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The preparation of samples for instrumental analysis is the most essential and time-consuming stage of the entire analytical process; it also has the greatest impact on the analysis results. Concentrating the sample, changing its matrix, and removing interferents are often necessary. Techniques for preparing samples for analysis are constantly being developed and modified to meet new challenges, facilitate work, and enable the determination of analytes in the most comprehensive concentration range possible. This paper focuses on using metal-organic frameworks (MOFs) as sorbents in the most popular techniques for preparing liquid samples for analysis, based on liquid-solid extraction. An increase in interest in MOFs-type materials has been observed for about 20 years, mainly due to their sorption properties, resulting, among others, from the high specific surface area, tunable pore size, and the theoretically wide possibility of their modification. This paper presents certain advantages and disadvantages of the most popular sample preparation techniques based on liquid-solid extraction, the newest trends in the application of MOFs as sorbents in those techniques, and, most importantly, presents the reader with a summary, which a specific technique and MOF for the desired application. To make a tailor-made and well-informed choice as to the extraction technique.

This paper presents an overview of the more recent applications of solid-phase extraction (SPE, from January 2015 to September 2018, which have been recorded in Web of Science) in preparation of food and environmental samples. First, the history, milestones, principles, and features of different formats of SPE are discussed. In addition, miniaturization of SPE techniques and comparison of classical SPE and miniaturized SPE—called dispersive micro solid-phase extraction (D-μ-SPE)—are covered. Next, the published applications in extraction and separation of diverse organic and inorganic analytes from a variety of food and environmental samples are classified on the basis of their sorbents including layered double hydroxide, metal organic frameworks, carbon nanotube-based sorbents, graphene-based sorbents, β-cyclodextrin-based sorbents, dendrimer-based sorbents, molecular or ion recognition sorbents, and restricted access materials. Finally, the future trends in this area are discussed.

This review presents a comprehensive update on the state-of-the-art of nanometer-sized materials in solid-phase extraction (SPE) of trace elements followed by atomic-spectrometry detection. Zero-dimensional nanomaterials (fullerene), one-dimensional nanomaterials (carbon nanotubes, inorganic nanotubes, and nanowires), two-dimensional nanomaterials (nanofibers), and three-dimensional nanomaterials (nanoparticles, mesoporous nanoparticles, magnetic nanoparticles, and dendrimers) for SPE are discussed, with their application for trace-element analysis and their speciation in different matrices. A variety of other novel SPE sorbents, including restricted-access sorbents, ion-imprinted polymers, and metal–organic frameworks, are also discussed, although their applications in trace-element analysis are relatively scarce so far. Graphical Abstract Nanometer-sized materials for solid-phaseextraction of trace elements and their species

There are a lot of review papers of sample pretreatment, but the comprehensive review on pipette-tip solid-phase extraction (PT-SPE) is lacking. This review (133 references) is mainly devoted to the development of different types of micro- and nanosorbent-based PT-SPE, including silica materials, carbon materials, organic polymers, molecularly imprinted polymers, and metal-organic frameworks. Each section mainly introduces and discusses the preparation methods, advantages and limitations of adsorbents, and their applications to environmental, biological, and food samples. This review also demonstrates the advantages of PT-SPE like convenience, speed, less organic solvent, and low cost. Finally, the future application and development trend of PT-SPE are prospected. Graphical abstract

AbstractThis minireview is dedicated to the discussion of analytical methods based on magnetic solid-phase extraction for the investigation of different analyte classes in complex matrices. Magnetic solid-phase extraction represents one of the most exploited approaches for sample preparation, which benefits from the development of new materials and from the coupling with other purification and clean-up strategies. New materials are continuously described for the isolation and enrichment of a variety of compounds, from small molecules to biologic macromolecules. Such magnetic materials developed for magnetic solid-phase extraction are discussed in this minireview, spanning across different types of materials, from the more traditional magnetic nanoparticles functionalized with polymers, to molecularly imprinted polymers, but also graphene, carbon nanotubes, graphitized carbon black, metal organic frameworks, covalent organic frameworks, composite materials, biopolymers (polydopamine, chitosan), materials from wastes and natural products and the newly introduced knitting aromatic polymers. The magnetic solid-phase extraction methods are collected from the recent literature and organized in sections based on the target analyte classes, which include drugs, endocrine-disrupting compounds, pesticides, polycyclic aromatic hydrocarbons, metals, toxins, peptides, proteins, metabolites and a final chapter dedicated to applications to other common pollutants, contaminants and multiresidue methods. A selection of recent applications and variations of the traditional magnetic solid-phase extraction protocols is discussed for food, environmental and biologic matrices. Finally, the compliance of magnetic solid-phase extraction with the principles of green analytical chemistry is also briefly discussed, with recent examples, indicating the use of waste or sustainable materials, development of green material preparations and reduction of organic solvents as the main strategies for future development of environmentally friendly magnetic solid-phase extraction methods.Graphical Abstract

Analysis of fatty acids (FA) in food and biological samples such as blood is indispensable in modern life sciences. We developed a rapid, sensitive and comprehensive method for the quantification of 41 saturated and unsaturated fatty acids by means of LC-MS. Optimized chromatographic separation of isobaric analytes was carried out on a C8 reversed phase analytical column (100 × 2.1 mm, 2.6 μm core–shell particle) with a total run time of 15 min with back pressure lower than 300 bar. On an old triple quadrupole instrument (3200, AB Sciex), pseudo selected reaction monitoring mode was used for quantification of the poorly fragmenting FA, yielding limits of detection of 5–100 nM. Sample preparation was carried out by removal of phospholipids and triglycerides by solid-phase extraction (non-esterified fatty acids in oils) or saponification in iso-propanol (fatty acyls). This is not only a rapid strategy for quantification of fatty acyls, but allows the direct combination with the LC-MS-based analysis of fatty acid oxidation products (eicosanoids and other oxylipins) from the same sample. The concentrations of fatty acyls determined by means of LC-MS were consistent with those from GC-FID analysis demonstrating the accuracy of the developed method. Moreover, the method shows high precisions with a low intra-day (≤ 10% for almost all fatty acids in plasma and ≤ 15% in oils) and inter-day as well as inter-operator variability (< 20%). The method was successfully applied on human plasma and edible oils. The possibility to quantify non-esterified fatty acids in samples containing an excess of triacylglycerols and phospholipids is a major strength of the described approach allowing to gain new insights in the composition of biological samples.

Dispersive solid-phase extraction ( DSPE ) and magnetic solid-phase extraction ( MSPE ) are methods of solid-phase sorption preconcentration. Compared to classical solid-phase extraction, these methods have a number of advantages, such as reduced consumption of sorbents and solvents, extraction time, and cost of analysis. The popularity of the method among the analysts is evidenced by the large number of reviews we have summarized in this publication. Information is systematized on different versions of these methods, differing in the way the preconcentration process is carried out, the nature of the sorbents used, and their combination with methods for the subsequent determination of the preconcentrated substances; examples of using DSPE and MSPE for the separation of organic compounds in the analysis of environmental samples, food products and biological fluids are given.

The present paper reports a detailed study that is based on the monitoring of naproxen, ibuprofen, and diclofenac in Mbokodweni River and wastewater treatment plants (WWTPs) located around the city of Durban in KwaZulu-Natal Province of South Africa. Target compounds were extracted from water samples using a multi-template molecularly imprinted solid-phase extraction prior to separation and quantification on a high-performance liquid chromatography equipped with photo diode array detector. The analytical method yielded the detection limits of 0.15, 1.00, and 0.63 μg/L for naproxen, ibuprofen, and diclofenac, respectively. Solid-phase extraction method was evaluated for its performance using deionized water samples that were spiked with 5 and 50 μg/L of target compounds. Recoveries were greater than 80% for all target compounds with RSD values in the range of 4.1 to 10%. Target compounds were detected in most wastewater and river water samples with ibuprofen being the most frequently detected pharmaceutical. Maximum concentrations detected in river water for naproxen, ibuprofen, and diclofenac were 6.84, 19.2, and 9.69 μg/L, respectively. The concentrations of target compounds found in effluent and river water samples compared well with some studies. The analytical method employed in this work is fast, selective, sensitive, and affordable; therefore, it can be used routinely to evaluate the occurrence of acidic pharmaceuticals in South African water resources.

A simple and robust analytical method for the determination of perfluorinated carboxylic acids (PFCAs) with C 2 to C 8 chains, based on solid-phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS), was developed, validated and applied to tap water, groundwater and surface water. Two stationary phases for LC (Obelisc N and Kinetex C 18 ) and two materials with weak anion-exchange properties for SPE (Strata X-AW and Oasis WAX) were evaluated. Robust separation and retention was achieved with the reversed phase column and an acidic eluent. Quantitative extraction recoveries were generally achieved for PFCAs with C > 3, but extraction efficiencies were different for the two shortest chained analytes: 36 to 114% of perfluoropropanoate (PFPrA) and 14 to 99% of trifluoroacetate (TFA) were recovered with Strata X-AW, while 93 to 103% of PFPrA and 40 to 103% of TFA were recovered with Oasis WAX. The sample pH was identified as a key parameter in the extraction process. One-step elution-filtration was introduced in the workflow, in order to remove sorbent particles and minimise sample preparation steps. Validation resulted in limits of quantification for all PFCAs between 0.6 and 26 ng/L. Precision was between 0.7 and 15% and mean recoveries ranged from 83 to 107%. In groundwater samples from sites impacted by per- and polyfluoroalkyl substances (PFASs), PFCA concentrations ranged from 0.056 to 2.2 μg/L. TFA and perfluorooctanoate were the predominant analytes. TFA, however, revealed a more ubiquitous occurrence and was found in concentrations between 0.045 and 17 μg/L in drinking water, groundwater and surface water, which were not impacted by PFASs.

An automated on-line solid-phase extraction (SPE) following liquid chromatography tandem mass spectrometry was established for the fast determination of plant growth regulator residues in soybean sprout and mung bean sprout. The crude extracted specimens were directly purified on a poly (2-(dimethylamino) ethyl methacrylate-co-ethylene dimethacrylate) monolithic column which was well-defined as the on-line SPE adsorbent. Under the optimized conditions, the developed method gave the linear range of 0.3–50 ng/mL for gibberellin and 2,4-dichlorophenoxyacetic acid, 0.2–50 ng/mL for 4-chlorophenoxyacetic acid, and 0.5–50 ng/mL for 1-naphthaleneacetic acid (r ≥ 0.998). The detection limits (S/N = 3) ranged from 1.0 to 2.5 μg/kg and the recoveries for spiked soybean sprout samples were in the range of 75.0–93.3%. Besides, the total time for one analysis was 16 min. The reusability of the monolith was up to 600 extractions. The proposed process facilitated fully automated SPE and accurate determination in one step with rapidity, simplicity, and reliability.