Search

The unfavourable impacts of organic solvents on the environmental and human health have increasingly drawn the attention of scientists and technologists for a long run solution. Recently, ionic liquids (ILs) have emerged as an environmentally friendly alternative of choice to reduce the use of organic solvents. This review covers the data of literature published from 2011 to 2021. Literature search was performed for the relevant journal articles including books, and book chapters using the keywords of 'ionic liquid', 'extraction', 'medicinal plants', 'essential oil', 'waste water treatment', 'green extraction technology' and combination of them. ILs are designer solvents due to their modifiable properties according to the application conditions. Therefore, this review highlights the application of ILs in the extraction and purification of bioactive compounds (glycosides, phenolic compounds, flavonoids, alkaloids and others) and essential oils from plant materials. This includes the use of ILs in the microwave and ultrasound assisted extractions, as well as solid phase extraction. Previous studies reported about 20–35 % of increment in the yield of bioactive compounds with the use of ILs. • Literature review on articles reporting ionic liquids and their applications. • The applications of ionic liquids in the extraction of bioactive compounds and essential oils. • Ionic liquids as green solvent in various conventional and advanced extraction techniques. [ABSTRACT FROM AUTHOR]

MXenes, an emerging category of 2D materials, have attracted significant attention of scientific community since their discovery in 2011. These materials show exciting properties such as exceptional surface functionalities, layered structures, hydrophilicity, tunable intercalated moieties, and high electrical conductivities. To date, MXene-based materials have been widely used in gas sensing, energy storage/conversion, photocatalysis, biomedical devices, electrochemical sensors and biosensors, electromagnetic shielding, and removal of organic and inorganic pollutants from different media. Recently, there has been a growing interest in utilizing these materials in analytical extraction techniques such as solid phase microextraction, dispersive solid phase extraction, magnetic solid phase extraction, and others. This review aims to provide a concise overview of this emerging trend to the analytical community. It discusses the synthesis of MXene-based materials for extraction applications, different modifications to improve their affinity towards target molecules, and their application as a sorbent for environmental, food, and biological samples. [Display omitted] • The synthesis and modification of MXene-based materials prepared for analytical extractions is discussed. • The applications of MXene-based materials in extraction of analytes from samples of different compositions are reviewed. • Different extraction and microextraction techniques that employ MXenes-based sorbents are discussed. • Modifications and functionalization that improve the interaction between MXene-based materials and analytes are discussed. • The potential research gaps and future research dimensions are briefly highlighted. [ABSTRACT FROM AUTHOR]

• Proposed naphthylamine microwave-assisted derivatization was fast and efficient. • Polypropylene membrane MMSPE devices are promising for aromatic amine extraction. • Obtained devices are viable low cost alternatives for aromatic amine biomonitoring. • This is the first use polypropylene membrane MMSPE devices with biological fluids. Exposure to tobacco smoke is highly correlated to the incidence of different types of cancer due to various carcinogenic compounds present in such smoke. Aromatic amines, such as 1-naphthylamine (1-NA) and 2-naphthylamine (2-NA), are produced in tobacco burning and are linked to bladder cancer. Miniaturized solid phase extraction techniques, such as microporous membrane solid phase extraction (MMSPE), have shown potential for the extraction of aromatic compounds. In this study, a bioanalytical method for the determination of 1-NA and 2-NA in human urine was developed using polypropylene microporous membranes as a sorptive phase for MMSPE. Urine samples were hydrolyzed with HCl for 1 h at 80 °C, after which pH was adjusted to 10. Ultrasound-assisted MMSPE procedure was optimized by factorial design as follows. To each sample, 750 µL of methanol was added, and ultrasound-assisted MMSPE was conducted for 1 h with four devices containing seven 2 mm polypropylene membrane segments. After extraction, the segments were transferred to 400 µL of hexane, and desorption was conducted for 30 min. Extracts were submitted to a simple and fast microwave-assisted derivatization procedure, by the addition of 10 µL of PFPA and heating at 480 W for 3 min, followed by clean-up with phosphate buffer pH 8.0 and GC–MS/MS analysis. Adequate linearity was obtained for both analytes in a range from 25 to 500 µg L −1, while the multiple reaction monitoring approach provided satisfactory selectivity and specificity. Intra-day (n = 6) and inter-day (n = 5) precision and accuracy were satisfactory, below 15 % and between 85 and 115 %, respectively. Recovery rates found were 91.9 and 58.4 % for 1-NA and 2-NA, respectively, with adequate precision. 1-NA was found in first-hand smokers' urine samples in a concentration range from 20.98 to 89.09 µg in 24 h, while it could be detected in second-hand smoker's urine samples, and 2-NA detected in all first and second-hand smokers' urine samples. The proposed method expands the applicability of low cost MMSPE devices to aromatic amines and biological fluids. [ABSTRACT FROM AUTHOR]

Toxicodendron vernicifluum bark has been used for many years as a component in foods and as a traditional herbal medication. Unfortunately, the presence of urushiols, which induce allergies, limits its application. This study used a vortex-blending matrix solid-phase dispersion microextraction technique to extract urushiols from Toxicodendron vernicifluum bark. HPLC was used to evaluate the amounts of the extracted urushiols (15:0, 15:1, 15:2, and 15:3). The modified magnetic adsorbent was prepared through an in situ coprecipitation method and characterized using a variety of techniques. The optimized extraction conditions are as follows: using magnetic Zeolite Socony Mobil-Five as an adsorbent, a 1:2 sample/adsorbent ratio, 2.5 min of vortex-blending time, 4 mL of 0.1% (V/V) trifluoroacetic acid-methanol as the elution solvent and 8 min of ultrasound time. There was good linearity and high repeatability in the method. Furthermore, the limits of detection for the urushiols ranged from 0.20 to 0.50 μg/mL. Under the optimized conditions, 50 compounds were identified by ultra high performance liquid chromatography and quadrupole time-of-flight mass spectrometry. These compounds included 8 phenolic acids, 9 monomeric urushiols, 11 urushiol dimers, 10 other components, and 11 flavonoids. The suggested approach, which has the advantages of few stages and high extraction efficiency over existing extraction procedures, is a potentially useful method for obtaining and evaluating urushiols in raw materials or extracts. [Display omitted] • A vortex mixed matrix solid-phase dispersion (VB-MSPD) was developed to analyse urushiols. • Magnetic Zeolite Socony Mobil-Five is the most effective adsorbent for extracting urushiols. • Through focused UPLC-Q-TOF/MS analysis, 9 urushiols and 11 urushiol dimers were identified. • It is a practical method for determining urushiols in raw materials or extracts. [ABSTRACT FROM AUTHOR]

Conventional chemical extraction methods may lead to overestimate or underestimate bioaccessibility due to their inability to provide realistic kinetic information regarding PAHs in soils. In this study, we propose the use of magnetic solid phase extraction (MSPE) technique for assessing the bioaccessibility of PAHs in the soil-earthworm system. Firstly, a novel polydopamine-coated magnetic core-shell microspheres (Fe 3 O 4 –C 16 @ PDA) was developed by a one-pot sol-gel and self-polymerization method. The PDA coatings not only enhance the hydrophilicity of material surfaces but also exhibit excellent biocompatibility. The maximum adsorption capacity of Fe 3 O 4 –C 16 @ PDA for 16 PAHs was 52.72 mg g−1, indicating that the proposed material fulfills the assessment requirements for highly contaminated soil. To compare the measurement of PAHs and their uptake by earthworms (Eisenia fetida), experiments were conducted using four different soils with varying properties. The desorption kinetics data obtained from these experiments demonstrated that the capability of the MSPE in accurately predicting the bioavailable portions of PAHs. After a 28-day exposure, the best predictor of bioavailable PAHs in earthworms was MSPE method exhibited the highest correlation coefficient (R2 > 0.90), and its slopes in the four soils were 0.972, 0.961, 1.012, and 0.962, respectively, all close to 1. These results demonstrate that the MSPE method successfully mimics the conditions encountered in soil-earthworm systems and effectively assess bioaccessibility of PAHs in soils. [Display omitted] • A novel polydopamine-coated magnetic core-shell microspheres was developed. • The improved hydrophilicity provided by the PDA polydopamine facilitates the separation of magnetic adsorbents from soil. • MSPE method can accurately predict the bioaccumulation of PAHs by earthworms in different soils types. • Conventional approaches are not suitable for soils with high TOC content. [ABSTRACT FROM AUTHOR]

The main direction of the development of analytical chemistry is the constant pursuit of simplification, shortening and the introduction of ecological solutions to each stage of analytical procedures. For years, extractants/sorbents based on natural compounds have been very popular, which is in line with the recent trend of using green analytical chemistry. This review will discuss the usage of biopolymers such as chitosan, agarose, alginate, cellulose, starch and cyclodextrin in various solid-phase (micro)extraction techniques. The above-mentioned compounds were initially used directly, but much more often they were subjected to surface modification using chemical methods or were proposed as composites with previously known sorbents such as carbon nanotubes, metal-organic frameworks, molecularly imprinted polymers or graphene oxide. [Display omitted] • Biopolymers such as chitosan, agarose/alginate, cellulose, starch have been described. • The biopolymers as composites with popular materials have been presented. • The use of biopolymers-based materials in (micro)extractions have been reviewed. [ABSTRACT FROM AUTHOR]

[Display omitted] • A new QuEChERS-MISPE technique for isolation of pesticides has been developed. • The technique was optimized using batch studies to understand adsorption process for DDTs. • Technique experiences less matrix effects and better sensitivity than QuEChERS-dSPE. • The technique was used to detect trace levels of DDTs in open market vegetables. • Evidence shows absorption of DDT and its derivatives in vegetables in South Africa. The current study synthesized a molecularly imprinted polymer, combined it with the QuEChERS method to form a new hybrid technique, the QuEChERS-MISPE as an alternative to the QuEChERS-dSPE for analysis of DDTs as model pesticides. Batch studies confirmed that the binding of the DDTs to the MIP cavities formed a monolayer formation through chemisorption resulting in an adsorption capacity of 429 ng g−1. A study of matrix effects indicated signal suppression for both techniques. However, the new QuEChERS-MISPE technique is less affected by matrix effects, has better sensitivity and recoveries compared to the conventional QuEChERS-dSPE technique. Application of the new QuEChERS-MISPE technique detected trace levels of DDTs in vegetables in South Africa. However, a health risk assessment indicated that potential risks for consumers was minimal. Although the risk is minimal, the detection of DDTs in vegetables in South Africa should be a concern and more constant monitoring is required. [ABSTRACT FROM AUTHOR]

[Display omitted] • Applications of MOFs as sorbents in extraction techniques were investigated. • Advantages, limitations, and modifications of extraction methods using MOFs were analyzed. • Coating techniques for prepared SPME fibers with MOFs as sorbents were evaluated. • Functionalization of MOF as sorbents and its impact on extraction procedures were examined. • Strategies to overcome MOF limitations and advance their use in extraction methods were addressed. Solid phase extraction (SPE) and solid phase microextraction (SPME) are widely used sample preparation techniques that selectively extract target analytes from complex sample matrices using sorbents. The choice of sorbent is crucial for determining extraction selectivity and efficiency. Metal-organic frameworks (MOFs) have emerged as promising sorbents due to their unique structure and tunable properties. MOFs possess a high surface area and tailored porosity, enabling efficient adsorption and retention of various analytes. This comprehensive review thoroughly investigates the applications of MOFs and their derivatives in extraction or microextraction methods. The advantages and limitations of each method are examined, providing insights into scenarios where MOFs outperform other sorbents. The review explores the incorporation of MOFs into existing extraction techniques, with a particular focus on coating techniques for SPME fibers with MOFs. Various coating methods are evaluated for their effectiveness in real applications. Besides, methods of preparation of appropriate devices for each microextraction technique such as SPME, HF-SPME, and In tube-SPME were discussed. The review also explores the benefits of MOF functionalization and its impact on the extraction process. Functionalization involves modifying the surface of MOFs to introduce additional selectivity and improve their affinity for specific analytes. Different functionalization strategies are discussed, highlighting their potential for enhancing extraction efficiency. Also, MOF hybrid materials including MOF-on-MOF are addressed to increase the sorbent ability. Despite the advantages of MOFs as sorbents, certain limitations need to be addressed. These include stability issues, limited choices of suitable MOFs for extraction, and challenges in regenerating the sorbents for reuse. The review proposes strategies to overcome these limitations, such as developing more stable MOF structures, exploring new MOF materials, and optimizing regeneration techniques. [ABSTRACT FROM AUTHOR]

[Display omitted] • Modern and conventional extraction techniques were compared. • Modern microextraction techniques had several advantages over conventional techniques. • The Phree™ plate and mini-LLE were the best methods for vitamin K analysis in human serum. As a representative of the lipophilic vitamins, vitamin K is one of the most difficult vitamins to analyze. Even modern approaches using mass spectrometry detection cannot be carried out without multi-step, time-consuming, economically, and ecologically demanding sample treatment. These findings suggest an opportunity to develop new modern trends that could shorten and simplify the whole procedure, whereby emphasizing the processing of a large number of samples with an additional focus on more environmentally friendly techniques. We selected and compared the main types of both, modern and conventional approaches for vitamin K analysis in human serum including liquid–liquid extraction and solid-phase extraction on the one hand, as well as supported liquid extraction, Phree™ phospholipid removal plate, miniaturized liquid–liquid extraction, and dispersive pipette extraction on the other hand. The different techniques were compared from an analytical perspective, including parameters such as recovery, limits of detection, and matrix effects, as well as from a non-analytical perspective, including time consumption, cost effectiveness, and manual labor required to perform the procedure. The modern techniques seem to have great advantages. Our results indicate that the Phree™ phospholipid removal plate, and the miniaturized version of the liquid–liquid extraction are the best techniques. This work was also carried out to provide a guide for the extraction of vitamin K while determining it using the liquid chromatography-mass spectrometry technique, which may improve sample handling and help to remove potential obstacles in the future. [ABSTRACT FROM AUTHOR]

[Display omitted] • A novel and simple fabric phase sorptive extraction technique was developed based on ethylenediamine tetra-acetic acid (EDTA-FPSE). • The proposed technique was used for the selective determination of Pb2+, Cu2+ and Zn2+ metal cations and their elimination by using ICP-OES. • It is the first time that the complexing agent has been bonded on the fabric substrate. A novel and simple fabric phase sorptive extraction technique based on using ethylenediamine tetra-acetic acid (EDTA-FPSE), was used for selective solid phase extraction of Pb2+, Cu2+ and Zn2+ cations followed by using inductively coupled plasma-optical emission spectrometry (ICP-OES). Then, the synthesized adsorbent was characterized by field emission scanning electron microscopy (FESEM) and energy dispersive X-Ray (EDX) analysis. The effect of some parameters including pH of the sample solution, extraction time, sample solution volume and the type and concentration of desorbent solution was investigated and they were optimized in details. Under the optimum experimental conditions, the limits of detection (LOD) were found to be: 0.062, 0.032 and 0.036 µg/L for Pb2+, Cu2+ and Zn2+cations, respectively and the limits of quantification (LOQ) were equal to 0.18, 0.1 and 0.12 µg/L for Pb2+, Cu2+ and Zn2+cations, correspondingly. Also, the reusability of the synthesized EDTA based on fabric phase sorptive adsorbent, showed that for these metal cations, it could be used for at least 12 adsorption/desorption cycles. Adsorption mechanism was evaluated by different isotherm models and based on the obtained results, the adsorption of Pb2+, Cu2+ and Zn2+ cations is followed by Langmuir isotherm model with a maximum adsorption capacity of 92.60, 75.76 and 101.10 mg g−1 for Pb2+, Cu2+ and Zn2+cations, respectively. Finally, the selective behavior, high recovery percentage (more than 90 %), simple extraction procedure (easily separation of adsorbent from solution), makes the EDTA based on fabric phase sorptive extraction (EDTA-FPSE) technique as an unique technique for solid phase extraction of these heavy metal cations in different real sample solutions. [ABSTRACT FROM AUTHOR]

Pipette tip solid-phase extraction (PT-SPE) as a miniaturized solid-phase extraction technique have a wide range of applications in the field of sample pretreatment. In this study, ionic covalent organic frameworks@cotton (iCOF@cotton) were facilely synthesized by mechanochemical grinding method only in half an hour, and used as the adsorbents of PT-SPE. The synthesized iCOF@cotton not only had high specific surface area, suitable pore structure and cationic charge groups of iCOF that can extract polar targets quickly, but also reduced the problem of high back pressure of PT-SPE by the addition of cotton, thus accelerating extraction time. Combined with high performance liquid chromatographic tandem mass spectrometry (HPLC-MS/MS), an efficient and sensitive method was established for detection of domoic acid (DA, a toxin produced by algae). Under the optimal conditions, the proposed analysis method displayed excellent analytical performance, including broad range of linearity (10–1000 pg mL−1), low limit of detection (LOD, 5 pg mL−1), high correlation coefficient (0.9993), satisfactory precision (RSDs ≤6.4 %). In addition, the developed method was applied to the detection of DA in marine samples, and detected trace DA (18.6 pg mL−1) with satisfactory recovery (85.7%–107.2 %). The above results indicated that the prepared iCOF@cotton have great potential as the adsorbents for PT-SPE. [Display omitted] • Ionic covalent organic frameworks@cotton were fast and conveniently synthesized by mechanochemistry methods. • Ionic covalent organic frameworks have abundant cationic charge groups and high adsorption capacity for domoic acid. • The cotton effectively reduced high back pressure in the pipette tip solid-phase extraction. • The method was successfully applied to the enrichment of domoic acid in marine samples. [ABSTRACT FROM AUTHOR]

• DLP 3D printing – using resin and C18 silica suspension for pharmaceutical analysis. • Study refines printing, material, and extraction parameters for enhanced performance. • Cost-effective, quick and inclusive: cheap 3D-printer with widely available materials. • 3D printing fabricates extraction devices – shaped as needed, with C18 silica particles. • 3D printed devices exhibit precise and accurate analytical performance. In recent years, there has been an increasing worldwide interest in the use of alternative sample preparation methods. Digital light processing (DLP) is a 3D printing technique based on using UV light to form photo-curable resin layer upon layer, which results in a printed shape. This study explores the application of this technique for the development of novel drug extraction devices in analytical chemistry. A composite material consisting of a photocurable resin and C18-modified silica particles was employed as a sorbent device, demonstrating its effectiveness in pharmaceutical analysis. Apart from estimating optimal printing parameters, microscopic examination of the material surface, and sorbent powder to resin ratio, the extraction procedure was also optimised. Optimisation included the type and amount of sample matrix additives, desorption solvent, sorption and desorption times, and proper number of sorbent devices needed in extraction protocol. To demonstrate this method's applicability for sample analysis, the solid-phase extraction followed by gas chromatography coupled with mass spectrometry (SPE-GC–MS) method was validated for its ability to quantify benzodiazepine-type drugs. This evaluation confirmed good linearity in the concentration range of 50–1000 ng/mL, with R2 values being 0.9932 and 0.9952 for medazepam and diazepam, respectively. Validation parameters proved that the presented method is precise (with values ranging in-between 2.98 %-7.40 %), and accurate (88.81 % to 110.80 %). A negative control was also performed to investigate possible sorption properties of the resin itself, proving that the addition of C18-modified silica particles significantly increases the extraction efficiency and repeatability. The cost-effectiveness of this approach makes it particularly advantageous for single-use scenarios, eliminating the need for time-consuming sorbent-cleaning procedures, common in traditional solid-phase extraction techniques. Future optimisation opportunities include refining sorbent size, shape, and geometry to achieve lower limits of quantification. As a result of these findings, 3D-printed extraction devices can serve as a viable alternative to commercially available SPE or solid-phase microextraction (SPME) protocols for studying new sample preparation approaches. [ABSTRACT FROM AUTHOR]

The fast rate of development in the software and electronics industries is forcing many other fields, like chemistry, to keep up; mobile labs are needed for more and more chemical processes and tests. The effective remediation of the ecosystem or water purification needs an efficient and versatile method involving rapid chemical reactions. Along with the development of smart devices and their use in daily life, micro/nanomotors (MNMs) have gained more attention from analytical chemists due to their unique characteristics. MNMs are promising candidates for future environmental treatment and separation sciences. MNMs are revolutionizing the environmental and bioanalytical sciences with their incredible versatility, ease of use, and precision. Future MNMs will replace environmental remediation equipment, smart drug delivery, portable smart biosensing devices, separation, catalysis, and operation in challenging environments. This review aims to explore the applications of MNMs in solid-phase extraction and its future aspects. • Smart devices in daily life, micro/nanomotors (MNMs) have gained more attention from analytical chemists. • MNMs are promising candidates for future environmental treatment and separation sciences. • MNMs is revolutionizing with their incredible versatility, ease of use, and precision. • The applications of MNMs in solid-phase extraction and its future aspects is discussed. [ABSTRACT FROM AUTHOR]

Carbonaceous materials, namely graphitized carbon black (GCB) and porous graphitic carbon (PGC), are an exciting class of stationary phases attracting remarkable attention due to their peculiar characteristics of retention behavior for non-polar and polar analytes, becoming an alternative to the typical reversed-phase stationary phases. The present review is focused on the recent and critical analytical applications of GCB and PGC in liquid phase applications. A comprehensive overview of GCB in sample preparation was done, primarily solid-phase extraction and related techniques. Traditional analytes, such as pesticides and hormones, are reviewed along with new applications, especially short-chain peptides and polar metabolites, where this sorbent allowed for filling a gap in sample preparation from complex biological matrices. The second part of the review article describes the applications of porous graphitic carbon in liquid chromatography and supercritical fluid chromatography. The discussion covers the most relevant analyte classes, with an extensive description of the advantages and disadvantages of PGC over other chromatographic techniques. [Display omitted] • The difference between GCB and PGC are discussed. • The extraction and analysis application of GCB are summarized. • A recent application of GCB in short-chain peptidomics is discussed. • The chromatographic application of PGC are summarized. • The forecast and challenges in the use of carbonaceous material are illustrated. [ABSTRACT FROM AUTHOR]

Sample pretreatment plays a vital role in determining and analyzing targets in complex samples like food, biological, and environmental samples. Particularly, graphene and graphene oxide have been widely explored as sorbents in sample preparation. More recently, their composites with magnetic materials, molecularly imprinted polymers, metal-organic frameworks, covalent organic frameworks, aerogels, and other materials have also been developed for sample preparation. Interestingly, these composites enhanced enrichment and selectivity towards different types of analytes by multiple mechanisms including hydrogen bonding, π-stacking, electrostatic, hydrophobic, and hydrophilic effects. Primarily, this review focuses on the recent development of graphene/graphene oxide-based sorbents in solid-phase extraction (SPE) and solid-phase microextraction (SPME) from 2017 to 2022. The main extraction techniques in this paper include column SPE, dispersive SPE, magnetic SPE, pipette-tip SPE, fiber SPME, in-tube SPME, etc. Meanwhile, the current problems and prospects are summarized and described. • The recent advances of G/GO-based sorbents in SPE are summarized. • The applications of G/GO-based sorbents in SPME are overviewed. • The extraction mechanism of G/GO-based materials is described. • The analysis of various targets in different samples is reviewed. • Prospects and challenges of G/GO-based extraction materials are discussed. [ABSTRACT FROM AUTHOR]

[Display omitted] • The principles of DSPE and the preparation DSPEs absorbent for FQs are addressed. • Analytical instrumentations and performances of DSPE towards FQs are highlighted. • Reviews on the application of DSPE on FQs analysis are discussed and summarized. • Recent advancements in the extraction of FQs using DSPE are addressed. Misuse and incorrect fluoroquinolones (FQs) disposal have led to environmental pollution and trace amounts of FQs contamination in food chains. Consequently, the quest for innovative, simple, and improved techniques of FQs analyte pre-treatment in real samples has focused on micro- and macroscale dispersive solid-phase extraction (DSPE). Recent studies have reported implementing DSPE-based techniques as a sample preparation step to determine FQs in various sample matrices. The present study summarises current FQs detection methods with various chromatographic and DSPE-based combinations. Furthermore, the merits and the analytical figures of DSPE performance when employed for actual samples were discussed. This study also comprehensively evaluated corresponding challenges, opportunities, and the potential of DSPE in detecting trace levels of FQs. The findings demonstrated that the DSPE-based technique provided undeniable advantages for routine sample pre-treatment of FQs and enhanced analytical performance. [ABSTRACT FROM AUTHOR]

• A stable core-shell MOF@COF composite was synthesized and utilized as SPE adsorbent. • The covalent integration of hydrophobic COF shell successfully enhanced the hydrophobicity of MOF core. • The excellent extraction efficiency was attributed to the presence of multiple interactions. • A sensitive method for the quantification of flavonoids in grape juice and honey samples was developed. Hydrophobization and stability is crucial for the practical application of most metal-organic frameworks (MOFs) in extraction technique. In this study, a stable core-shell MOF@COF composite (NH 2 -MIL-101(Fe)@TAPB-FPBA-COF) was successfully prepared by Schiff base reaction and applied to solid-phase extraction (SPE) of hydrophobic flavonoids. Notably, the TAPB-FPBA-COF shell acts as a hydrophobic "shield", which not only improves the hydrophobicity and stability of hydrophilic NH 2 -MIL-101(Fe), but also makes the extraction efficiency of flavonoids from MOF@COF composite significantly higher than that of pure NH 2 -MIL-101(Fe) and TAPB-FPBA-COF. In addition, a sensitive analytical method with excellent linearities (0.1–500 ng mL−1, R2 ≥ 0.9967), low limits of detection (0.02–0.04 ng mL−1 for water; 0.04–0.07 ng mL−1 for grape juice; 0.06–0.08 ng mL−1 for honey), good repeatability (intra-day/inter-day precision are 1.86–5.37%/1.82–7.79%, respectively) and only 5 mg of adsorbent per cartridge was established by optimizing the SPE process combined with high performance liquid chromatography with ultraviolet-visible detector (HPLC-UV). Meanwhile, selectivity study and comparative experiments with the commercial C18 adsorbent showed that the MOF@COF adsorbent exhibited satisfactory extraction efficiency for flavonoids due to multiple interactions such as hydrogen bonding, hydrophobic, and π-π interactions. Finally, the good recoveries in grape juice (84.5–102.5%) and honey (87.5–104.6%) samples further validated the applicability of the proposed method in complex samples. [ABSTRACT FROM AUTHOR]

• Successful preparation of smart temperature-responsive aerogel reactors for target recognition of UA. • ITR&AR(G570)&UA-MIP for intelligent response to absorption and desorption of UA under specific temperature conditions. • The prepared aerogel reactor was used for the extraction of UA from lingonberry. • The developed adsorbent exhibited good extraction efficiency and selectivity. In this article, thermosensitive molecularly imprinted polymer and composite aerogel were combined for the first time to create an intelligent temperature-responsive aerogel reactor to effectively enrich ursolic acid (UA). Because aerogel carrier had a higher specific surface area and higher porosity compared to other carriers, the ursolic acid molecularly imprinted intelligent temperature responsive aerogel reactor (ITR&AR(G570)&UA-MIP) demonstrated a higher adsorption capacity for UA. More notably, ITR&AR(G570)&UA-MIP have the extraordinary capacity to spontaneously adsorb-desorb target molecule UA by regulating the reaction temperature. The ratio of the target molecule UA to the functional monomer and crosslinker in the grafting process and external influences had a major impact on how ITR&AR(G570)&UA-MIP were prepared overall. When the molar ratio of UA to 4-VP was 1:8, the weight ratio between ITR&AR(G570)&UA-MIP and EGDMA/DVB was 1:2:10, the reaction temperature was 60 °C, and the ambient pH = 6, the material showed the best adsorption capacity, reaching a peak of about 70 mg g−1. After researching the appropriate synthesis conditions, ITR&AR(G570)&UA-MIP were applied to lingonberry (Vaccinium Vitis-Idaea L.) berry extracts in this work. The outcomes show that this technique provides a new, intelligent, temperature-controlled adsorption material for the solid-phase extraction of triterpenoid acids in natural products, with good specific adsorption performance for the target molecule UA. [ABSTRACT FROM AUTHOR]

[Display omitted] • Molecularly imprinted polymers (MIPs) synthesized using penconazole as template molecule and N-Isopropylacrylamide (NIPAM) as functional monomer show good recognition properties toward the triazole ring. • Widely employed triazole pesticides can be efficiently isolated from complex matrices (i.e. juices, surface water) by the strategy of dispersive solid phase extraction using the developed MIPs as selective sorbents (MIP-d-SPE). • Plackett-Burman design of experiment is a useful tool to screen the effect of different combinations of functional monomers and cross linkers as well as the effect of different extraction conditions. In the present study, novel molecularly imprinted polymers were prepared using penconazole as template and different combinations of functional monomers (acrylic acid (AA) and N-isopropylacrylamide (NIPAM)) and cross-linkers (ethylene glycol dimethacrylate (EGDMA) and trimethylolpropane trimethacrylate (TRIM)), according to a Plackett-Burman design of experiments. Materials were fully characterized by Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and nitrogen adsorption analysis. Rebinding behaviors in solution were studied both at the equilibrium (Langmuir, Freundlich and Temkin models), and at the non-equilibrium (pseudo-first, pseudo-second order kinetics). Materials were further tested as sorbents for dispersive solid phase extraction (d-SPE) on apple juice for multicomponent recovery of triazole fungicides at trace level, testing several variations of extraction parameters (juice pH, amount of sorbent, adsorption time, desorption solvent, desorption time) leading to the selection of the best materials and simultaneously of the best extraction conditions. MIPs synthesized with NIPAM showed significatively higher affinity for triazole pesticides in apple juice than the ones synthesized with AA, while no differences emerged for the two cross-linkers employed (EGDMA, TRIM). Selectivity was also assessed, testing MIPs as d-SPE sorbents in undiluted apple juice spiked with triazole pesticides concurrently with other interfering compounds. The newly developed NIPAM-based penconazole-imprinted MIPs showed an excellent recognition mechanism towards compounds containing the triazole ring, and significatively lower recoveries for other compounds. The developed analytical procedure based on molecularly imprinted polymer dispersive solid phase extraction and liquid chromatography coupled with mass spectrometry (MIP-d-SPE-LC-MS) was validated for selective enrichment and determination of triazole compounds in apple juice samples and river water samples with good recoveries (94.67%–109.03% for river water, 89.79%–110.23%, for apple juice), high repeatability (RSD% < 3.97 for river water, RSD% < 4.85 for apple juice), and reproducibility (RSD% < 5.95 for river water and RSD% < 7.14 for apple juice). [ABSTRACT FROM AUTHOR]

[Display omitted] • LDHs are inert with high surface areas and low operating pressure, used for solid phase microextraction. • LDHs showed an impressive extraction efficiency of various analytes especially ions in different matrices. • Extraction efficiency of LDHs has been enhanced by hybridization with nanomaterials, such as MOFs. • The preparation, characterization, regeneration and analytical performances are also discussed. Microextraction is a technique that can be used to selectively extract substances from a complex matrix using small amounts of extracting agents and/or solvents. The technique can be broadly classified into liquid- and solid-phase microextraction methods, according to the specific nature of the system. The principle of the solid-phase microextraction (SPME) is founded on selective equilibrium-based extraction of compounds using a microporous adsorbent that acts as a solid phase extraction (SPE) sorbent. In recent years, there has been growing interest in the use of layered double hydroxides (LDHs) as microextraction sorbents. The main advantages of using LDHs are their high surface area to volume ratio, low operating pressure, and simplicity of fabrication and purification. They are also relatively inert and easy to purify by simple washing. Several recent studies have shown that LDHs are good candidates for drug delivery, catalysis, environmental remediation, energy storage and chemical analysis. The use of LDH in analytical chemistry includes sensing, electrochemical analysis, and extraction. In this review, the roles of LDHs in solid phase extraction and microextraction including dispersive-solid phase microextraction (dSPME), in-tube solid phase microextraction (IT-SPME), headspace solid phase microextraction (HS-SPME), stir bar sorptive extraction (SBSE) and thin film microextraction (TFME) were discussed. The preparation, characterization, regeneration and analytical performances/applications were also discussed. [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]

• Ultrasound energy enhanced preconcentration efficiency of targeted analytes using advance extraction methodology. • The novel DES based microextraction was developed to overcome hazardous effects of conventional reagents. • The CGS have higher levels of lead under investigation as compared to cadmium. • Proposed method has the advantages of being simple, safe, greener and economical. The present study was carried out to develop a green and novel ultrasonically modified solid phase micro-extraction method (Um-SPµE) to quantify the cadmium (Cd2+) and lead (Pb2+) in acidic water extract (pH < 6.5) of coal gangue soil (CGS) samples collected from the block II of Thar coal field Sindh Pakistan. The 8-hydroxyquinoline (8-HQ) embedded benzophenone allows quantitative enrichment of the Cd2+ and Pb2+ at pH ∼ 6.0. The ultrasonic energy applied to enhance the dissolution/extraction of hydrophobic complex of Cd2+ and Pb2+ in deep eutectic solvent (DES), which synthesized by mixing of zinc chloride and acetamide at 1:2 mol ratios. The extraction capability of DES was enhanced by addition of a nonionic surfactant (Triton X-114) to improve the phase transfer ratio, to notably enhance the recovery of hydrophobic complex of Cd2+ and lead Pb2+. There were various factors (pH, concentration of ligand, adsorbent quantity, volume of DES and nonionic surfactant, and sonication time), effecting the enrichment factor, preconcentration and % recoveries of both metals; were optimized. The certified reference materials and spiking recovery test were applied to real samples in order to check precision and validity of the developed methodology. The % recoveries of both selected metals were found to be > 98% by applying developed method (p < 0.05). [ABSTRACT FROM AUTHOR]

• Comprehensive overview of common argentation separations is provided. • Selectivity mechanisms of argentation separations are described. • Optimization methods for liquid- and gas-phase argentation separations are discussed. • Recent advancements and novel innovations for argentation separations are highlighted. • Wide range of applications utilizing argentation separations are reviewed. The use of silver(I) ions in chemical separations, also known as argentation separations, is a powerful approach for the selective separation and analysis of many natural and synthetic organic compounds. In this review, a comprehensive discussion of the most common argentation separation techniques, including argentation-liquid chromatography (Ag-LC), argentation-gas chromatography (Ag-GC), argentation-facilitated transport membranes (Ag-FTMs), and argentation-solid phase extraction (Ag-SPE) is provided. For each of these techniques, notable advancements, optimized separations, and innovative applications are discussed. The review begins with an explanation of the fundamental chemistry underlying argentation separations, mainly the reversible π-complexation between silver(I) ions and carbon-carbon double bonds. Within Ag-LC, the use of silver(I) ions in thin-layer chromatography, high-performance liquid chromatography, as well as preparative LC are explored. This discussion focuses on how silver(I) ions are employed in the stationary and mobile phase to separate unsaturated compounds. For Ag-GC and Ag-FTMs, different silver compounds and supporting media are discussed, often with relation to olefin-paraffin separations. Ag-SPE has been widely employed for the selective extraction of unsaturated compounds from complex matrices in sample preparation. This comprehensive review of Ag-LC, Ag-GC, Ag-FTMs, and Ag-SPE techniques emphasizes the immense potential of argentation separations in separations science and serves as a valuable resource for researchers seeking to learn, optimize, and utilize argentation separations. [ABSTRACT FROM AUTHOR]

[Display omitted] • The review summarizes the most important roles of DESs in solid-phase (micro)extraction techniques. • The use of DESs as modifiers of sorbents, parts of sorbents, and directly as sorbents is discussed. • The use of DESs as eluting solvents and as dispersing agents is described. • The use of DESs in hyphenated extraction techniques is presented. One of the key challenges of modern analytical chemistry is the monitoring of trace amounts of contaminants using sensitive and selective instrumental techniques. Due to the variety and complexity of some samples, it is often necessary to properly prepare a sample and to perform a preconcentration of trace amounts of analytes. In line with the principles of Green Analytical Chemistry (GAC), it is important for an analytical procedure to reduce labor and time consumption and to decrease the use of volatile and hazardous solvents. Therefore, solvent-free extraction techniques, such as SPE, µSPE, SPME and their various modifications, which are mainly aimed at increasing their "greenness", have been very popular for many years. Deep eutectic solvents fit perfectly into GAC principles, which is why they have been used as extractants in liquid-phase microextraction techniques for a long time. This review is a follow-up to our recently published article on the use of deep eutectic solvents (DESs) in liquid-phase microextraction techniques and summarizes the most important applications of DES in solid-phase (micro)extraction techniques. [ABSTRACT FROM AUTHOR]

Since the implementation of Green Chemistry into analytical practice, significant efforts have been made to improve the sustainability of chemical analysis. These include reducing the use of hazardous chemicals and solvents, minimizing waste, and improving energy efficiency. Surfactants can be applied in chemical analysis as an environmentally friendly alternative to conventional solvents and chemicals. The use of surfactants can increase extraction efficiency by improving solubility, increasing selectivity, and reducing organic solvent consumption. In addition, surfactants can also reduce interference with the sample matrix and improve limits of detection. This review covers recent developments in surfactant-based extraction techniques, highlighting the use of surfactants in both liquid-phase and solid-phase extraction. The main principles of surfactant-based extraction methods are discussed, as well as their application as assisting agents or surface modifiers. The effects of deep eutectic solvents on surfactants micellization and the application of biocompatible surfactants are also discussed. [Display omitted] • Overview of surfactant-based extraction techniques. • Surfactants in liquid-phase and solid-phase extraction. • Biosurfactants in the extraction process. • Influence of DES on the behavior of surfactants. [ABSTRACT FROM AUTHOR]

Determination of pollutants present in environmental samples at a low concentration level very often requires the analytical protocol that includes analytes isolation and/or enrichment prior to the final quantification. Miniaturized SPE offers an interesting alternative to LLE. Nowadays, many types of sorbents are available and can be used as selective materials for extraction of varied analytes in different kinds of samples. The characteristic of sorbent plays a crucial role because determines the resulting extraction mechanism of particular technique. SPE techniques have numerous positive features. This review provides an updated, comprehensive overview of new types of sorbents used in SPE-based techniques. In addition, miniaturized SPE techniques applied to environmental problems are described, based on the most recent, relevant, and representative examples of successful application. The perspective of the most promising directions for the development of the SPE technology in the near future, and the greatest challenges that will have to be faced, are also outlined. • SPE has been practiced in a modern form for more than half a century. • SPE technique was constantly developing, driven by the needs of analysts chemists. • SPE-type techniques connected with quantufication methods are perfect to be applied for environmental pollution analysis. • Many type of new sorbents are ised in SPE techniques. • Application of miniaturized SPE techniques to environmental problems brings many advantages. [ABSTRACT FROM AUTHOR]

• Recent advances in CPE over the last three years (2020 – 2022) are reviewed. • Various innovative approaches in CPE are discussed. • Positive effect of auxiliary energies is emphasized. • Advantages of the combination of CPE with nanomaterial-based SPE are highlighted. Cloud-point extraction (CPE) is a pre-treatment technique for the extraction and preconcentration of different chemical compounds, such as metal ions, pesticides, drugs, phenols, vitamins etc., from various samples. CPE is based on the phenomenon of two phases (micellar and aqueous) forming after the heating of an aqueous isotropic solution of a non-ionic or zwitterionic surfactant above the cloud-point temperature. If analytes are added to the surfactant solution under suitable conditions, they should be extracted into the micellar phase, also called the surfactant-rich phase. Recently, the traditional CPE procedure is being increasingly replaced by improved CPE procedures. In this study, recent advances in CPE over the last three years (2020 – 2022), including the application of various innovative approaches, are reviewed. In addition to the basic principle of CPE, alternative extraction media in CPE, CPE supported by various auxiliary energies, a different modified CPE procedure and the use nanomaterials and solid-phase extraction in combination with CPE are presented and discussed. Finally, some future trends for improved CPE are presented. [ABSTRACT FROM AUTHOR]

[Display omitted] • Two methods were used in a raw for preconcentration of anti-depressants before HPLC analysis. • Dμ-SPE coupled SSME was exploited for determination of ultra-trace levels of these drugs. • The devised method was selective, sensitive, green, and highly beneficial. • Wide linearities, acceptable RSD values, and good LODs and LOQs were obtained. • The devised method was tested for analysis of biological samples with complex matrices. A selective, sensitive, and green sample preparation method was devised by applying a supramolecular solvent-based microextraction (SSME), based on the salting out effect, after conducting the dispersive micro solid phase extraction (Dμ-SPE). The technique was employed for preconcentrative extraction and determination of five anti-depressant drugs in human plasmas and urine samples. The first step was conducted by synthesizing and using a layered double hydroxide-carbon nanotube nanohybrid adsorbent. Multiple interactions betwixt the nanoadsorbent and target analytes, including electrostatic, hydrogen bonding, and π-π interactions and the large surface area of the adsorbent led to an effective performance. In the next step, after emulsification in the presence of supramolecular solvent by ultrasonication, the salting-out effect was applied to separate the extraction phases. At Optimization conditions, wide linearities were obtained, in the ranges of 1.5–3500, 2.0–3500, 1.0–3200, 2.0–3000, and 2.0–3000 ng mL−1 for imipramine, amitriptyline, trimipramine, sertraline, and citalopram, respectively, with low limits of detection ranging from 0.3 to 0.6 ng mL−1. Also, acceptable RSD values (≤8.9%; n = 5) for intra- and inter–day precision were obtained, along with acceptable spiked recoveries (94.5–100.0%) in complex matrices. Overall, the effectiveness of the nanosorbent, ultrasonication, supermolecule green solvents with easy solidification and collection, and elimination of the centrifugation bestowed a highly beneficial method for analyzing anti-depressant drugs. [ABSTRACT FROM AUTHOR]

• Current strategies (over the last 5 years) towards Gingerol extraction are given. • Innovative techniques for the purification of Gingerol are highlighted. • The most recent outcomes for the effective extraction are stated. • MAME technique exhibits extraction yield of 6-shogaol as high as 97%. Currently, ginger is one the most consumed plants when dealing with the treatments of various illnesses. So far, it is known that various biologically active molecules, such as gingerols, shogaols and zingerone, among others, are the main responsible for specific biological activities, opening a new window for its utilization as a nutraceutical in foods. In pioneering extraction processes, solvent extraction has been initially used for these applications; however, the drawbacks of this typical extraction method compared with other emergent separation techniques make it possible for the exploration of new extraction pathways, including microwave, ultrasound, supercritical, subcritical and pressurized-assisted extraction, along with three phase partitioning, high-speed counter current chromatography and magnetic solid phase extraction. To the best of our knowledge, there is no report documenting the recent studies and cases of study in this field. Therefore, we comprehensively review the progress and the latest findings (over the last five years) on research developments, including patents and emerging extraction methods, aiming at the purification of biologically active molecules (gingerols, shogaols and zingerone) contained in ginger. Over the course of this review, particular emphasis is devoted to breakthrough strategies and meaningful outcomes in ginger components extraction. Finally, dosage and safety concerns related to ginger extracts are also documented. [ABSTRACT FROM AUTHOR]

The review presents an evaluation of the development of on-line, at-line and in-line sample treatment coupled with capillary and microchip electrophoresis over the last 10 years. In the first part, it describes different types of flow-gating interfaces (FGI) such as cross-FGI, coaxial-FGI, sheet-flow-FGI, and air-assisted-FGI and their fabrication using molding into polydimethylsiloxane and commercially available fittings. The second part deals with the coupling of capillary and microchip electrophoresis with microdialysis, solid-phase, liquid-phase, and membrane based extraction techniques. It mainly focuses on modern techniques such as extraction across supported liquid membrane, electroextraction, single drop microextraction, head space microextraction, and microdialysis with high spatial and temporal resolution. Finally, the design of sequential electrophoretic analysers and fabrication of SPE microcartridges with monolithic and molecularly imprinted polymeric sorbents are discussed. Applications include the monitoring of metabolites, neurotransmitters, peptides and proteins in body fluids and tissues to study processes in living organisms, as well as the monitoring of nutrients, minerals and waste compounds in food, natural and wastewater. [Display omitted] • On-line coupling of sample treatment with capillary and microchip electrophoresis. • Cross, coaxial, sheet-flow, and air-assisted flow gating interface. • Coupling to microdialysis, solid-phase, liquid-phase, and membrane extraction. • Construction of sequential analysers and fabrication of SPE microcartridges. • Monitoring of processes in living organisms, food composition and contaminants in waters. [ABSTRACT FROM AUTHOR]

Capillary electrophoresis (CE) handles complex samples with excellent resolution, but has poor sensitivity because of the small detection volume and suffers from destacking of high-conductivity samples; therefore, sample preparation is often required for matrix cleanup and analyte enrichment. This review discusses operationally-simple sample preparation schemes which are easily adoptable by researchers using commercial CE instruments, wherein various solid-phase microextraction (SPME) and liquid-phase microextraction (LPME) techniques are 'in-line' coupled (i.e., integrated) to the separation capillary without modifying the commercial CE instrument with sophisticated interfaces. In-line coupling refers to scenarios where the prepared sample is injected directly into the separation capillary. Then, sample loss is reduced and the enrichment factors can be significantly increased as the acceptor volume can be reduced to the nanoliter level. Cases involving subsequent on-line preconcentration are also discussed. In-line SPME-CE and LPME-CE are powerful tools for analyzing various samples, especially trace substances in complex biological matrices. • Simple in-line coupled sample preparation schemes with capillary electrophoresis. • Micro solid-phase extraction integrated in the separation capillary. • Liquid-phase microextraction using a supported liquid membrane, or single drop. • In-tube microextraction using a liquid plug in a capillary. • Combination of in-line microextraction and on-line sample preconcentration. [ABSTRACT FROM AUTHOR]

Solid Phase Extraction (SPE) has been practiced in a modern form for more than half a century. It was constantly developing, driven by the analysts needs. These needs are coming from the importance to select an appropriate analytical method, which should have satisfactory accuracy, precision and sensitivity. In the case of sorbent-based microextraction techniques, the choice of miniaturized variants that meet these requirements as well as the requirements of GAC is extremely wide. The increasing popularity of the technique has spurred the influx of many manufacturers into the commercial side of the technology, and many columns, cartridges and discs are comercially available. SPE-type techniques which can be connected with quantification techniques, are perfect to be applied for pollution analysis. The purpose of this article is to provide the reader with an updated, comprehensive overview of modern SPE techniques for different kind of pollutants analysis. • SPE has been practiced in a modern form for more than half a century. • SPE technique was constantly developing, driven by the needs of analysts chemists. • SPE-type techniques connected with quantufication methods are perfect to be applied for environmental pollution analysis. • Many columns (cartridges), discs and packings of SPE are comercially available. [ABSTRACT FROM AUTHOR]

• Extraction phases compared for different sampling formats. • For aqueous samples selectivity is controlled by the properties of water. • For gas phase samples selectivity is controlled by sorbent properties. • For non-aqueous samples selectivity is controlled by the sample solvent or matrix. Extraction is the most common sample preparation technique prior to chromatographic analysis for samples which are too complex, too dilute, or contain matrix components incompatible with the further use of the separation system or interfere in the detection step. The most important extraction techniques are biphasic systems involving the transfer of target compounds from the sample to a different phase ideally accompanied by no more than a tolerable burden of co-extracted matrix compounds. The solvation parameter model affords a general framework to characterize biphasic extraction systems in terms of their relative capability for solute-phase intermolecular interactions (dispersion, dipole-type, hydrogen bonding) and within phase solvent-solvent interactions for cavity formation (cohesion). The approach is general and allows the comparison of liquid and solid extraction phases using the same terms and is used to explain the features important for the selective enrichment of target compounds by a specific extraction phase using solvent extraction, liquid-liquid extraction, and solid-phase extraction for samples in a gas, liquid, or solid phase. Hierarchical cluster analysis with the system constants of the solvation parameter model as variables facilitates the selection of solvents for extraction, the identification of liquid-liquid distribution systems with non-redundant selectivity, and evaluation of different approaches using liquids and solids for the isolation of target compounds from different matrices. [ABSTRACT FROM AUTHOR]

• This review provides conceptual information on the recent advancement of SPE techniques. • The current progress in the methodology and parameters affecting extraction are discussed. • Instrumental and operational advancement for SPE has been described. • In-depth analysis of nanosorbent for antimicrobial analysis has been presented. • In detail physicochemical properties of antibiotics has been tabulated. • Future directions in SPE research and the challenges that have arisen so far are discussed. Antibiotics are life-saving medications for treating bacterial infections; however it has been discovered that resistance developed by bacteria against these incredible agents is the primary contributing factor to rising global mortality rates. The fundamental cause of the emergence of antibiotic resistance in bacteria is the presence of antibiotic residues in various environmental matrices. Although antibiotics are present in diluted form in environmental matrices like water, consistent exposure of bacteria to these minute levels is enough for the resistance to develop. So, identifying these tiny concentrations of numerous antibiotics in various and complicated matrices will be a crucial step in controlling their disposal in those matrices. Solid phase extraction, a popular and customizable extraction technology, was developed according to the aspirations of the researchers. It is a unique alternative technique that could be implemented either alone or in combination with other approaches at different stages because of the multitude of sorbent varieties and techniques. Initially, sorbents are utilized for extraction in their natural state. The basic sorbent has been modified over time with nanoparticles and multilayer sorbents, which have indeed helped to accomplish the desired extraction efficiencies. Among the current traditional extraction techniques such as liquid-liquid extraction, protein precipitation, and salting out techniques, solid-phase extractions (SPE) with nanosorbents are most productive because, they can be automated, selective, and can be integrated with other extraction techniques. This review aims to provide a broad overview of advancements and developments in sorbents with a specific emphasis on the applications of SPE techniques used for antibiotic detection and quantification in various matrices in the last two decades. [ABSTRACT FROM AUTHOR]

• A honeycomb morphology resin modified by porogen P123 and F127 was synthesized. • The honeycomb resin had good adsorption properties for alectinib and metabolite M4. • Spin column solid phase extraction technique was used for the pretreatment of urine. • A new method was developed for the therapeutic drug monitoring of alectinib and M4. Alectinib and its metabolite, M4, have demonstrated a satisfactory clinical therapeutic effect in the treatment of anaplastic lymphoma kinase-positive advanced non-small-cell lung cancer. Due to individual differences among patients, therapeutic drug monitoring (TDM) is critical for guaranteeing appropriate clinical drug use. To realize TDM for alectinib and its metabolite, M4, a honeycomb phenol-formaldehyde resin (PFR) with excellent hydrophilic properties, abundant adsorption force, and a stable porous structure was synthesized by modifying the porogens F127 and P123. The prepared PFR was employed as an adsorbent in a simple and efficient spin-column solid-phase extraction (SPE) process. A rapid method for detecting alectinib and its metabolite M4 in urine was thereby established. The established method showed a linear range of 0.0200 μg mL–1–5.00 μg mL–1 and the recovery range of 98.8–103% for spiked urine samples, with relative standard deviations of ≤ 4.87% (n = 3). Our results proved the practicability of the proposed honeycomb-PFR spin-column SPE method in TDM for alectinib and its metabolite, M4. [ABSTRACT FROM AUTHOR]

Ag modified ZnO nanoflowers were synthesized by using hydrothermal method and used as dispersive micro-solid phase extractant for separation and preconcentration prior to its flame atomic absorption spectrometric detection. The Ag modified ZnO nanoflowers has been characterized by FT-IR, XRD, FESEM, EDX and BET. The factors effecting extraction efficiency like pH, Adsorbent dose, sample volume, eluent concentration, eluent volume was optimized. Matrix effects were also studied. The limit of detection and preconcentration factor (PF) were calculated as 8.52 μg L−1, and 100, respectively. The presented dispersive micro-solid phase extraction technique was validated using GBW07424 (GSS-10) soil and GBW07425 (GSS-11) soil certificated reference materials (CRMs) with satisfactory recovery results. The presented dispersive micro-solid-phase extraction (d -μSPE) procedure was successfully applied to food and water samples. [Display omitted] • Ag modified ZnO nanoflowers were synthesized by using hydrothermal method. • Ag modified ZnO nanoflowers were used for the solid phase extraction of lead (II). • The limit of detection and preconcentration factor were calculated as 32.7 ng/mL, and 100, respectively. • The method was successfully applied to food and water samples. [ABSTRACT FROM AUTHOR]

Imidazolium ionic liquids (ILs) are chemical compounds beginning to be used on a mass scale. Although their presence in the environment is usually treated as only potential threat, there are already first evidences that this has become a real case. Taking into account their increasing use it might be expected that this problem will also increase in the nearest future. Given that some of the imidazolium cations exhibit high potential for bioconcentration, it is likely that they will accumulate in the tissues of wild organisms. Thus, there is no doubt that monitoring the presence of these compounds in organisms from potentially contaminated waters will be needed. Therefore, the aim of our study was to develop and fully validate a novel and reliable analytical procedure for the determination of the mixture of imidazolium ILs in Mytilus trossulus mussels. For this purpose, different extraction techniques were tested such as: microwave-assisted extraction (MAE), accelerated-solvent extraction (ASE) and bullet-blender homogenization (HOMO). Finally, the proposed procedure is based on the application of MAE technique for the extraction of imidazolium cations and SPE technique using Oasis HLB cartridges for the purification of the obtained extracts and LC-MS/MS technique with QqQ analyzer for their final determination. Absolute recoveries of the proposed analytical procedure reached 71–90%. The developed procedure is characterized with low limits of quantification, at 50–100 ng g−1 dry tissue and allows for reliable determination of trace amounts of the tested compounds in complex biological matrix. Matrix effects obtained for the optimized procedure ranged from 7.8 to 37.5%. As a result, this is the first study presenting the analytical procedure for the analysis of imidazolium ILs in aquatic animal tissues. [Display omitted] • A novel procedure for analysis of imidazolium ILs in mussels was developed. • The potential application of different extraction techniques was compared. • Microwave-assisted extraction proved to be the most effective technique. • The obtained procedure detection limits are applicable to environmental samples. [ABSTRACT FROM AUTHOR]

[Display omitted] • Detailed background of BPA and its analogues are elaborated. • Recent advancements in extraction of bisphenols using SPE are addressed. • Comparison between types of analysis involved post SPE were described. • Reviews on the analysis of BPA and its analogues were discussed and summarized. Bisphenols in the natural environment have recently attracted global attention as they pose many potential hazards to both human health and the aquatic ecosystem. Due to their trace-level presence, the direct determination of bisphenols in food and water matrices is quite challenging. Most of the existing analytical instrumentation cannot directly handle complex sample matrices. Thus, sensitive, effective, rapid, and simple methods are required to extract and concentrate these compounds. The sample preparation is crucial in the overall chemical analyses. It is essential to isolate and concentrate the analytes of interest from the given matrices to ensure their suitability for separation and detection systems. Many new methods have been recently developed to overcome the limitations of the conventional sample preparation methods. This review provides a detailed background of bisphenol A and its analogues, along with recent advancements in their extraction from various matrices using solid-phase extraction techniques. A critical overview of the analysis type is also presented. [ABSTRACT FROM AUTHOR]

[Display omitted] • Developed a novel dispersive solid phase filtration extraction pretreatment technique. • A large particle size of ZIF-8@SiO 2 was prepared as the adsorbent. • Rapidly and accurately analysis of seaweed polysaccharides in undaria pinnatifida. Laminarin and fucoidan belong to seaweed polysaccharides, which are abundant in kelp, such as undaria pinnatifida, and have a variety of beneficial pharmacological activities. This study developed a dispersive solid-phase filter extraction (DSPFE) method by combining the high mass transfer efficiency of traditional dispersive solid-phase extraction (DSPE) with the timesaving and convenient advantages of filter solid-phase extraction (FSPE). Although the surface interactions enable ZIF-8 to separate large molecules, the small particle size of ZIF-8 generates ultrahigh pressures during solid-phase extraction (SPE). Hence, a large particle size of ZIF-8@SiO 2 can be obtained by growing ZIF-8 on SiO 2. Using ZIF-8@SiO 2 as the adsorbent for DSPFE combined with high-performance size exclusion chromatography (HPSEC), the conditions of vortex-assisted DSPFE were optimized to realize the economic (adsorbent amount: 5 mg), rapid (extraction time: 10 min), and efficient (recovery: 88.5–91.1%) extraction and analysis of laminarin and fucoidan in undaria pinnatifida. The adsorption process followed Freundlich isotherm (R2 ≥ 0.9792) and pseudo-second-order kinetics (R2 ≥ 0.9870). The proposed method showed good linearity (0.01–2 mg/mL, R2 ≥ 0.9990), limit of detection (0.027–0.114 mg/mL), limit of quantitation (0.089–0.379 mg/mL), accuracy (93.4–104.7%), and precision (2.2–5.6%). [ABSTRACT FROM AUTHOR]

• The review focuses on the quantification of endocrine disrupting chemical PAEs in beverages. • Methodologies proposed in last 20 years is reviewed (2000-2020). • Toxic effects on human exposure as well as the permissible levels of types of PAEs in beverages and liquid foods are considered. • Analytical methods and extraction techniques are described. • Analytical challenges in the assessment of PAEs are also mentioned. Phthalates (PAEs) are the class of lipophilic chemicals, which are used as additives in the manufacturing of plastics. It results in presence of PAEs in water and beverages because of their migration capacity. Their presence has attracted considerable attention due to their potential impacts on ecosystem functioning and public health. In addition, an enormous number of research articles have been published between 2000 and 2020, which have been identified and their results have been tabulated displaying PAEs analyzed, matrices, sample preparation, analytical method used, the limit of detection (LOD), and recovery percentages. Numerous sample preparation and analytical methods are found which are suitable for the reliable determination of the PAEs. The analysis of the PAEs is difficult due to their ubiquitous presence and their complexity, therefore suitable precautions, should be taken into account. In this review, we provide an overview of various pre-treatment measures and detection methods for PAEs in several types of water and beverages, mainly focusing on the last 20 years published works have been discussed. Pre-treatment methods mainly include liquid-liquid extraction (LLE), solid-phase extraction (SPE), solid-phase microextraction (SPME), liquid-phase microextraction (LPME), and many more rare techniques. Chromatographic and non-chromatographic techniques coupled with or without diodes, spectrophotometers, and detectors, have been described. The concept of "green analytical chemistry" for PAE determination has also been discussed. Hereby, the limitations and challenges in these applications are also included. [ABSTRACT FROM AUTHOR]

• CeO 2 NPs have different affinities to triterpene acids with different structure. • CeO 2 NPs have selective adsorption to triterpene acids. • Open-ring Lanostane-type triterpene acids- poricoic acid a and poricoic acid b can be separated preferentially and quickly. • Dispersive solid-phase extraction (D-SPE) based on CeO 2 NPs has high efficiency and low energy consumption for the separation and purification of triterpene acids. Researches on the adsorption for triterpene acids by cerium oxide nanoparticles (CeO 2 NPs) as adsorbent were carried out. The results demonstrated that CeO 2 NPs could selectively adsorb triterpene acids. Using triterpene acid standards as model compounds, the adsorption and desorption conditions were optimized. The adsorption was conformed to be a pseudo-first-order model and single-layer adsorption after being characterized by adsorption kinetics and adsorption thermodynamics. It has been found that the adsorption efficiency of open-ring type triterpene acids was better than that of closed-ring type triterpene acids. The CeO 2 NPs was successfully applied to enrichment and selective separation of triterpene acids in the crude extract of Poria cocos. The adsorption by CeO 2 NPs has the advantages of high efficiency, low energy consumption and high selectivity, and is expected to become an alternative to traditional triterpene acid separation techniques such as chromatographic separation methods and liquid-liquid extraction enrichment techniques. [ABSTRACT FROM AUTHOR]

Phthalate esters are high production volume chemicals and are widely used as additives in the plastics industry. Since they are not chemically bound to the plastics, they can easily leach into the environment. They can also be transformed into phthalate monoesters via degradation or metabolization. As numerous studies have reported the negative effects of phthalate diesters and monoesters on marine biota, these contaminants are an emerging concern. In this article we review the most important analytical methods for determining phthalate esters in seawater, marine sediments and biota. The QuEChERS method and ultrasound-assisted extraction are the most common techniques for extracting solid samples, while solid-phase extraction is the most common technique for seawater samples. We also describe the occurrence and distribution of phthalate esters in the marine environment. Bis(2-ethylhexyl) phthalate, di-n-butyl phthalate and diisobutyl phthalate, as well as their metabolites, are the main compounds detected in the reviewed matrices. • Methods for determining phthalates in seawater, sediments and biota are reviewed. • GC and LC are the most applied techniques for PAE and MPE separation, respectively. • Extraction and clean-up techniques for liquid and solid marine samples are compared. • The presence of PAEs and MPEs in seawater, sediment and biota samples is discussed. • Little information about MPEs in seawater and sediment samples is available. [ABSTRACT FROM AUTHOR]

Flavour analysis remains challenging due to the range of selectivity demands, from the extraction of multiclass volatile compounds to the purification of low-concentration odourants (e.g. organosulfur compounds) amidst the high food matrix noise. In this study, the varying selectivities of solid-phase extraction (SPE) were leveraged upon for both multiclass and organosulfur compound analysis, using coffee as a model matrix. Polymeric SPE (Bond Elut ENV) was screened for significant (p < 0.05) parameters affecting the recovery of 37 multiclass compounds, and the most influential parameters were optimised using a Box-Behnken design (elution solvent of 67:33 dichloromethane:ethyl acetate, loading pH of 4.8, and wash solvent of water). Following this, low-concentration organosulfur compounds which were challenging to detect in the complex coffee matrix were purified by adding a sequential SPE step for selectivity. A silver-based ligand-exchange SPE step (MetaSEP IC-Ag) was optimised for organosulfur compound recovery (wash solvents of dichloromethane and 43% acetonitrile in dichloromethane, elution solvent of 90 mmol/L 1,4-dithiothreitol in dichloromethane). This was found to be complementary to polymeric SPE's matrix clean-up effect (which improved average organosulfur compound recovery by 5.45 times). Finally, both multiclass and sequential organosulfur extraction techniques demonstrated good performance in terms of reproducibility (1.0–9.0%) and linearity (R 2 > 0.995), allowing for the detection of 3-mercapto-3-methylbutyl formate (3.741 ± 0.387 ng/mL) in coffee samples. In conclusion, this study highlights the potential for SPE to address a variety of complex flavour analysis demands with the appropriate selection and combination of solid-phases. [Display omitted] • Novel sequential solid-phase extraction for multiclass and organosulfur volatiles. • Polymeric SPE selection and optimisation for recovery of multiclass volatiles. • Sequential optimisation of ligand-exchange sorbent improved organosulfur selectivity. • Polymeric SPE step simplified complex samples to enhance ligand-exchange recovery. • Application of sequential SPE to purify organosulfurs from complex coffee matrix. [ABSTRACT FROM AUTHOR]

• Analytical methods of lipid-soluble vitamins (LSVs) in different milk sources were critically reviewed. • Saponification process is very important step for the recovery of LSVs from milk samples. • LC-MS is the most common method for the quantification of LSVs in milk samples. • Ion mobility MS appears to be suitable for separation and quantification of LSVs in milk samples. Milk and dairy products are considered as essential sources of lipid-soluble vitamins (LSVs) for human nutrition. Due to the lower concentrations, complexity, and instability of LSVs during extraction, their quantification remains challenging. This review focus on advances in the extraction and quantification of LSVs from different dairy products. Saponification, and liquid-liquid (LLE), solid-phase (SPE), and supercritical fluid (SFE) extraction methods, as well as dispersive liquid-liquid microextraction, are the most common techniques. Liquid chromatography-mass spectrophotometry (LC-MS) has unique advantages for LSVs determination and quantification due to its high sensitivity and specificity. [ABSTRACT FROM AUTHOR]

• Amino-containing MOFs MIL-125-NH 2 was designed as a new sorbent in d-SPE. • MIL-125-NH 2 enrich the target analytes directly to improve sensitivity. • Amino-containing MIL-125-NH 2 has good adsorption capacity. • The detection limits were lower than most of traditional methods. • MIL-125-NH 2 is recovered easily and reused at least 8 times. A simple, environmentally-friendly and reliable method was developed to simultaneously monitor the residue of methyl 1-naphthalene acetate, parathion-methyl, fenitrothion, bromophos and phenthoate in pomelo by using dispersive solid-phase extraction technique (d-SPE). In this method, these target analytes were captured by MIL-125-NH 2 and detected by GC–MS/MS. The key parameters of d-SPE were optimized by the single factor experiment. Under the optimized conditions, a good determination coefficient (R2 > 0.9922) and extraction recoveries (64.7–116.8%) are obtained. The limit of detections (0.03–1.07 ng/g) is lower than the MRLs in citrus fruits established by EU (10–15000 ng/g) and China (10–10000 ng/g). The precisions of intra-day and inter-day are 1.3–8.9% and 3.8–14.9%, respectively. In addition, the sorbent MIL-125-NH 2 is stable and can be reused at least eight times. These results prove the established method is efficient and reliable to detect the pesticide residues in pomelo. [ABSTRACT FROM AUTHOR]

A novel COF-based smart adsorbent of Fe 3 O 4 @C 3 N 4 @COFs was fabricated via a versatile layer-by-layer assembly strategy and applied to the simultaneous selective recognition, detection, and removal of profenofos. [Display omitted] • Multifunctional ternary Fe 3 O 4 @C 3 N 4 @covalent organic framework was synthesized and characterized. • The adsorbent was used for adsorption and detection of profenofos by HPLC-MS/MS. • The optimized method characterized low LODs, wide linearity, and good repeatability. • Composite materials were applied to the analysis of apple grapes and oranges samples. In this study, a magnetic composite material was prepared based on covalent organic framework (COFs) materials for the detection of trace organophosphorus pesticides. Fe 3 O 4 @C 3 N 4 @COFs were synthesized by a layer-by-layer assembly strategy and applied to the selective identification, detection and removal of profenofos pesticides using magnetic solid-phase extraction technique. After seven regeneration cycles, the composite exhibited excellent selectivity and affinity for profenofos, and eventually still achieved an extraction efficiency higher than 75%. Under optimized conditions, the proposed magnetic solid-phase extraction method coupled with high-performance liquid chromatography-tandem mass spectrometry showed a low limit of detection (1 × 10−5 μg/mL) for profenofos. The developed method was successfully used to detect profenofos in spiked fruit samples with satisfactory recoveries (74.33% −116.59%) and relative standard deviations (0.27% −7.41%). This study highlights the potential of COFs-based magnetic composites in sample pretreatment for targeted analysis and is a novel pathway for efficient sample preparation in food safety analysis. [ABSTRACT FROM AUTHOR]

Bisphenol A (or BPA) is a toxic endocrine disrupting chemical that is released into the environment through modern manufacturing practices. BPA can disrupt the production, function and activity of endogenous hormones causing irregularity in the hypothalamus-pituitary-gonadal glands and also the pituitary-adrenal function. BPA has immuno-suppression activity and can downregulate T cells and antioxidant genes. The genotoxicity and cytotoxicity of BPA is paramount and therefore, there is an immediate need to properly detect and remediate its influence. In this review, we discuss the toxic effects of BPA on different metabolic systems in the human body, followed by its mechanism of action. Various novel detection techniques (LC-MS, GC-MS, capillary electrophoresis, immunoassay and sensors) involving a pretreatment step (liquid-liquid microextraction and molecularly imprinted solid-phase extraction) have also been detailed. Mechanisms of various remediation strategies, including biodegradation using native enzymes, membrane separation processes, photocatalytic oxidation, use of nanosorbents and thermal degradation has been detailed. An overview of the global regulations pertaining to BPA has been presented. More investigations are required on the efficiency of integrated remediation technologies rather than standalone methods for BPA removal. The effect of processing operations on BPA in food matrices is also warranted to restrict its transport into food products. [Display omitted] • Toxicity, mechanism of action and environmental impact of BPA was analyzed. • BPA degrades faster in freshwater (half life = 4.6 days) than in seawater (> 30 days). • Major pretreatment and detection strategies for BPA have been discussed. • Biological degradation and adsorption strategies for remediation are currently effective. • BPA intake has been restricted to ≤ 50 μg/kg body weight per day, globally. [ABSTRACT FROM AUTHOR]

• Solid-phase extraction was the technique used to purify pigments. • The pigments investigated were obtained from a microalga. • A commercial resin was applied of the separation of chlorophylls from other pigments. • Ionic liquids were successfully used to elute chlorophylls from the resin. • The continuous process in a column was also performed with success. There is a need for handy and fast techniques to purify biomolecules, increasing their stability and value, because the separation units are current bottlenecks in downstream processes. Solid-phase extraction is a technique that enables the purification of a compound by its adsorption from a liquid matrix. The AmberLite™ HPR900 OH resin allows the separation of chlorophylls from complex extracts, however the recovery of the chlorophylls is not easy to achieve. An innovative procedure to elute the chlorophyll from AmberLite™ HPR900 OH, based on the use of aqueous solutions of surface-active ionic liquids is proposed in this work. The operational conditions were optimized, showing that the resin can be reused for at least five cycles without losing its efficiency and the chemical structures of the pigments recovered were identified. [ABSTRACT FROM AUTHOR]

[Display omitted] • The proposed CPME scheme can be easily used in routine bioanalysis. • CPME is an interesting alternative to traditional preparation approaches. • Accuracy profiles were implemented for method validation. • A sol–gel polytetrahydrofuran sorbent was used for the extraction of ibuprofen. Undoubtedly, the exploration of new sample preparation techniques is in the forefront of research in bioanalysis. Capsule phase microextraction (CPME) is a recently introduced extraction technique based on the sol–gel sorbents which are incorporated into a porous tubular polymeric membrane. Herein, we exploited the advantageous features of CPME in biological matrices by utilizing sol–gel poly(tetrahydrofuran) (sol–gel PTHF) sorbent in CPME device for the extraction of ibuprofen (model compound) from urine samples. In CPME, both filtration and stirring mechanisms are merged into a unified extraction device allowing the direct extraction of the analytes from biological matrix without any pretreatment process. The main parameters (sample pH and volume, adsorption and elution time, volume of elution volume etc.) affecting the extraction efficiency of the CPME method were systematically investigated and optimized. The determination of ibuprofen was performed using UHPLC-PDA. The reported method was validated in terms of linearity, selectivity, accuracy, and precision, limit of detection and limit of quantification using the total error concept. Employing the accuracy profiles – as a graphical decision-making tool – the β -expectation tolerance intervals did not exceed the acceptance criteria of ± 15% meaning that 95% of future results will be included in the defined bias limits. The limit of detection (LOD) of the method was adequate, corresponding to 14 ng mL−1. The relative bias in the spiking levels was acceptable being in the range of −4.1 and +3.9% while the relative standard deviation (RSD) was lower than 4.6%. Moreover, the sol–gel sorbent integrated microextraction capsules were found to be reusable for at least 20 extraction cycles. The CPME protocol was successfully employed for the analysis of real urine samples obtained by a healthy volunteer. Finally, the developed CPME method was characterized by absence of matrix-effect and thus its application can be potentially expanded to other types of biological matrices. [ABSTRACT FROM AUTHOR]

Because of its many advantages, solid phase extraction (SPE) is considered to be the best process for removing heavy metals from water. Ion-imprinted polymers (IIPs) have been broadly used in the last decade as SPE adsorbents for the retention of metals ions from aqueous solutions. This itemized review list thorough literature over the last decade from 2010 until present and highlights the main results related to adsorption studies where IIPs are used as SPE adsorbents for the selective separation of heavy metals. In the first part of this review elaboration methods, components, and major polymerization techniques to produce IIPs have been described. In the second part, synthesis parameters, adsorption performance and a descriptive analysis of SPE of heavy metals by IIPs have been provided. In this review it is underlined that there are many parameters to optimize in order to obtain the required performance of the IIPs. These parameters are mainly linked to synthesis process and one of the most important is the synthesis of new ligands to improve the selectivity with respect to the target ion. Application of IIPs as solid-phase extraction adsorbents for the removal of heavy metals in solution. [Display omitted] • Main techniques for the preparation of IIPs are described, with their main advantages. • Classification of relevant experimental parameters in the synthesis of IIPs reported in the last decade. • Special focus in the application of IIPs as SPE adsorbents for the selective separation of heavy metals from simple and complex media. [ABSTRACT FROM AUTHOR]