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• Early prognosis of neuroblastoma in infants must be a priority to act against it asap. • The neuroblastoma prognosis can based on the study of catecholamines metabolites from urine. • Catecholamine metabolites from baby pee-covered diapers were detected by CE-UV. • Disposable diapers were employed as sampling devices to collect the urine. • The variables of the sample preparation step were optimized and the method was validated. A method has been developed for the analysis of vanillylmandelic acid, homovanillic acid, and 5-hydroxyindoleacetic acid from baby urine as biomarkers of neuroblastoma in infants. Disposable diapers were employed as sampling devices in order to guarantee a low invasiveness during this step. The proposed method consists on a simple extraction step with water from the used diaper followed by the measurement using capillary electrophoresis with UV detection. The Box-Behnken design (BBD) was utilized to optimize the process of extracting catecholamine metabolites from the examined samples. The variables of the sample preparation step were optimized and the method was validated obtaining limits of quantification of 1.65 μg mL−1, good intraday and inter-day precision with RSDs under 15 %. Finally the method was applied to real samples collected from the Department of Neonatology, University Clinical Centre (Gdańsk, Poland). The greenness of the proposed method was also evaluated with different tools (i.e., AGREEPrep and GAPI) with satisfactory results, which allow to state that the method can be considered green. Moreover, its practicality was evaluated by application of BAGI tool, proving to be a practical and economical method to be applied in routine laboratories for determination of catecholamine metabolites in urine-type samples. [ABSTRACT FROM AUTHOR]

• Media for biological sample preparation presented. • Media integrated analytical technique for biomarkers analysis. • Perspectives of media promote biological sample preparation. The analysis of biological samples is highly valuable for disease diagnosis and treatment, forensic examination, and public safety. However, the serious matrix interference effect generated by biological samples severely affects the analysis of trace analytes. Sample preparation methods are introduced to address the limitation by extracting, separating, enriching, purifying trace target analytes from biological samples. With the raising demand of biological sample analysis, a review focuses on media for biological sample preparation and analysis over the last 5 years is presented. High-performance media in biological sample preparation are first reviewed, including porous organic frameworks, imprinted polymers, hydrogels, ionic liquids, and bioactive media. Then, application of media for different biological sample preparation and analysis is briefly introduced, including liquid samples of body fluids, solid samples (hair, feces, and tissues), and gas samples of exhale breath gas. Finally, conclusions and outlooks on media promoting biological sample preparation are presented. [ABSTRACT FROM AUTHOR]

• Simple, applicable and reproducible extraction method was developed for PAHs. • IL/IL-96(Al) provided high extraction efficiency for PAHs. • The suggested method provided low LODs and wider linear ranges for PAHs. • The method was successfully applied in the analysis of PAHs in real samples. Aluminum-based metal organic framework composite containing ionic liquid was prepared and used as sorbent for extraction of sixteen polycyclic aromatic hydrocarbons in list of priority pollutants of United States Environmental Protection Agency before their analysis by gas chromatography/mass spectrometry. The dispersive micro solid-phase extraction method, known as a simple and fast method, was preferred as the extraction method. The optimized parameter conditions were 5 mL of sample solution, 10 min sonication by ultrasonic bath, 30 mg of sorbent, 30 °C extraction temperature, 0.1 mL of hexane as elution solvent with 5 min elution time. The suggested method presented that limit of detection and limit of quantification were in the range of 0.01–0.10 μg l -1, and 0.04–0.33 μg L-1, respectively. The intra-day and inter-day repeatability were within the ranges of 1.18–4.88 % and 1.02–5.06 %, respectively. The recoveries for polycyclic aromatic hydrocarbons in peach juice, cherry juice, tap water and rain water samples were obtained in the range of 84.9–99.9 % for spiked 5, 50 and 100 μg l -1 standard polycyclic aromatic hydrocarbons solution. [ABSTRACT FROM AUTHOR]

• This review focuses on terpenoids extracted from essential oils. • Terpenoids have enantiomers with distinct physiological activities. • Predominant extraction methods are HD, SFME, HS-SPME and supercritical fluid. • 2D GC is found to have stronger chiral chromatography resolution ability. • Specific distribution and enantiomer excess results could be used as quality markers. Terpenoids possess significant physiological activities and are rich in essential oils. Some terpenoids have chiral centers and could form enantiomers with distinct physiological activities. Therefore, the extraction and separation of terpenoids enantiomers are very important and have attracted extensive attention in recent years. Meanwhile, the specific distribution and enantiomer excess results (the excess of one enantiomer over the other in a mixture of enantiomers) could be used as quality markers for illegitimate adulteration, origin identification, and exploring component variations and functional interrelations across different plant tissues. In this study, an overview of the progress in the extraction of terpenoids from essential oils and the separation of their enantiomers over the past two decades has been made. Extraction methods were retrieved by the resultant network visualization findings. The results showed that the predominant methods are hydrodistillation, solvent-free microwave extraction, headspace solid-phase microextraction and supercritical fluid extraction methods. GC–MS combined with chiral chromatography columns is commonly used for the separation of enantiomers, while 2D GC is found to have stronger resolution ability. Finally, some prospects for future research directions in the extraction and separation identification of essential oils are proposed. [ABSTRACT FROM AUTHOR]

• Extraction of mRNA from LNPs is required to control the quality of mRNA in final drug products. • Different methods have been compared to extract mRNA from LNPs. • Advantages and disadvantages of the different methods are highlighted. • Selection should be based on the method's efficiency, duration, ease of use, automation level, and use of toxic reagents. Messenger RiboNucleic Acid (mRNA) vaccines have recently shown considerable promises for both prophylactic and therapeutic vaccines. These vaccines do not carry an antigen but the information for producing it using the cell machinery, turning the human body into an antigen factory. However, mRNA is an unstable molecule, susceptible to physical, chemical and enzymatic degradation by exo- and endonucleases. If the mRNA is degraded, it can no longer be translated correctly into the antigen of interest and the vaccine lose its efficacy. To protect from nucleases degradation and allow it to get into the cells, mRNA can be encapsulated in lipid nanoparticles (LNPs). As part of the manufacturing process, the quality of the mRNAs should be controlled before the encapsulation (at the drug substance stage) as well as after formulation on the final vaccine product (at the drug product stage). Therefore, it is necessary to be able to extract the mRNA from the LNPs, that is to deformulate the final vaccine product. In this work, different deformulation methods have been compared: spin column extraction, magnetic particle extraction, organic extraction, and direct disruption. Advantages and disadvantages of each of these methods are highlighted. [ABSTRACT FROM AUTHOR]

• Ionic DESs like choline-based DES, are green solvents similar to ionic liquids. • They are most popular DESs and wined wide application. • This review summarized current ionic DESs including composition and application. • Especially for application in natural products extraction and separation. Room ionic liquids (ILs) used as green solvents have received considerable attention and wide application in different research and industrial fields, such as chemistry, biology, catalysis, energy, and even environmental sciences. Recently, a new class of sustainable solvents named deep eutectic solvents (DESs) have been developed, which share the promising solvent characteristics of ILs, such as thermal and chemical stability, low vapor pressure and design ability. In addition, the major advantages of DESs over ILs are their lower prices and easier preparation. Therefore, DESs have been considered to be a potential alternative to replace conventional organic solvents and ILs. Currently, the developed DESs may be classified into ionic and nonionic liquids. Typically, choline chloride (ChCl)/urea (1:2) is an ionic DES, while glucose/sucrose (1:1) is a nonionic DES. Although several reviews have covered advancements in DESs, in this review, we aim to provide a general insight into DESs, particularly ionic DESs, like choline-based DES, in terms of their preparation and application in the extraction of natural products (NPs) mainly from traditional Chinese medicines and the recovery of extracted compounds from their extracts. Additionally, various factors affecting the extraction efficiency of DESs are discussed. [ABSTRACT FROM AUTHOR]

• A new method for the analysis of cannabinoids in honey was developed. • A QuEChERS extraction procedure with an un-buffered method was optimised. • RP-HPLC with ESI-MS/MS detection was used for qualitative and quantitative analysis. • The method was applied to honey samples from different floral sources. • Honey from Cannabis sativa L. was analysed for the first time. Fibre-type Cannabis sativa L. (hemp) represents a valuable resource in many different fields, including both the pharmaceutical and food ones. This plant contains non-psychoactive cannabinoids, a class of bioactive compounds biosynthesized in both female and male inflorescences. Among them, cannabidiol (CBD) is the most interesting compound from a medicinal point of view. Indeed, several scientific studies have proved its therapeutic potential in a large number of pathologies, in addition to its biological effects attributable to its antioxidant, neuroprotective and anti-inflammatory properties. The analysis of the amount of cannabinoids in food and food supplements represents a critical issue in the ambit of both the quality assurance and the dietary intake control of these biologically active compounds. In this ambit, a particular attention is necessary for apiary products, since they are widely consumed and they can be produced by bees starting from different floral sources. In the light of all the above, the aim of this study was to develop for the first time a new analytical method based on RP-HPLC with ESI-MS/MS detection for the determination of CBD and related cannabinoids in honey. A quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction procedure with an un-buffered method was selected and optimised as the more suitable protocol. As regards detection, it was carried out by using a linear ion trap quadrupole (QTRAP) mass analyser, operated in the multiple reaction monitoring (MRM) mode. Hemp male inflorescences and pollen were analysed in parallel by means of HPLC-UV/DAD, since bees can transfer pollen into their hives and, consequently, into beehive products. The method developed and validated for the first time in this work was finally applied to the analysis of cannabinoids in honey samples, thus demonstrating to be a useful tool for both quality control and safety assurance. [ABSTRACT FROM AUTHOR]

Highlights • Single-laboratory validation of a new method for folate quantification in food. • The single-enzymatic extraction step is used for folate analyses in food. • A plant origin hydrolase enables folate deglutamylation within 1 h. • Conversion between 10-HCO-PteGlu, 5,10-CH+=H 4 folate and 5-HCO-H 4 folate is studied. • 50% of 5,10-CH+=H 4 folate is converted into 5-HCO-H 4 folate during folate analysis. Abstract A rapid, sensitive and reproducible method for analysis of naturally-occurring folates and folic acid in food has been developed and validated. A single-enzyme extraction step, in which a pure recombinant enzyme of plant origin (Arabidopsis thaliana) was used, enabled fast and reproducible deglutamylation during folate extraction within the incubation time of 1 h. Six commonly occurring folate forms (tetrahydrofolate, 5,10-methenyltetrahydrofolate, 10-formylfolic acid, 5-formyltetrahydrofolate, folic acid and 5-methyltetrahydrofolate) were detected and quantified in 9 min using liquid chromatography-tandem mass spectrometry (LC–MS/MS). 13C 5 -labeled 5-formyltetrahydrofolate, 13C 5 -labeled folic acid and 13C 5 -labeled 5-methyltetrahydrofolate were used as internal standards for the quantification. The method is described by a calibration curve (R2>0.99 and trueness 85–115%), a limit of quantification at 0.1 μg/100 g, trueness at 80–120% in spiked samples and certified reference materials, and a precision <10%. However, the precision in quantification of tetrahydrofolate was not within the acceptable limits due to the lack of use of the corresponding internal standard. An interconversion study of unstable formyl forms was performed which showed that 50% of 5,10-methenyltetrahydrofolate is converted to 5-formyltetrahydrofolate during the analysis. The developed LC–MS/MS method is a candidate for a future standard method for folate analysis in food. [ABSTRACT FROM AUTHOR]

Highlights • Ability and reliability of six methods to recover lipids from artery were evaluated. • A dichloromethane-based extraction method was the most efficient one. • Lipids were separated by class, identified and quantified by UHPSFC/QTOF-MS/MS. • The extraction method affects fragmentation of monoacylglycerols in the ion source. Abstract Pulmonary artery grafts are needed as cardiovascular bioprosthetics. For successful tissue recellularization after transplantation, lipids have to be removed from the donor artery. Developing a selective process to remove lipids without damaging the extracellular matrix greatly depends on knowing the amount and type of lipid compounds in the specific tissue. Here we present an efficient methodology for the study of lipids present in porcine pulmonary arteries. The performance of six extraction methods to recover lipids from artery was evaluated. For this purpose, a supercritical fluid chromatography method coupled to quadrupole time-of-flight mass spectrometry detection (UHPSFC/QTOF-MS) was adapted. The method enabled separation of lipids of a wide range of polarity according to lipid class in less than 7 min. One dichloromethane-based extraction method was shown to be the most efficient one for the recovery of lipids from pulmonary artery. However, one MTBE-based extraction method was able to show the highest fatty acid extraction yields (to the expense of longer extraction times). Lipids were relative quantified according to class, and the major species within each class were identified. Triacylglycerols and glycerophospholipids were the most abundant classes, followed by sphingomyelins, monoacylglycerols and fatty acyls. The matrix effect exerted no interference on the analytical method, except for some few combinations of extraction method and lipid class. These results are of relevance for lipidomic studies from solid tissue, in particular for studies on pulmonary and cardiovascular diseases. Finally, our work sets the basis for the further development of a selective processes to remove lipids from pulmonary artery without damaging the tissue prior to transplantation. [ABSTRACT FROM AUTHOR]

Highlights • Importance of volatile oxygenated organic compounds (O-VOC) analysis in effluents. • Comprehensive review on GC applications for the determination of O-VOC in effluents. • Discussion on advantages and issues of each alternative analytical protocols. • Current trends and novelties in research of wastewater samples. Abstract The paper is a review of the procedures for the determination of volatile and semivolatile oxygenated organic compounds (O-VOCs) in effluent samples by gas chromatography. Current trends and outlook for individual steps of the procedure for the determination of O-VOCs in effluents are discussed. The available sample preparation techniques and their limitations are described along with GC capillary columns used for O-VOCs separation and selective and universal detectors used for their determination. The results of determination of O-VOC content in various types of real effluents are presented. The lack of legal regulations regarding the presence of the majority of O-VOCs is pointed out as well as the availability of just a few procedures allowing a comprehensive evaluation of the O-VOC content in effluents. [ABSTRACT FROM AUTHOR]

Highlights • ELM containing tropine IL was prepared and applied for the first time. • The new system can enrich tropane alkaloids from herb and drug. • A high extraction efficiency and satisfactory selectivity were obtained. • Phase/separation behaviors and mechanism were explored in detail. Abstract Emulsion liquid membrane (ELM) coupled with tropine-based ionic liquid was prepared and successfully adopted for the extraction and quantitative analysis of tropane alkaloids (TA) in Radix physochlainae. Effects of formation conditions of ELM were explored and then optimized; the ideal oil-water mass ratio was determined to be 1:2.5, chloroform, Span 80 and 0.05 mol L−1 N -propyl-tropine hexafluorophosphate ([C 3 Tr][PF 6 ]) aqueous solution were stirred for 30 min with the speed of 1500 r min-1. In order to extract and enrich TA with ELM efficiently, key factors related with their extraction efficiency such as stirring speed, volume of the extracts (feed solution), migration time and initial concentration of TA were systematically investigated. Under optimal conditions, 1.5 mL extracts containing 1.6 mg mL−1 of TA was stirred with ELM at 250 r min-1 for 5 min, the extraction efficiency of target alkaloid can reach 94.14%. Finally, the method could be used in quantitative analysis of TA in herbal material and patent medicine after demulsification. By comparison, application of ELM for the enrichment and quantitation of TA offers a more straightforward and effective strategy, which is expected to provide a meaningful reference for similar separation processes. [ABSTRACT FROM AUTHOR]

Highlights • First use of ethanol-water mixture to produce pressurized vapor in the DIC process. • Optimized DIC was applied to extract essential oil from Hyssopus officinalis L. • The optimal DIC yield was higher than HD, UAE and Soxhlet methods. • SEM revealed significant structure modifications caused by the DIC process. Abstract To determine the optimum condition for the extraction of Hyssopus officinalis L. essential oil (EO) by instant controlled pressure drop (in French: Détente Instantanée Contrôlée or DIC), the influential parameters of pressure, heating time per cycle, number of cycles, mean particle diameter of the herb, and water concentration in the steam generator feed were evaluated using response surface methodology (RSM). The impact of using an ethanol-water mixture to generate the required vapor in the DIC process on EO extraction was investigated. The optimum condition was found to be at pressure = 1 bar, heating time = 100 s, cycles = 12, particle diameter = 1 mm, and water concentration = 80 v%. The addition of ethanol turned out to be more efficient at higher heating times and cycle numbers. The optimum yield in DIC was highest compared with hydrodistillation (HD), ultrasound-assisted extraction (UAE), and Soxhlet (SOX) methods; their values, expressed as total area percentages per internal standard area percentage, were 39.04, 10.98, 1.58, and 7.71, respectively. Comparison of the four methods also indicated that the DIC-EO was of a superior quality. The analysis of the DIC-treated residual herb in the optimum experiment revealed that unlike the low amount of valuable oxygenated monoterpenes, the availability of sesquiterpenes increased, which proved that DIC performs selectively while extracting more valuable EO components. The DIC-EO and its extract were examined for total phenolic content (TPC) and antioxidant activity using Folin-Ciocalteu and DPPH assay, respectively. Comparison of these results with those obtained from HD demonstrated higher TPC and antioxidant activity of the DIC-EO. Moreover, scanning electron microscopy (SEM) of the raw material and residual herb in the optimum experiment showed significant structure modifications induced by the DIC process. [ABSTRACT FROM AUTHOR]

• A novel LC‒MS/MS method detects bronopol in aquatic tissues with high sensitivity. • Optimized extraction and cleanup steps yield reliable quantification of bronopol. • Calibration curves show excellent linearity for fish, shrimp, crab, and shellfish matrices (r > 0.99). • The developed method successfully addressed the challenge of extracting bronopol from aquatic products. • Successful validation supports method's potential for safeguarding aquatic product quality and public health. Fish farming plays a vital role in providing food, nutrition, and employment globally. However, this industry faces security challenges, necessitating the use of fungicides and preservatives, such as bronopol, to increase product yields. Bronopol (2‑bromo-2-nitropropan-1,3-diol; CAS:52–51–7) is widely used in various fields, including food production, cosmetics, and, more recently, aquaculture. Currently, there is a limited number of techniques available for detecting bronopol in aquaculture products. This is primarily due to bronopol's instability, susceptibility to degradation, and tendency to form precipitates that pose challenges in extraction from aquaculture products. For this issue, this study presents a comprehensive method for detecting bronopol content in aquaculture tissues using liquid chromatography-tandem mass spectrometry (LC‒MS/MS). The methodology was optimized, involving extraction with Cu-Zn precipitant, cleanup using a small HLB column, separation on a T3 column, and gradient elution with water and acetonitrile mobile phases. The quantitative approach was employed without the use of an internal standard, following the external standard method. The spiked recoveries at 3 fortification levels (0.1, 0.2, and 1 mg/kg) ranged from 87.1 % to 108.1 % with relative standard deviations RSD ≤ 9.0 %. By applying this method to fresh fish, shrimp, crab, and shellfish samples from a local supermarket, no residues of bronopol were detected, ensuring the reliability of the results. The simplicity, rapidity, and high sensitivity of the method make it a suitable alternative to conventional techniques for bronopol detection. Moreover, the successful validation of the method's recovery and precision supports its potential application in monitoring and preventing the misuse of bronopol in aquaculture, thereby safeguarding aquaculture product quality and protecting public health. [ABSTRACT FROM AUTHOR]

Highlights • Efficient method for the extraction of the anti-inflammatory drug by nano-sorbent. • Representing excellent linearity, recovery, LOD and RSD by SPE technique with HPLC. • Developed method for dendritic β-CD in order to obtain high sorption capacity. Abstract This study introduced a developed approach for dendritic β-cyclodextrin (β-CD) in order to obtain high sorption capacity. Synthetic strategy exploits the reactivity between acrylic acid and allyl glycidyl ether for high-yielding assembly via grafting on to the magnetic nanoparticles that are modified using 3-mercaptopropyltrimethoxysilane for various building branches and host–guest molecules of β-CD. The methodology has been applied for the preparation of a series of β-CD conjugated magnetic nanoparticles with dendrimers as a nano-sorbent for the extraction of methylprednisolone acetate. This study allowed us to probe (i) the effects of the dendric-cyclodextrin architecture on the affinity of sorption capacity, (ii) the drug influence between the cyclodextrin core and the polyester dendrimer, and (iii) the result of sorbent formation for using the anti-inflammatory drug as a target guest into the ring of β-CD on biological extraction. It was found that the adsorption behavior could be fitted by the Langmuir adsorption isotherm model. The adsorption capacity of MPA is found to be 12.4 mg g−1 and indicated the homogeneous sites onto polymer grafted magnetite nano-sorbent surface. Our results confirm the high capability of this type of dendrimer-β-CD for drug extraction in biological fluids and pharmaceutical samples. This nano-sorbent assists the magnetic solid phase extraction technique represented in the high extraction yield (up to 97%) for methylprednisolone acetate in biological human fluids and pharmaceutical samples. Moreover, the achieved polymeric nano-sorbent of the reaction combination was facilitated by a magnetic field and reusability was performed without any notable loss in the sorbent activity. [ABSTRACT FROM AUTHOR]

Human activities are responsible for the release of innumerous substances into the aquatic environment. Some of these substances can be used as pollution tracers to identify contamination sources and to prioritize monitoring and remediation actions. Thus, their identification and quantification are of high priority. However, due to their presence in complex matrices and at significantly low concentrations, a pre-treatment/concentration step is always required. As an alternative to the currently used pre-treatment methods, mainly based on solid-phase extractions, aqueous biphasic systems (ABS) composed of ionic liquids (ILs) and K 3 C 6 H 5 O 7 are here proposed for the simultaneous extraction and concentration of mixtures of two important pollution tracers, caffeine (CAF) and carbamazepine (CBZ). An initial screening of the IL chemical structure was carried out, with extraction efficiencies of both tracers to the IL-rich phase ranging between 95 and 100%, obtained in a single-step. These systems were then optimized in order to simultaneously concentrate CAF and CBZ from water samples followed by HPLC-UV analysis, for which no interferences of the ABS phase-forming components and other interferents present in a wastewater effluent sample have been found. Based on the saturation solubility data of both pollution tracers in the IL-rich phase, the maximum estimated concentration factors of CAF and CBZ are 28595- and 8259-fold. IL-based ABS can be thus envisioned as effective pre-treatment techniques of environmentally-related aqueous samples for a more accurate monitoring of mixtures of pollution tracers. [ABSTRACT FROM AUTHOR]

In recent years, there has been an increasing worldwide interest in the use of alternative sample preparation methods that are proceeded by separation techniques. Fused deposition modeling (FDM) is a 3D printing technique that is based the consecutive layering of softened/melted thermoplastic materials. In this study, a group of natural steroids and sexual hormones – namely, aldosterone, cortisol, β-estradiol, testosterone, dihydrotestosterone, and synthetic methyltestosterone and betamethasone – were separated and determined using an optimized high-performance liquid chromatography coupled to mass spectrometry (LC–MS) method in positive ionization mode. 3D-printed sorbents were selected as the pre-concentration technique because they are generally low cost, fast, and simple to make and automate. Furthermore, the use of 3D-printed sorbents helps to minimize potential errors due to their repeatability and reproducibility, and their ability to eliminate carry over by using one printed sorbent for a single extraction of steroids from biological matrices. The extraction procedure was optimized and the parameters influencing 3D-printed Layfomm 60 ® based sorbent and LC–MS were studied, including the type of extraction solvent used, sorption and desorption times, temperature, and the salting-out effect. To demonstrate this method’s applicability for biological sample analysis, the SPME-LC–MS method was validated for its ability to simultaneously quantify endogenous steroids. This evaluation confirmed good linearity and an R 2 that was between 0.9970 and 0.9990. The recovery rates for human plasma samples were 86.34–93.6% for the studied steroids with intra- and inter-day RSDs of 1.44–7.42% and 1.44–9.46%, respectively. To our knowledge, this study is the first time that 3D-printed sorbents have been used to extract trace amounts of endogenous low-molecular-weight compounds, such as steroids, from biological samples, such as plasma. [ABSTRACT FROM AUTHOR]

The medicinal compositions or active components in medicinal plants are the major sources to find new drugs or lead compounds. Exploring novel sorbents with good selectivity for extraction and separation of medicinal compositions or active components from complex medicinal plants are interesting and challenging. Metal-organic frameworks (MOFs) show great potential in adsorption and extraction recently. Herein, we report our primary attempt of zeolitic imidazolate framework-8 (ZIF-8) as a model MOF for selective extraction of a flavonoid named 3,4-dihydroxy-8,9-methylenedioxypterocarpan (compound 1) from a traditional medicinal plant Caragana Jubata. The enrichment factor of ZIF-8 for compound 1 is 57.7. The recoveries of compound 1 at three spiked levels (50, 100, 150 mg L −1 ) in Caragana Jubata dichloromethane extract are 62.1%, 66.4%, and 75.4%, respectively, with the relative standard deviations of less than 2.9%. The compound 1 also gave good linearity ( R 2 of 0.999) in the concentration range of 5–1000 mg L −1 . The obtained compound 1 gave highly antioxidant activity (DPPH radical scavenging rate of 79.03%, inhibitory rate on lipid peroxidation of 75.30%, which were higher than the positive controls Vitamin C and BHT) and low IC 50 values (5.438 ± 0.068, 20.970 ± 0.083 μg mL −1 for DPPH radical scavenging activities and inhibitory effects on lipid peroxidation, respectively). These results demonstrated the feasibility of MOFs in selective extraction of medicinal compositions or active components from complex medicinal plants. The current work may open a new way of MOFs in selective extraction of pharmacological active components from medicinal plants. [ABSTRACT FROM AUTHOR]

Essential oils extraction from Bunium Persicum (Boiss) was performed using instant controlled pressure drop (in French: Détente Instantanée Contrôlée or DIC) thechnology and optimum extraction conditions were obtained. Response surface methodology (RSM) was used to determine the optimal conditions and the results were 20 s heating time, 3.5 bar pressure, 0.44 mm particle diameter and 9 cycles. Essential oils extraction was also compared with Hydrodistillation (HD), ultrasound-assisted extraction (UAE) and Soxhlet (SOX) extraction. Results show higher efficiency of the DIC than other methods and more oxygenated components were observed. Impact of DIC, HD, UAE and SOX on the morphological structure of the plant was studied by SEM. Antioxidant activity and total phenolic content (TPC) of the extract were determined and comapred by HD. Results show that DIC facilitates achieving to higher TPC and more antioxidant activity. [ABSTRACT FROM AUTHOR]

• A novel solid-supported ABS is characterized for the sorption of dyes. • Dye uptake by a commercial sorbent (ABEC) was measured under the same conditions. • The capacity, kinetics, and sorption efficiency of the two materials are comparable. • Unlike ABEC, dye sorption on the supported ABS can be readily "tuned". • Dye recovery from the supported ABS leads to loss of the biphasic system, however. An aqueous biphasic system (ABS) comprising solutions of ammonium sulfate and polyethylene glycol-2000 (PEG-2000) in which the latter is supported on a porous polymeric substrate (Amberlite XAD-16) has been characterized by examining its performance in the removal of dyes from aqueous solution. Comparison of its behavior to that of a commercial sorbent (ABEC) consisting of a polyethylene glycol covalently bound to a polymer support indicates that the capacity, uptake kinetics, and efficiency of the supported ABS are comparable or superior to that of the ABEC resin. In addition, results obtained at various PEG-2000 concentrations and with PEGs of a range of molecular weights demonstrate that in contrast to ABEC resin, the behavior of a supported ABS can be readily "tuned" to provide the desired dye retention. The relative retention of various dyes is not generally predictable from their behavior in an analogous liquid-liquid system, however, the apparent result of synergistic effects between the XAD-16 support and the PEG phase. [ABSTRACT FROM AUTHOR]

Layered double hydroxides (LDHs) are ideal sorbents for solid phase extraction (SPE) because of the excellent ion exchange capacity and high specific surface area. However, difficult elution of the analytes from the LDHs is a problem due to the strong ionic interaction between anions and LDHs. High concentrated NaOH solution is employed to elute the sample, but it not suitable for analyzing by HPLC. To solve this problem, a simple acid-base neutralization method was proposed after elution, and then the neutral samples were directly injected to HPLC for analysis. Nickel-aluminum layered double hydroxides (NiAl-LDHs) were synthesized by co-precipitation method and packed into a micro pipette tip for the extraction of three non-steroidal anti-inflammatory drugs (NSAIDs) including ketoprofen, naproxen and flurbiprofen from aqueous samples. After optimization of the experimental parameters such as the concentration of the NaOH, sample pH, sampling rate and sample volume, excellent extraction efficiency towards three NSAIDs was obtained with high enrichment factors of 28–32. A NiAl-LDHs based SPE-HPLC method was developed for quantitative analysis of NSAIDs, and the method showed low limits of detection (0.002–0.1 ng/mL), good linearity (R 2 ≥ 0.9995) and good reproducibility (intraday RSD ≤ 4.37%). The developed method was also applied to the analysis of three NSAIDs in spiked human plasma and rat plasma after oral administration, which demonstrated the practicality of the proposed method. [ABSTRACT FROM AUTHOR]

The majority of studies based on phenolic compounds from plants are focused on the extractable fraction derived from an aqueous or aqueous-organic extraction. However, an important fraction of polyphenols is ignored due to the fact that they remain retained in the residue of extraction. They are the so-called non-extractable polyphenols (NEPs) which are high molecular weight polymeric polyphenols or individual low molecular weight phenolics associated to macromolecules. The scarce information available about NEPs shows that these compounds possess interesting biological activities. That is why the interest about the study of these compounds has been increasing in the last years. Furthermore, the extraction and characterization of NEPs are considered a challenge because the developed analytical methodologies present some limitations. Thus, the present literature review summarizes current knowledge of NEPs and the different methodologies for the extraction of these compounds, with a particular focus on hydrolysis treatments. Besides, this review provides information on the most recent developments in the purification, separation, identification and quantification of NEPs from plants. [ABSTRACT FROM AUTHOR]

Cooling a 1:1 (v/v) solution of acetonitrile and water at −16° C is known to result in two clear phases. We will refer to this event as “cold-induced aqueous acetonitrile phase separation (CIPS)”. On a molar basis, acetonitrile is 71.7% and 13.6% in the upper and lower phases, respectively, in our study. The phase separation proceeds as a descending cloud of microdroplets. At the convenient temperature (typical freezer) employed here the lower phase is rather resistant to solidification, although it emerges from the freezer as a solid if various insoluble matter is present at the outset. In a preliminary way, we replaced the initial (salting-out) step of a representative QuEChERS procedure with CIPS, applying this modified procedure (“CIPS-QuEChERS”) to a homogenate of salmon (and partly to beef). Three phases resulted, where only the upper, acetonitrile-rich phase is a liquid (that is completely clear). The middle phase comprises ice and precipitated lipids, while the lower phase is the residual matrix of undissolved salmon or meat. Treating the upper phase from salmon, after isolation, with anhydrous MgSO 4 and C18-Si (typical QuEChERS dispersive solid phase extraction sorbents), and injecting into a GC–MS in a nontargeted mode, gives two-fold more preliminary hits for chemicals, and also number of spiked pesticides recovered, relative to that from a comparable QuEChERS method. In part, this is because of much higher background signals in the latter case. Further study of CIPS-QuEChERS is encouraged, including taking advantage of other QuERChERS conditions. [ABSTRACT FROM AUTHOR]

Madder ( Rubia tinctorum L.) has been widely used as a red dye throughout history. Acid-sensitive colorants present in madder, such as glycosides (lucidin primeveroside, ruberythric acid, galiosin) and sensitive aglycons (lucidin), are degraded in the textile back extraction process; in previous literature these sensitive molecules are either absent or present in only low concentrations due to the use of acid in typical textile back extraction processes. Anthraquinone aglycons alizarin and purpurin are usually identified in analysis following harsh back extraction methods, such those using solvent mixtures with concentrated hydrochloric acid at high temperatures. Use of softer extraction techniques potentially allows for dye components present in madder to be extracted without degradation, which can potentially provide more information about the original dye profile, which varies significantly between madder varieties, species and dyeing technique. Herein, a softer extraction method involving aqueous glucose solution was developed and compared to other back extraction techniques on wool dyed with root extract from different varieties of Rubia tinctorum . Efficiencies of the extraction methods were analysed by HPLC coupled with diode array detection. Acidic literature methods were evaluated and they generally caused hydrolysis and degradation of the dye components, with alizarin, lucidin, and purpurin being the main compounds extracted. In contrast, extraction in aqueous glucose solution provides a highly effective method for extraction of madder dyed wool and is shown to efficiently extract lucidin primeveroside and ruberythric acid without causing hydrolysis and also extract aglycons that are present due to hydrolysis during processing of the plant material. Glucose solution is a favourable extraction medium due to its ability to form extensive hydrogen bonding with glycosides present in madder, and displace them from the fibre. This new glucose method offers an efficient process that preserves these sensitive molecules and is a step-change in analysis of madder dyed textiles as it can provide further information about historical dye preparation and dyeing processes that current methods cannot. The method also efficiently extracts glycosides in artificially aged samples, making it applicable for museum textile artefacts. [ABSTRACT FROM AUTHOR]

A new rapid monitoring method by means of high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS) following the heat-assisted extraction was developed for measurement of total inorganic arsenic species in rice flour. As(III) and As(V) eluted at the same retention time and completely separated from organoarsenic species by an isocratic elution program on a reversed phase column. Therefore, neither ambiguous oxidation of arsenite to arsenate nor the integration of two peaks were necessary to determine directly the target analyte inorganic arsenic. Rapid injection allowed measuring 3 replicates within 6 min and this combined with a quantitative extraction of all arsenic species from rice flour by a 15 min HNO 3 -H 2 O 2 extraction makes this the fastest laboratory based method for inorganic arsenic in rice flour. [ABSTRACT FROM AUTHOR]

• Three-dimensional-printed devices fabricated from different materials are reviewed. • The applications of 3D printing in various extraction modes are discussed. • 3D printing challenges for analytical applications are presented and addressed. Sample pretreatment is an important and necessary process in chemical analysis. Traditional sample preparation methods normally consume moderate to large quantities of solvents and reagents, are time- and labor-intensive and can be prone to error (since they usually involve multiple steps). In the past quarter century or so, modern sample preparation techniques have evolved, from the advent of solid-phase microextraction and liquid-phase microextraction to the present day where they are now widely applied to extract analytes from simple as well as complex matrices leveraging on their extremely low solvent consumption, high extraction efficiency, generally straightforward and simple operation and integration of most, if not all, of the following aspects: Sampling, cleanup, extraction, preconcentration and ready-to-inject status of the final extract. One of the most interesting features of the progress of microextraction techniques over the years lies in the development of devices, apparatus and tools to facilitate and improve their operations. This review explores the application of a recent material fabrication technology that has been receiving a lot of interest, that of three-dimensional (3D) printing, to the manipulation of microextraction. The review highlights the use of 3D-printed devices in the extraction of various analytes and in different methods to address, and improves upon some current extraction (and microextraction) problems, issues and concerns. [ABSTRACT FROM AUTHOR]

• Synthesis procedures of the nanofiber-based sorbents are studied. • Unique properties of nanofiber and nanofiber nanocomposites are discussed. • The application of nanofibers in extraction methods is reviewed. • The challenges and future development of nanofiber-based sorbents are discussed. Advanced sorbents gradually become a research hotspot on account of the increasing attention paid to environmental problems. Due to the prominent physicochemical features of nanofibers (NFs), such as high porosity, large surface area, favorable interconnectivity, high adsorption capacity, wettability, and the possibility of surface modification using functional groups, these nanostructures are regarded as excellent candidates for extraction applications. Therefore, the research in the field of NFs and their nanocomposites has been increasing in recent years. In the present review, we summarize the most recent studies on NFs-based sorbents focusing on strategies for preparation, characterization, and their unique capabilities as porous sorbents in various sorbent-based extraction methods. Moreover, we further described the performance and selectivity of sorbents to achieve improved extraction efficiency. Finally, some perspectives on the challenges and outlook are provided to aid future investigations related to this topic. [ABSTRACT FROM AUTHOR]

An aqueous two-phase system composed of Triton X-100 − (NH 4 ) 2 SO 4 − H 2 O was proposed for extraction and separation of tungsten(VI) from aqueous solution without using any extractant. The effects of aqueous pH, concentration of ammonium sulfate, Triton X-100 and tungsten, extracting temperature on the extraction of tungsten were investigated. The extraction of tungsten has remarkable relationship with aqueous pH and are to above 90% at pH = 1.0–3.0 under studied pH range (pH = 1.0–7.0) and increases gradually with increasing Triton X-100 concentration, but decreases slightly with increasing ammonium sulfate concentration. The extraction percentage of tungsten is hardly relevant to temperature but its distribution coefficient linearly increases with increasing temperature within 303.15–343.15 K. The distribution coefficient of tungsten increases with the increase of initial tungsten concentration (0.1–3%) and temperature (303.15 K-333.15 K). The solubilization capacity of tungsten in Triton X-100 micellar phase is independent of temperature. FT-IR analysis reveals that there is no evident interaction between polytungstate anion and ether oxygen unit in Triton X-100, and DLS analysis indicates that zeta potential of Triton X-100 micellar phase have a little change from positive to negative after extracting tungsten. Based on the above-mentioned results, it can be deduced that polytungstate anions are solubilized in hydrophilic outer shell of Triton X-100 micelles by electrostatic attraction depending on its relatively high hydrophobic nature. The stripping of tungsten is mainly influenced by temperature and can be easily achieved to 95% in single stage stripping. The tungsten (VI) is separated out from solution containing Fe(III), Co(II), Ni(II), Cu(II), Zn(II), Al(III), Cr(III) and Mn(II) under the suitable conditions. [ABSTRACT FROM AUTHOR]

This work presents a new method by electrical matrix solid phase dispersion for the extraction and clean-up of marbofloxacin, ofloxacin, norfloxacin, ciprofloxacin, enrofloxacin, difloxacin and sarafloxacin in bovine milk. Composition and pH of the eluent, applied electrical potential and polarity were optimized by experimental designs. The combination of the chromatographic and electrophoretic mechanisms allowed the extraction and clean-up in one step with low organic solvent consumption, high extraction throughput and elution automation. Linearity, precision, trueness and limit of quantification were evaluated and provided values in accordance with other methods recently developed for the analysis of fluoroquinolones in milk. This technique proved to be promising for the extraction and clean-up of ionizable analytes in different milk matrices. [ABSTRACT FROM AUTHOR]

The widespread use of organophosphate pesticides (OPPs) in agriculture leads to residue accumulation in the environment which is dangerous to human health and disrupts the ecological balance. In this work, one nanocomposite immobilized zirconium (Zr, IV) was prepared and used as the affinity probes to quickly and selectively extract organophosphorus pesticides (OPPs) from water samples. The Fe 3 O 4 -ethylenediamine tetraacetic acid (EDTA)@Zr(IV) nanocomposites (NPs) were prepared by simply mixing Zr(IV) ions with Fe 3 O 4 -EDTA NPs synthesized by one-pot chemical co-precipitation method. The immobilized Zr(IV) ions were further utilized to capture OPPs based on their high affinity for the phosphate moiety in OPPs. Coupled with GC–MS, four OPPs were used as models to demonstrate the feasibility of this approach. Under the optimum conditions, the limits of detection for target OPPs were in the range of 0.10–10.30 ng mL −1 with relative standard deviations (RSDs) of 0.61–4.40% (n = 3), respectively. The linear ranges were over three orders of magnitudes (correlation coefficients, R 2 > 0.9995). The Fe 3 O 4 -EDTA@Zr(IV) NPs were successfully applied to extract OPPs samples with recoveries of 86.95–112.60% and RSDs of 1.20–10.42% (n = 3) from two spiked real water. By the proposed method, the matrix interference could be effectively eliminated. We hope our finding can provide a promising alternative for the fast extraction of OPPs from complex real samples. [ABSTRACT FROM AUTHOR]

A fast environment-friendly extraction method, ball mill-assisted deep eutectic solvent-based extraction, was used for the extraction of natural products from plants. In this study, tanshinones were selected as target compounds to evaluate the efficiency of the developed extraction method. Under the optimized experimental conditions, cryptotanshinone (0.176 mg/g), tanshinone I (0.181 mg/g), and tanshinone II A (0.421 mg/g) were extracted from Salvia miltiorrhiza Bunge, and the developed method was found to be greener, more efficient, and faster than conventional, environmentally harmful extraction methods such as methanol-based ultrasound-assisted extraction and heat reflux extraction. The analytical performances including recovery, reproducibility (RSD, n = 5), correlation of determination ( r 2 ), and the limit of detection, with the ranges of 96.1–103.9%, 1.6–1.9%, 0.9973–0.9984, and 5–8 ng/mL, were respectively obtained. Application of ball mill-assisted deep eutectic solvent-based extraction may fundamentally shape the future development of extraction methods. [ABSTRACT FROM AUTHOR]

A disposable integrated microfluidic device was developed for rapid sample stacking, separation and extraction of multiple DNA fragments from a relatively large amount of sample. Isotachophoresis hyphenated gel electrophoresis (ITP-GE) was used to pre-concentrate and separate DNA fragments, followed by extraction of pure DNA fragments with electroelution on-chip. DNA fragments of 200 bp, 500 bp and 1 kbp were successfully separated and collected in the extraction chamber within 25 min. The extraction efficiency obtained from the chip was 49.9%, 52.1% and 53.7% for 200 bp, 500 bp and 1 kbp DNA fragments, respectively. The extracted DNA fragments exhibited compatibility with downstream enzymatic reactions, for example PCR. The chip was also used to extract DNA fragments with specific size range from sheared genomic DNA and demonstrated similar performance to that using traditional gel cutting method. The whole assay can finish in 32 min, 6 times faster than traditional method. [ABSTRACT FROM AUTHOR]

In this study, a reliable and fast method using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction procedure without any clean-up step was developed for simultaneous extraction of 15 mycotoxins, i.e., aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, aflatoxin M1, aflatoxin M2, deoxynivalenol, 3-acetyldeoxynivalenol, 15-acetyldeoxynivalenol, de-epoxy-DON, zearalenone, α-zearalenol, β-zearalenol, α-zearalanol, and β-zearalanol, from eggs. High-performance liquid chromatography tandem mass spectrometry was used to separate and detect all of the analytes. Electrospray ionization at both negative and positive modes and multiple reaction-monitoring mode were applied to detect these analytes. The main factors, such as extraction time, extraction solvent, evaporation temperature, and pH of the solvent, were carefully optimized to improve the extraction efficiency. The coefficients of determination of the calibration curves ranged from 0.9884 to 0.9998. The recoveries of most of the analytes were between 71.3% and 105.4% at three concentration levels, except for AFB1 that showed recovery rates of not more than 67.5% in all concentrations. The repeatability and intra-lab reproducibility of this method were both lower than 15% and 25%, respectively. The limit of quantification ranged from 0.2 μg/kg to 5 μg/kg. The matrix effect was evaluated and reduced by the use of matrix-matched calibration curves. The validated method was applied in a pilot study to analyze mycotoxin contamination in 12 eggs, and trace amounts of deoxynivalenol, 15-acetyldeoxynivalenol, aflatoxin B1, aflatoxin G2, zearalenone and β-zearalenol were detected in these samples. [ABSTRACT FROM AUTHOR]

Size exclusion chromatography is extensively used to separate proteins and to determine their apparent molecular weights. It separates proteins based on hydrodynamic volume, but interactions between the chromatography resin and proteins lead to non-size effects. This report discusses the impact of co-solvents [salt, urea, sodium dodecyl sulfate (SDS), dithiothreitol] in extraction media when separating wheat gluten proteins, soy glycinin, bovine serum albumin and ovalbumin on a Biosep-SEC-S4000 column. With acetonitrile/water (1:1, v/v) containing 0.05% (v/v) trifluoroacetic acid as eluent, salts and SDS in the extraction media increase while urea decreases non-size effects. Most gluten and globular proteins are extractable in sodium phosphate buffer (0.050 M; pH 6.8) containing 2.0% (w/v) SDS. This chromatographic medium allows analyzing mixtures of various proteins without any non-size effects. [ABSTRACT FROM AUTHOR]

A new method based on the use of porous organogel materials in combination with liquid chromatography–tandem mass spectrometry (LC–MS–MS) was assessed for the quantification of trace contaminants in complex matrices. As a demonstration of the use of these new materials, the contaminant chosen as a model was bisphenol A (BPA) and its extraction was investigated in urine. Organogel materials consist of an organic solvent immobilized by an organogelator. The composition of the organogel materials was optimized in terms of extraction efficiency and compatibility with LC–MS–MS. Porosity was introduced into the organogel by means of the particulate leaching method using sugar crystals. This new absorbing material is simple to use; the extraction method is reduced to a few steps. The originality of the method lies in the complete dissolution of the material for analysis by LC–MS–MS. The matrix effect of the organogel components was studied and was found to be minimal in atmospheric-pressure chemical ionization (APCI) compared to electrospray ionization (ESI) in negative mode. The influence of matrix components on the extraction was investigated by working with different media (acidified water, synthetic urine, horse urine and human urine). The partition coefficient was not affected within the margin of error (±0.1). After optimization, bisphenol A recoveries from urine samples reached 80%. The actual concentration factor was 10. The relative standard deviation (RSD, n = 6) for the extraction and determination of BPA in horse urine spiked at 10 ng mL −1 was 9%. Tests with spiked human urine showed that the extraction performances were the same as with the solutions tested previously. The use of porous organogel allowed a fast, simple, sensitive, robust, green method to be developed for the determination of trace contaminants in complex matrices. [ABSTRACT FROM AUTHOR]

The present study is focused on the development of a pre-analytical strategy for the quantification of intracellular nucleotides from cultured cell lines. Different protocols, including cell recovery, nucleotide extraction and purification, were compared on a panel of nucleoside mono-, di- and triphosphates from four cell lines (adherent and suspension cells). The quantification of nucleotides was performed using a validated technique with on-line solid-phase extraction coupled with liquid chromatography–triple quadrupole tandem mass spectrometry (LC–MS/MS). Designed experiments were implemented to investigate, in a rigorous and limited-testing experimental approach, the influence of several operating parameters. Results showed that the technique used to harvest adherent cells drastically affected the amounts of intracellular nucleotides. Scraping cells was deleterious because of a major leakage (more than 70%) of intracellular nucleotides during scraping. Moreover, some other tested conditions should be avoided, such as using pure methanol as extraction solvent (decrease over 50% of intracellular nucleotides extracted from NCI-H292 cells) or adding a purification step with chloroform. Designed experiments allowed identifying an interaction between the percentage of methanol and the presence of chloroform. The mixture methanol/water (70/30, v/v) was considered as the best compromise according to the nucleoside mono-, di-, or triphosphates and the four cell lines studied. This work highlights the importance of pre-analytical step combined with the cell lines studied associated to sensitive and validated assay for the quantification of nucleotides in biological matrices. [ABSTRACT FROM AUTHOR]

A novel sample preparation method based on the complete dissolution of marine biological samples in choline chloride-oxalic acid (ChCl-Ox) deep eutectic solvent was developed for fast and efficient extraction of eight polycyclic aromatic hydrocarbons (PAHs) using minimum volumes of cyclohexane. The extracted PAHs were purified and then measured by high-performance liquid chromatography-fluorescence detection (HPLC-FL). The effect of key parameters on extraction recoveries and precision was investigated. At optimized conditions, the studied samples were dissolved under atmospheric pressure in ChCl-Ox (1:2) at 55 °C for 30 min, which is considerably lower than the temperature used in the classical and current methods. After dissolution, it took approximately 20 min to quantitatively extract the PAHs from ChCl-Ox using 5 mL cyclohexane. Depending on the analyte, the developed method was linear over the calibration range 1.0–250, 2.0–250, and 5.0–250 ng g −1 , with r 2 > 0.996. The detection limits of the method were between 0.50 and 3.08 ng g −1 . The intra-day and inter-day precisions (based on the relative standard deviation, n = 5) of the spiked PAHs at a concentration level of 50 ng g −1 were better than 12.6% and 13.3%, respectively. Individual PAH recoveries from spiked marine fish and macroalgae samples were in the range of 71.6% to 109.6%. For comparison, the spiked samples were also subjected to the Soxhlet extraction method. The simplicity of the procedure, high extraction efficiency, short analysis time, and use of safe and inexpensive components suggest the proposed method has a high potential for utilization in routine trace PAH analysis in biological samples. [ABSTRACT FROM AUTHOR]

The control of pesticide residues on raw coffee is a task of great importance due to high consumption of this beverage in Italy and in many other countries. High caffeine content can hamper extraction and measurement of any pesticide residue. A tandem extraction protocol has been devised by exploiting the quick easy cheap effective rugged and safe (QuEChERS) scheme for extraction, coupled to a dispersive liquid–liquid micro-extraction (DLLME) in order to drastically reduce caffeine content in the final extract. Gas chromatography–mass spectrometry (GC–MS) has been used for quantification of organo-chlorine pesticides in single ion monitoring (SIM) mode. Method has been validated and performances meet the criteria prescribed by European Union regulations. [ABSTRACT FROM AUTHOR]

In this study, deep eutectic solvent (DES) based systems were evaluated for selective extraction and optimized for increased recovery of chlorogenic acid derivatives, flavone glycosides and iridoid glycosides from Dipsacus fullonum L. leaves. Bioactives from Dipsacus plants has shown great antioxidant and antimicrobial activities as well as effectiveness against several cancer strains and a source for anti- Borrelia compounds. Twelve different hydrophilic and hydrophobic DESs were tested to find the best solvent composition. Choline chloride and betaine were used as hydrogen bond acceptors (HBA) for the preparation of hydrophilic DESs and menthol for hydrophobic DESs. The tested hydrogen bond donors (HBD) were various organic acids and glycerol. The composition of most effective DES was optimized using the Box-Behnken design for each of the three main group of analytes from D. fullonum L. to evaluate possible selectivity and highest recovery. HPLC-DAD-MS was used to identify and quantify the main bioactive compounds extracted from plant material. The optimal extraction for highest overall recovery was achieved using a molar ratio of choline chloride and lactic acid of 1:2.4 with 35% water and 27 mL of the solvent per one gram of dry material. The optimized DES extract gave concentrations 1.8 to 2.2 times higher than traditional organic solvent extracts depending on the group of analytes. [ABSTRACT FROM AUTHOR]

• A new online μ-MCE method with soil-packed cartridge was developed for fipronil extraction in soil. • Online μ-MCE exhibited ultrahigh desorption efficiency compared with traditional extraction methods. • Its universality was validated in different interactions, compounds and soils. • The method is mild, fast, efficient, cost-effective, and automatic. Nowadays, environment fate and behavior of pesticides in soil is still not fully understood due to the lack of standardized soil extraction method. In this work, a soil-filled micro-matrix cartridge was online combined with high performance liquid chromatography-mass spectrometry (HPLC-MS) through a six-way valve for the simultaneous extraction and determination of residual fipronil in soil. Compared with conventional extraction methods, such as hydroxypropyl-β-cyclodextrin (HPCD) extraction, shaking extraction, ultrasonic-assisted extraction (UAE), three-step extraction and matrix solid phase dispersion (MSPD), the novel, miniaturized, and integrated online micro-matrix cartridge extraction (online μ-MCE) method exhibited better performance in terms of desorption efficiency (99.4%), analysis time, solvent consumption, sensitivity, and automation. In sequential extraction, online μ-MCE could further desorb fipronil from the extracted soil with the percentage of 1.05%-58.55%. High recovery of 92.69% obtained for the ISO certificated test- soil verified the satisfactory accuracy of the method. Besides, its wide universality was also validated in three variables: 1) various pesticides-soil interactions, 2) four types of compounds (aromatic hydrocarbons, carboxylic acids, alcohols and aldehydes), and 3) three types of soils (sandy soil, silty loam and silty clay). The superior desorption capacity might be attributed to the instantaneously increased high-pressure, continuous flow dynamic desorption and short residence time. The present encouraging findings might shed light on new ways to develop a mild, highly efficient, reliable and one-fit-all extraction method toward pesticide contaminated soil. [ABSTRACT FROM AUTHOR]

• Multi-residue analysis for 151 chemicals in fish was developed and validated. • Captiva EMR-Lipid cartridge showed better protein removal efficiency than QuEChERS. • LC-QTOF-MS/MS combined with Captiva EMR-Lipid cartridge showed good performance. • 867 chemicals were tentatively identified in cultured fish by nontarget screening. An effective analytical method for target and non-target screening of multi-class emerging organic chemicals in aquaculture fish muscle samples using liquid chromatography coupled with high resolution time-of-flight mass spectrometry (LC-QTOF-MS/MS) was reported. Two sample pretreatment methods (QuEChERS and Captiva EMR-Lipid cartridge) were compared and assessed for 151 organic compounds covering a wide range of log Kow (-1.37—11.51) in freeze-dried fish samples. Captiva EMR-Lipid cartridge outperformed QuEChERS by high detection frequency (> 87.5%) and effective matrix removal with satisfactory standard deviation of the compounds (< 20%), and meanwhile provided acceptable recoveries for most organic chemicals at three spiking concentration levels (10, 50, and 100 ng g−1). Spiking experiments suggested that the developed non-target screening workflow showed further convincible identification results with over 83.3% of the chemicals confirmed at even low spiking levels. A list of 867 organic chemicals were tentatively identified in fish samples collected from fish ponds with 21 of them classified as high confidence levels (L1 and L2). The results showed that the simplified analytical strategy can be applied for the quantification and screening analysis of a broad range of emerging organic chemicals in fish samples. [ABSTRACT FROM AUTHOR]

Highlights: [•] Functionalization of cotton fibers with graphene-aminosilica nanoparticles. [•] Extraction of PAHs, phthalates, musks, phenolics, haloacetic acids from environmental waters. [•] Hydrophobic, π–π stacking, hydrophilic (hydrogen bonding) and ionic interactions are responsible for the extraction performance. [ABSTRACT FROM AUTHOR]

• Implementation of electropermeabilization-assisted into liquid biphasic flotation. • Greener and non-thermal technique for the permeabilization of cell membrane. • Optimized conditions achieved yield extracted fucoxanthin of 16.09 ± 0.27 mg/g. • Extracted fucoxanthin exhibited satisfactory antioxidant activities based on TEAC and TPC. Electropermeabilization-assisted liquid biphasic flotation (LBF) system is an emerging extraction system facilitated by the adsorptive bubble separation and the electroporation in an aqueous two-phase medium. This integrative extraction system is well suited for the direct recovery of intracellular biocompounds from cells without the needs of discrete steps of mid- or down-stream bioprocessing. The potential of electropermeabilization-assisted LBF system in bioseparation was demonstrated in this study by using the diatom Chaetoceros calcitrans (C. calcitrans) as the source of fucoxanthin, which is a promising antioxidant highly demanded by food and pharmaceutical industries. The extraction performances of LBF and electropermeabilization-assisted LBF system were comprehensively evaluated under the optimal operating conditions. Comparatively, the optimized LBF and electropermeabilization-assisted LBF systems achieved the satisfactory yields of fucoxanthin, i.e., 14.78 mg/g and 16.09 mg/g, respectively. The good recovery of fucoxanthin using electropermeabilization-assisted LBF system could be attributed to the higher release of fucoxanthin from the electrotreated C. calcitrans , allowing a higher partition of fucoxanthin to the top phase of LBF system (236.72 as compared to 152.15 from LBF system). In addition, the fucoxanthin extracted suing both methods exhibit satisfactory antioxidant activities. The application of electropermeabilization-assisted LBF system in the extraction of fucoxanthin is a greener and highly efficient bioprocessing route which can be prospectively extended to other biocompound extraction from microalgal sources. [ABSTRACT FROM AUTHOR]

Highlights: [•] Development of a new portable instrumentation for the extraction of essential oils. [•] Extraction of essential oil from rosemary directly in a crop. [•] Procedure appropriate for teaching laboratory. [Copyright &y& Elsevier]

Highlights: [•] Fe3O4@polypyrole (PPy) NPs were synthesized via oxidative polymerization of pyrrole. [•] The size, morphology and surface coating of synthesized NPs were characterized. [•] The Fe3O4@ PPy NPs were used as the magnetic adsorbent for extraction nitrophenols. [•] Anionic forms of nitrophenols were extracted with an anion exchange process. [•] The developed method was applied for determination of nitrophenols in water samples. [ABSTRACT FROM AUTHOR]

Highlights: [•] Four extraction methods of tetracyclinic antibiotics from fish filet were compared. [•] HPLC with fluorescence detection was used to evaluate the methods. [•] Method validation was performed with the phenyl cartridge SPE method. [•] Good recovery and low cost for the analyses of TCs residues were achieved. [ABSTRACT FROM AUTHOR]

Highlights: [•] We have developed a new water-based gas purge microsyringe extraction. [•] Organic-free sample pretreatment technique does not need drying process. [•] The extracts are directly submitted into the LC analysis. [•] Sample treatment is completed within 5min with high recovery and precision. [•] This technique is suitable for ionizable volatile and semivolatile compounds. [ABSTRACT FROM AUTHOR]

Highlights: [•] A sample preparation method was proposed for anionic surfactants determination. [•] CTAB-coated nanomagnets allowed quantitative extraction of C10–C13 LAS homologues. [•] Excellent extractability was achieved with reduced amounts of CTAB and nanoparticles. [•] The proposed method was applicable to the analysis of natural aqueous matrices. [Copyright &y& Elsevier]

Highlights: [•] Simultaneous determination of 29 typical substituted and parent PAHs. [•] The method was optimized for analyzing water, particulate and sediment samples. [•] The LOQ below 20.25ng/L, 131.66 and 28.04ng/g in water, particulate and sediment. [•] Transformation from 7-NBA to BA-7,12-D occurred during pretreatment procedure. [•] Certain SPAHs and PAHs were detected in water, particulate and sediment samples. [Copyright &y& Elsevier]

Abstract: Deep eutectic solvents (DESs) are emerging rapidly as a new type of green solvent instead of an ionic liquid (IL), and are typically formed by mixing choline chloride with hydrogen bond donors. Few studies have applied DESs to the extraction and determination of bioactive compounds. Therefore, in the present study, DESs were used to extract flavonoids (myricetin and amentoflavone), which are well known and widely used antioxidants, to extend their applications. A range of alcohol-based DESs with different alcohols to choline chloride (ChCl) mixing ratios were used for extraction using several extraction methods. Other factors, such as temperature, time, water addition and solid/liquid ratio, were examined systematically using a response surface methodology (RSM). A total of 0.031 and 0.518mgg−1 of myricetin and amentoflavone were extracted under the optimized conditions: 35vol% of water in ChCl/1,4-butanediol (1/5) at 70.0°C for 40.0min and a solid/liquid ratio of 1/1 (g10mL−1). Good linearity was obtained from 0.1×10−3 to 0.1mgmL−1 (r 2 >0.999). The excellent properties of DESs highlight their potential as promising green solvents for the extraction and determination of a range of bioactive compounds or drugs. [Copyright &y& Elsevier]