glycobiology research has been advanced by innovative techniques with further progression in the post-genome era. Although significant technical progress has been made in terms of analytical throughput, comprehensiveness, and sensitivity, most methods for glycosylation analysis still require laborious and time-consuming sample preparation tasks. Additionally, sample preparation methods that are focused on specific glycan(s) require an in-depth understanding of various issues in glycobiology. In this review, modern sample preparation and chemical modification methods for the structural and quantitative glycan analyses together with the challenges and advantages of recent sample preparation methods are summarized. The techniques presented herein can facilitate the exploration of biomarkers, understanding of unknown glycan functions, and development of biopharmaceuticals.

Recent advances in column switching high-performance liquid chromatography for bioanalysis

Bioanalysis is a relevant area of analytical chemistry for clinical studies. Biological samples are complex and diverse, so sample preparation represents a challenge when chromatographic methods are developed. According to the principles of green analytical chemistry (GAC), recent trends in sample preparation include miniaturization, automation (online coupling to the analytical instrument), and high-throughput performance. In this context, column switching liquid chromatography stands out as a multidimensional chromatographic method in which an extraction column is directly coupled to high-performance liquid chromatography (HPLC) systems. This online method consists of two steps and involves two columns, the extraction and the chromatographic columns. In the former column, the analytes are isolated from the sample and preconcentrated; in the latter column, the analytes are separated. Online systems improve the sensitivity and accuracy of analytical methods, consume lower amounts of organic solvents, and minimize sample handling. This review summarizes state-of-the-art column switching liquid chromatography and focuses on selective stationary phases for preconcentration of analytes (first dimension), including reversed phases, monolithic phases, restricted access materials (RAMs), and molecularly imprinted polymers (MIP). Principles, instrumental aspects, applications in bioanalysis, and future trends in column switching liquid chromatography are also discussed.

Sustainable green solvents for microextraction techniques: Recent developments and applications

The development and application of alternative green solvents in analytical techniques consist of trends in sample preparation, since this subject represents an important step toward sustainability in experimental procedures. This review is focused on the main theoretical aspects related to deep eutectic solvents (DES), switchable hydrophilicity solvents (SHS) and supramolecular solvents (SUPRAS). Recent applications are highlighted, particularly for the extraction of different analytes from environmental, biological and food matrices. Moreover, novel configurations are emphasized, aiming for efficient, automated and high-throughput procedures. This review also provides some critical points regarding the use of these solvents and their green aspects.

Benzene, toluene, ethylbenzene, and xylene: Current analytical techniques and approaches for biological monitoring

Abstract Benzene, toluene, ethylbenzene, and xylene (BTEX) are a group of volatile organic compounds that human exposure to them may result in the development of some diseases, including cancer. Biological monitoring plays an important role in exposure assessment of workers occupationally exposed to chemicals. Several metabolites have been proposed for biological monitoring of individuals who are exposed to BTEX. There are a variety of extraction methods and analytical techniques for the determination of unmetabolized BTEX in exhaled air and their urinary metabolites. The present study aimed to summarize and review the toxicokinetics of BTEX and sample preparation and analytical methods for their measurement. Metabolites of BTEX are discussed to find out reliable ones for biological monitoring of workers exposed to these chemicals. In addition, analytical methods for unmetabolized BTEX in exhaled air and their metabolites were reviewed in order to obtain a comparison between them in term of selectivity, sensitivity, simplicity, time, environmental-friendly and cost. Given the recent trends in sample preparation, including miniaturization, automation, high-throughput performance, and on-line coupling with analytical instrument, it seems that microextraction techniques, especially microextraction by packed sorbents are the methods of choice for the determination of the BTEX metabolites.

Advances on preparation methods for mycotoxins in food samples

Mycotoxins are toxic secondary metabolites with low molecular weight that are produced by fungus under certain environmental conditions. Mycotoxins are of various types and show strong toxicity. They can enter the food chain directly or indirectly, causing diseases or even death to humans and other animals. It is very crucial to use efficient sample preparations to realize the separation and enrichment of targets before analysis due to diversified foods, complex matrix and low concentrations in real samples. In this paper, preparation methods using new separation media, such as liquid phase extraction, solid phase extraction, magnetic solid phase extraction, ultrasound-assisted extraction, microwave-assisted extraction, immunoaffinity chromatography and QuEChERS are introduced. In addition, future trends in sample preparation for food mycotoxins are prospected.

New Advanced Materials and Sorbent-Based Microextraction Techniques as Strategies in Sample Preparation to Improve the Determination of Natural Toxins in Food Samples.

Natural toxins are chemical substances that are not toxic to the organisms that produce them, but which can be a potential risk to human health when ingested through food. Thus, it is of high interest to develop advanced analytical methodologies to control the occurrence of these compounds in food products. However, the analysis of food samples is a challenging task because of the high complexity of these matrices, which hinders the extraction and detection of the analytes. Therefore, sample preparation is a crucial step in food analysis to achieve adequate isolation and/or preconcentration of analytes and provide suitable clean-up of matrix interferences prior to instrumental analysis. Current trends in sample preparation involve moving towards “greener” approaches by scaling down analytical operations, miniaturizing the instruments and integrating new advanced materials as sorbents. The combination of these new materials with sorbent-based microextraction technologies enables the development of high-throughput sample preparation methods, which improve conventional extraction and clean-up procedures. This review gives an overview of the most relevant analytical strategies employed for sorbent-based microextraction of natural toxins of exogenous origin from food, as well as the improvements achieved in food sample preparation by the integration of new advanced materials as sorbents in these microextraction techniques, giving some relevant examples from the last ten years. Challenges and expected future trends are also discussed.

Microextraction approaches for bioanalytical applications: An overview

Biological samples are usually complex matrices due to the presence of proteins, salts and a variety of organic compounds with chemical properties similar to those of the target analytes. Therefore, sample preparation is often mandatory in order to isolate the analytes from troublesome matrices before instrumental analysis. Because the number of samples in drug development, doping analysis, forensic science, toxicological analysis, and preclinical and clinical assays is steadily increasing, novel high throughput sample preparation approaches are calling for. The key factors in this development are the miniaturization and the automation of the sample preparation approaches so as to cope with most of the twelve principles of green chemistry. In this review, recent trends in sample preparation and novel strategies will be discussed in detail with particular focus on sorptive and liquid-phase microextraction in bioanalysis. The actual applicability of selective sorbents is also considered. Additionally, the role of 3D printing in microextraction for bioanalytical methods will be pinpointed.

Trends in Sample Preparation for the HPLC Determination of Penicillins in Biofluids

Trends in Sample Preparation for the HPLC Determination of Penicillins in Biofluids

Current trends in sample preparation for cosmetic analysis.

The widespread applications of cosmetics in modern life make their analysis particularly important from a safety point of view. There is a wide variety of restricted ingredients and prohibited substances that primarily influence the safety of cosmetics. Sample preparation for cosmetic analysis is a crucial step as the complex matrices may seriously interfere with the determination of target analytes. In this review, some new developments (2010-2016) in sample preparation techniques for cosmetic analysis, including liquid-phase microextraction, solid-phase microextraction, matrix solid-phase dispersion, pressurized liquid extraction, cloud point extraction, ultrasound-assisted extraction, and microwave digestion, are presented. Furthermore, the research and progress in sample preparation techniques and their applications in the separation and purification of allowed ingredients and prohibited substances are reviewed.

Recent Trends in Sample Preparation and Liquid Chromatography/Mass Spectrometry for Pesticide Residue Analysis in Food and Related Matrixes.

A rising interest by consumers and various governmental organizations towards the quality of food has been continuously observed. Pesticide residue analysis has a significant role in assessing food safety and quality. This article reviews the new analytical approaches for efficient extraction and reliable identification and quantification of pesticides in foodstuffs and related matrixes. Emphasis is given to the new materials used for effective extract purification. We discuss the potential and pitfalls of the different LC/MS approaches, including application of high resolution mass spectrometry in the area of pesticide residue analysis. Untargeted and retrospective screening is outlined, highlighting prospects and achievements as well as its major drawbacks.

Cardiovascular drug determination in bioanalysis: an update.

The great impact of cardiovascular diseases in human health has led to the development of a huge number of drugs and therapies to improve the treatment of these diseases. Cardiovascular drug analysis in biological fluids constitutes an important challenge for analytical scientists. There is a clear need for reliable methods to carry out both qualitative and quantitative analysis in a short time of analysis. Different problems such as drug monitoring, analysis of metabolites, study of drugs interactions, drugs residues or degradation products, chiral separation, and screening and confirmation of drugs of abuse in doping control must be solved. New trends in sample preparation, instrumental and column technology advances in LC and innovations in MS are described in this work.

Microextraction by packed sorbent: an emerging, selective and high-throughput extraction technique in bioanalysis.

Sample preparation is an important analytical step regarding the isolation and concentration of desired components from complex matrices and greatly influences their reliable and accurate analysis and data quality. It is the most labor-intensive and error-prone process in analytical methodology and, therefore, may influence the analytical performance of the target analytes quantification. Many conventional sample preparation methods are relatively complicated, involving time-consuming procedures and requiring large volumes of organic solvents. Recent trends in sample preparation include miniaturization, automation, high-throughput performance, on-line coupling with analytical instruments and low-cost operation through extremely low volume or no solvent consumption. Micro-extraction techniques, such as micro-extraction by packed sorbent (MEPS), have these advantages over the traditional techniques. This paper gives an overview of MEPS technique, including the role of sample preparation in bioanalysis, the MEPS description namely MEPS formats (on- and off-line), sorbents, experimental and protocols, factors that affect the MEPS performance, and the major advantages and limitations of MEPS compared with other sample preparation techniques. We also summarize MEPS recent applications in bioanalysis.

Multi-target screening of biological samples using LC-MS/MS: focus on chromatographic innovations.

Multi-target screening of biological fluids is a key tool in clinical and forensic toxicology. A complete toxicological analysis encompasses the sample preparation, the chromatographic separation and the detection. The present review briefly covers the new trends in sample preparation and detection and mainly focuses on the chromatographic stage, since a lot of technical improvements have been proposed over the last years. Among them, columns packed with sub-2μm fully porous particles and sub-3μm core-shell particles allow for significant improvements of resolution and higher throughput. Even if reversed-phase LC remains the most widely used chromatographic mode for toxicological screening, hydrophilic interaction chromatography and supercritical fluid chromatography appear as promising alternatives for attaining orthogonal selectivity, retention of polar compounds, and enhanced MS sensitivity.