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Effective recycling of organic residues contributes to solving energy crisis and resource recycling. In Egypt, sugarcane is considered one of the most produced agricultural product, which in terms leads to the production of a vast amount of its by-products. In this work, for the first time, untreated sugarcane bagasse (SCB) was utilised as a sorbent in the solid-phase extraction (SPE) of selected pesticides including chlorfenvinphos, chlorpyrifos, diazinon, ethion, profenofos (organophosphorus compounds) and cyprodinil (anilinopyrimidine) from water. Optimal parameters influencing the recovery of the studied pesticides including eluting solvent (type, volume and pH), amount of sorbent and water pH were adjusted. Method performance criteria using SCB cartridges were compared with that of commercial SPE cartridges, indicating SCB as an effective and green chemistry alternative. The final SPE procedure can be briefly described as follows: the SCB (500 mg) SPE cartridge was conditioned with 5 mL methanol followed by 5 mL distilled water. Then, 500 mL water sample (DIW) was loaded on the SCB SPE cartridge. Afterwards, the cartridge was dried using nitrogen for 15 min. Then, 4 mL acetonitrile containing 5% formic acid was used as the eluting solvent to be analysed using LC-MS/MS. The method was validated in accordance with (SANTE/2020/12830 and Eurachem Second Edition 2014). Rapid adsorption and desorption performance for SCB was confirmed by using adsorption kinetic and isotherm studies. Finally, five environmental water samples were analysed using the developed method, only one sample had positive result (profenofos 0.01 µg/L), which is below the accepted limits. [ABSTRACT FROM AUTHOR]

An applicable liquid chromatography-tandem mass spectrometry (LC-MS/MS) method is developed to enable the efficient residue detection of fifteen acidic pesticides in water (drinking, ground, irrigating, and agricultural drainage water). The extraction and sample concentration were accomplished using the solid-phase extraction (SPE) technique. The developed method was fully validated according to the EU validation guidelines. The accuracy and precision calculations were evaluated by sample fortifications at concentrations of 0.1–1.0 µg/L. Acceptable recoveries and precisions were obtained of 70–120% and below 20%, respectively. The method showed good linearity ≥0.995. The developed method's quantitation limit was 0.1 µg/L for most studied pesticides. The uncertainty measurement, expressed as expanded uncertainty, in terms of relative standard deviation (at 95% confidence level) is within the range of ±44%. A survey study was successfully conducted by collecting 108 water samples from different water sources in Egypt during the period between June 2020 and May 2021. The obtained results showed the absence of residue for most of the acidic pesticides in the collected samples, except for bentazone which was present in 33% of the collected samples with a concentration range of 0.1 to 0.29 µg/L. [ABSTRACT FROM AUTHOR]

An analytical method for the determination of imatinib (IMA, the primary treatment for chronic myeloid leukemia), based on the fluorescence properties of graphene quantum dots (GQDs), is reported in this work. The method is addressed to the analytical control of IMA in biological and pharmaceutical samples, due to the present interest in the control of the doses of this anticancer drug, as well as the therapeutic monitoring. The whole method involves the use of a solid-phase extraction (SPE) procedure, followed by an evaporation step, for the treatment of biological samples. For that, tC18 sorbent cartridges were used. After the sample treatment, the solution containing the analyte was mixed with an aqueous solution of GQDs at pH 7.2, and the fluorescent quenching of GQDs was measured. IMA was determined in the 10–250 µg L−1 range, with a limit of detection of 21 µg L−1 and a precision of 1.5% as relative standard deviation, measured in terms of reproducibility. The recovery for biological samples was in the 84–113% range. [ABSTRACT FROM AUTHOR]

Cr (III) is an essential element for maintaining glucose, lipid, and protein metabolism in mammals. Removal/recovery of such heavy metals is crucial. For this purpose, dendrimer-based novel magnetic nanoparticles to enrich Cr (III) were synthesized and characterized by spectroscopic methods such as SEM-EDX, TEM, FT-IR, XRD, and VSM. The optimum parameters such as pH, eluent type-concentration, adsorbent amount, and time, which are important in the recovery of Cr (III) with solid magnetic-based nanoparticles (MNPs), were determined by flame atomic absorption spectroscopy. After the enrichment of Cr (III) with MNPs, the device's detection power enhancements were increased by 8653 ± 145 times. The optimum conditions obtained for Cr (III) ions with MNPs were successfully applied to water, honey, and hardaliye samples. Furthermore, the reusability results of the MNPs were determined to be approximately 99% for Cr (III) up to the 10th use. [ABSTRACT FROM AUTHOR]

Restricted Access Media-Methacrylic Resin with the ability of protein exclusion was prepared by the free radical polymerization using methacrylic acid, ethylene glycol dimethacrylate and glycidyl methacrylate as monomer, cross-linker and comonomer, respectively. Protein exclusion ability of this material was studied. The results showed that the material was able to eliminate 93.6% of protein after bovine serum albumin solution was added and shaken for 220 min. Adsorption kinetics and adsorption isotherms of Lamotrigine on this material were investigated. The experimental data were the most suitable for the pseudo-second-order kinetics model and Freundlich isotherm model. Restricted Access Media-Methacrylic Resin was used as sorbent for Solid-Phase Extraction to extract Lamotrigine from Human Plasma. The method for the determination of Lamotrigine in human plasma by SPE followed by the HPLC–UV presented linear range from 1.0 to 66.6 µg/mL with correlation coefficient 0.9930 for Lamotrigine, assay precision with relative standard deviation value 6.24%, and assay accuracy 94.7–104.7% with relative standard deviation values 4.33–5.81%. SPEs filled with this material were used at least 7 times without any significant changes in their performance. Analytical validation parameters demonstrated that the method could be applied to the determination of Lamotrigine at the therapeutic plasma levels without other treatments. [ABSTRACT FROM AUTHOR]

Preservatives can be used in natural and organic cosmetics to prevent quality deterioration during distribution and use, but the ingredients permitted are limited in the Republic of Korea. A method of simultaneous analysis was developed to monitor natural and organic cosmetics distributed online for the presence of 15 illegally used preservatives. Considering the complexities of the cosmetic matrices, an optimized sample preparation method is essential. Therefore, we developed the optimal purification method by comparing three preparation methods: QuEChERS, high-speed centrifugation, and solid-phase extraction (SPE). The SPE method, which exhibited the most favorable results in matrix reduction, was employed. To establish the SPE-ultra-high-performance liquid chromatography-diode array detection method, factors such as the mobile phase and column were optimized. The optimal separation of the 15 preservatives was observed under the following conditions: mobile phase A comprising 0.1% phosphoric acid in water with 0.5 mM sodium hexanesulfonate and a C8 column (1.7 μm, 2.1 × 150 mm) as the stationary phase. The linear correlation coefficients were > 0.9998, and the limits of detection and quantitation ranged from 0.05 to 0.67 and 0.15 to 2.02 μg mL−1, respectively. Using the established analytical method, illegally used preservatives were detected in products claimed to be natural and organic cosmetics sold on the market, and these findings were subsequently verified using liquid chromatography-tandem mass spectrometry. Six out of 47 samples contained phenoxyethanol and parabens. Therefore, this method will help manage the addition of illegal preservatives to natural and organic cosmetics. [ABSTRACT FROM AUTHOR]

Lipophilic marine toxins (LPMTs) are toxic secondary metabolites produced by microalgae. With rising sea surface temperatures driven by climate change, the spread of harmful microalgae is increasing. This study established and validated a simultaneous analysis method for 16 LPMTs, including compounds from the okadaic acid (OA), yessotoxin (YTX), azaspiracid (AZA), pectenotoxin (PTX), and cyclic imine (CI) groups. The method was validated in mussel, clam, and flatfish matrices and applied to seafood collected from three coastal areas in Korea (the East, West, and South Seas), to assess LPMT contamination. The limit of detection for the method was calculated to be 0.01–3.54 μg kg−1 for all 16 toxins. Accuracy and precision were confirmed through repeated intraday and interday analyses, with all results satisfying CODEX guidelines (accuracy: 60–115%, precision: ≤ 22%), indicating that the method can be successfully applied to fish and shellfish matrices. From the 25 collected samples, compounds from the OA group were found in seven (28%) at a positive mean of 82.0 μg OA eq. kg−1, YTX-group compounds were found in two (8%) at a positive mean of 224.4 μg YTX eq. kg−1, and CI-group compounds were found in two (8%) at a positive mean of 14.3 μg kg−1. No PTX- or AZA-group toxins were detected in any samples. LPMTs were detected in all three sea areas. The established method for the simultaneous analyses of 16 LPMTs in both bivalves and fish saves analytical time and allows proactive monitoring of regulated as well as unregulated LPMTs. [ABSTRACT FROM AUTHOR]

The measurement of selected norepinephrine metabolites, such as 3,4-dihydroxyphenylglycol (DHPG), 3-methoxy-4-hydroxyphenylethylenglycol (MHPG), and vanillylmandelic acid (VMA), in biological matrices—including urine—is of great clinical importance for the diagnosis and monitoring of diseases. This fact has forced researchers to evaluate new analytical methodologies for their isolation and preconcentration from biological samples. In this study, the three most popular extraction techniques—liquid-liquid extraction (LLE), solid-phase extraction (SPE), and a new 3D-printed system for dispersive solid-phase extraction (3D-DSPE)—were investigated. Micellar electrokinetic chromatography (MEKC) with a diode array detector (DAD) at 200 nm wavelength was applied to the separation of analytes, allowing for the assessment of the extraction efficiency (R) and enrichment factor (EF) for the tested extraction types. The separation buffer (BGE) consisted of 5 mM sodium tetraborate decahydrate, 50 mM SDS, 15% (v/v) MeOH, 150 mM boric acid, and 1 mM of 1-hexyl-3-methylimidazolium chloride (the apparent pH of the BGE equaled 7.3). The EF for each extraction procedure was calculated with respect to standard mixtures of the analytes at the same concentration levels. The 3D-DSPE procedure, using DVB sorbent and acetone as the desorption solvent, proved to be the most effective approach for the simultaneous extraction and determination of the chosen compounds, achieving over 3-fold signal amplification for DHPG and MHPG and over 2-fold for VMA. Moreover, all extraction protocols used for the selected norepinephrine metabolites were estimated and discussed. It was also confirmed that the 3D-DSPE-MEKC approach could be considered an effective tool for sample pretreatment and separation of chosen endogenous analytes in urine samples. [ABSTRACT FROM AUTHOR]

Over recent decades, the global occurrence of pesticide residues in aquatic environments has been a pivotal issue; however, their trace-level concentrations necessitate the establishment of ultra-sensitive and reliable analytical approaches. To this end, the present study describes the optimization and validation of an LC-HRMS-based method for the accurate determination of 18 pesticides in river and sea water, accompanied by a measurement uncertainty estimation. This method was applied to analyze 17 real samples from agriculture and aquaculture-impacted areas in Greece and Albania. Different solid-phase extraction (SPE) protocols were tested. For the analysis, cutting-edge Orbitrap MS technology and MS/MS fragmentation, along with the use of matrix-matched calibration curves, provided unprecedented accuracy (<5 ppm) and sensitivity for the confirmation of positive detections. Regarding method performance, exceptional linearity was obtained; the limits of quantification ranged from 1.7 ng L−1 to 90 ng L−1, recoveries varied from 61% to 96% in river water, while slightly higher recoveries (60–111%) were observed in seawater. In all cases, repeatability and intra-laboratory reproducibility were below 15%. The measurement expanded uncertainty (U′, k = 2) was estimated considering precision and bias. MU% values were lower than 50% in all cases, as recommended in SANTE guidelines and applied to the quantified results. The matrix effect study exhibited negative values (<20%) for all compounds. Application to real samples showed a low pesticide contamination load that should not be underestimated. [ABSTRACT FROM AUTHOR]

This study focuses on the development of eco-friendly biobased adsorbents through a sustainable hydrothermal and freeze-drying synthesis process, utilizing cost-effective bio-sourced materials to minimize energy consumption and waste. The biobased adsorbents were elaborated using hydroxyethyl cellulose-ionic liquids and bentonite clay. The elaborated biocomposites were characterized using X-ray diffraction (XRD), Fourier-transform infrared spectroscopy/attenuated total reflection (FTIR/ATR), thermogravimetric analysis (TGA), and electron microscopy-energy dispersive X-ray (SEM–EDX), Brunauer–Emmett–Teller (BET) and zeta potential (ZP). Structural analysis confirms the intercalation and incorporation of HEC-ILs polymeric chains into Be-Na matrix and the formation of biocomposites. The [HEC-ILs/Be-Na] composite was subsequently employed for solid-phase extraction of Co(II) by investigating the effect of pH, initial Co(II) concentrations, time, temperature, and the presence of co-existing ions (Na(I), Li(I), Mn(II), Ni(II), and Al(III)). The adsorption kinetics of Co(II) metal ions were suitably characterized using the pseudo-second-order model (with R2 > 0.99). Furthermore, the adsorption isotherms conformed to the Langmuir model (with R2 > 0.97), suggesting a chemisorption process with an adsorption capacity of 69.8 mg/g. The thermodynamic study reveals that the adsorption process exhibits characteristics of spontaneity and endothermicity (ΔH° = 74.197 kJ mol−1, ΔG° < 0 kJ mol−1). The proposed mechanism for Co(II) adsorption on the developed biocomposite involves electrostatic interactions, ion exchange, and anion-π interactions. The biobased composite exhibited remarkable selectivity for Co(II) and demonstrated great potential as an adsorbent for industrial applications. [ABSTRACT FROM AUTHOR]

Due to the increase in the global population, industrialization, and the transition to climate neutrality through low‐emission technologies, the pressure on critical materials (CMs) continues to grow. CMs are defined as materials with a significant risk of supply chain disruption and limited substitutability. In this context, rare‐earth elements, platinum group metals, lithium, and cobalt are particularly crucial for the shift to carbon‐free economy and sustainability. One of the important strategies to endorse the goal of carbon reduction is to promote the recycling of resources. As a solution, effective recovery strategies have been developed, such as solid‐phase separation technologies based on advanced functional sorbents. This perspective article aims to provide a general assessment of the role of porous materials in closing the loop of critical materials recycling. Here, comprehensive insights are provided into recent development, design, and application of porous adsorbents commonly applied in solid‐phase extraction systems. Their current research status and problems related to their future application are also highlighted. This review covers recent advances in porous and hierarchical silica‐based materials, aerogels, covalent organic frameworks, metal–organic frameworks, and carbon‐based adsorbents. [ABSTRACT FROM AUTHOR]

Solid‐phase extraction (SPE) using a polyaniline molecularly imprinted polymer (PANI@MIP) is optimized for the extraction of benzophenone‐4 (BP4) from aqueous matrices. First, the three main variables influencing the washing step of the SPE method—type, composition, volume, and percolation flow rate of the washing solvent—were investigated. The optimal conditions for the washing step using the new PANI@MIP‐SPE for maximum retention of BP4 and elimination of interfering molecules (benzophenone‐3 [BP3] and benzophenone [BP]) were determined as follows: 1.25 mL acetonitrile/acetic acid/hexane (45/05/50 v/v/v) as wash solvent at a flow rate of 1 mL min−1. A multiple linear regression model was validated using Student's t‐test to identify the most significant variables affecting this step, including the type and volume of each eluent solvent and the volume of the ternary mixture solvents. The reliability of the model was further confirmed by analysis of variance (ANOVA) and Fisher's F‐test at α = 0.05. The extraction recoveries of the target analyte exceeded 92% over the range of concentrations (from 0.1 to 120 mg L−1), and the maximum retention capacity of PANI@MIP‐SPE was 600 µg g−1, in contrast to 50 µg g−1 for PANI@NIP‐SPE. [ABSTRACT FROM AUTHOR]

New psychoactive substances are produced and marketed to mimic the effects of their illicit counterparts and to attempt to evade drug tests and prosecution. Here, we present the optimisation, validation and application of an analytical method using liquid chromatography–time‐of‐flight mass spectrometry to detect and quantify 37 new psychoactive substances and illicit substances in wastewater from South Wales, UK, using a targeted analysis method. Sample preparation was performed using solid‐phase extraction with Oasis HLB cartridges. The LC separation was performed using a YMC‐Triart Phenyl 450 bar column (12 nm, 5 μm, 100 × 3 mm) which provided good separation and resolution for all targeted analytes with a run time of 9 min. The method was validated using the following parameters: sensitivity, selectivity, linearity, accuracy, precision, recovery and matrix effects. The method was then applied to influent wastewater samples collected from two wastewater treatment plants in Wales, UK. [ABSTRACT FROM AUTHOR]

Nucleic acid (NA) testing at the point‐of‐care requires efficient NA extraction followed by post‐NA amplification to achieve necessary detection sensitivity. Nanofibers (NFs) are demonstrated to be an ideal solid surface in an NA extraction process but necessitate harsh conditions that interfere with the subsequent NA amplification process. It is demonstrated that novel, pH tunable, zwitterionic NFs composed of uncharged nylon doped with the weakly basic, cationic polyallylamine hydrochloride and the weakly acidic anionic polycarboxylic acid to address the issue. Unlike the other cationic polymers investigated, e.g. polybrene and polyaniline, these polymers allow efficient NA extraction in Tris‐ethylenediamine tetra‐acetic acid buffer under mild conditions (pH 4.5 containing 0.1% Tween 20 for adsorption, and pH 10 with 50 mM NaCl for elution). Adsorption and elution yields over 95% and 70%, respectively, are achieved. It also discovered a correlation between material morphologies and the NA extraction suggests that the combination of polymer chemistries and nanofiber morphologies facilitates efficient NA extraction at low concentrations (ng range) within a short time period (<10 min). Considering the simple protocols and instrument‐free operation the as‐developed NFs are highly attractive for use in sample‐to‐answer NA testing in point‐of‐care settings. [ABSTRACT FROM AUTHOR]

The solid phase extraction of Au, Ir, Pd, Pt, and Rh on a polymer gel modified with ionic liquid containing methylimidazolium groups (MIA-PG) has been investigated. The positively charged surface of the sorbent is highly suitable for the sorption of stable chlorido complexes of the studied analytes, while the retention of base metals Cu, Fe, Ni, Zn, and Mn is negligible. Optimization experiments performed showed that, at 0.05 M HCl, the degree of sorption of Au, Ir, Pd, and Pt is above 95%, and only for Rh, the maximum degree is 65%; complete elution is achieved in the mixture of thiourea in HCl. The results obtained from the equilibrium adsorption studies are fitted in various adsorption models, such as Langmuir and Freundlich, and the model parameters have been evaluated. The kinetics analysis indicated that the adsorption of Au, Ir, Pd, Pt, and Rh onto the sorbent follows the pseudo-second-order model. Intraparticle diffusion and ion exchange reactions were the rate-limiting steps. Analytical procedures were developed for Pd, Pt, and Rh determination in road dust and soil and for Au determination in copper ore and copper concentrate. The procedures are validated by the analysis of certified reference materials. Analytical figures of merit confirmed their applicability in routine laboratory practice. [ABSTRACT FROM AUTHOR]

Macrolides are a group of compounds used to treat bacterial infections in humans and animals. Their widespread use results in the contamination of the water environment, which, on the one hand, has a detrimental effect on aquatic organisms and, on the other hand, can lead to the emergence of resistant strains of microorganisms. All of the above determines the need for monitoring of these compounds in the environment, particularly, in water objects. Usually, the high‐performance liquid chromatography combined with tandem mass spectrometry method is used to solve this problem, however, this work shows the possibility of using the supercritical fluid chromatography‐tandem mass spectrometry method. An approach for the determination of four common macrolides, namely erythromycin, clarithromycin, midecamycin, and josamycin, was developed. The use of solid‐phase extraction allowed to achieve limits of quantification at 0.57–6.8 ng/L. The presented approach was validated and tested on a real object—a sample of municipal wastewater. [ABSTRACT FROM AUTHOR]

Indacaterol, a β2 agonist prescribed for long-term management of patients with chronic obstructive pulmonary disease and asthma. In this study the first MISPE cartridges was developed using indacaterol as a template for its selective extraction from rat lung tissues, enabling precise pharmacokinetic evaluation at the drug's site of action. A molecular imprinting polymer was synthesized using indacaterol as a template, methacrylic acid as a functional monomer and ethylene glycol dimethacrylate as a cross-linker with a molar ratio (1: 4: 20). The polymer was characterized by a high binding capacity of 9840 ± 0.86 and high selectivity with an imprinting factor of 4.53 ± 0.12. The synthesized polymer was utilized as a sorbent in solid-phase extraction to purify and extract indacaterol from lung tissue matrix. The optimum molecularly imprinted solid-phase extraction (MISPE) conditions were 20.0 mg of molecular imprinting polymer and non-imprinting polymer, acetonitrile as the loading solvent, acetonitrile: water (20: 80; by volume) as the washing solvent, and methanol: acetic acid (90: 10; by volume) as the eluting solvent. A pharmacokinetic study was performed for indacaterol in rat lungs using the synthesized and optimized MISPE cartridge as a tool for sample purification. These parameters were determined in the lung tissues of rats emphasizing the local exposure of indacaterol to its target organ. The Cmax and Tmax were 51.020 ± 2.810 µg mL− 1 and 0.083 ± 0.001 h, respectively. The AUC 0−24 and AUC0 − inf were 175.920 ± 1.053 and 542.000 ± 5.245 µg h mL− 1, respectively. The elimination rate constant was 0.014 ± 0.00012 h− 1 and the half-life time was 48.510 ± 0.012 h. This study successfully developed and optimized MISPE cartridges using indacaterol as a template, enabling precise pharmacokinetic evaluation in rat lung tissues. The cartridges demonstrated high binding capacity and selectivity, providing crucial insights into the local exposure of indacaterol at its site of action. [ABSTRACT FROM AUTHOR]

Digital light processing (DLP) 3DP, commercial acrylate-based photocurable resins, and thermally expandable microspheres-incorporated flexible photocurable resins were employed to fabricate an SPE column with a thermally expanded monolithic foam for extracting Mn, Co, Ni, Cu, Zn, Cd, and Pb ions prior to the determination using inductively coupled plasma mass spectrometry. After optimization of the thermally activated foaming, the design and fabrication of the SPE column, and the automatic analytical system, the DLP 3D-printed SPE column with the thermally expanded monolithic foam extracted the metal ions with up to 14.8-fold enhancement (relative to that without incorporating the microspheres), with absolute extraction efficiencies all higher than 95.6%, and method detection limits in the range from 0.5 to 5.2 ng L–1. We validated the reliability and applicability of this method by determination of the metal ions in several reference materials (CASS-4, SLRS-5, 1643f, and Seronorm Trace Elements Urine L-2) and spiked seawater, river water, ground water, and human urine samples. The results illustrated that to incorporate the thermally expandable microspheres into the photocurable resins with a post-printing heating treatment enabled the DLP 3D-printed thermally expanded monolithic foam to substantially improve the extraction of the metal ions, thereby extending the applicability of SPE devices fabricated by vat photopolymerization 3DP techniques. [ABSTRACT FROM AUTHOR]

Zanthoxylum bungeanum, as a vital spice, the presence of its bitter components has a notable impact on the overall flavor of the food. To deeply explore the formation mechanism of the bitter components in Z. bungeanum and correlated influencing factors, this study used bitterness intensity as an indicator and employed sensory evaluation to optimize the processing conditions of Z. bungeanum during boiling and frying through single-factor optimization. Furthermore, organic solvent extraction, solid-phase extraction, and preparative high-performance liquid chromatography were used to isolate and concentrate the bitter fractions from Z. bungeanum water and oil. Subsequently, taste dilution analysis was employed to evaluate the contribution of these bitter fractions to the sensory characteristics of food. Additionally, high-performance liquid chromatography-mass spectrometry was adopted to identify the bitter components in Z. bungeanum water and oil. The results indicated that during the boiling process, increasing the amount of Z. bungeanum and extending the boiling time intensified the bitterness, while the bitterness of Z. bungeanum during frying process increased with raised temperature, extended frying time, and increased amount of Z. bungeanum. The recommended conditions for consumption and processing of Z. bungeanum water and Z. bungeanum oil were as follows: Z. bungeanum water was recommended to be boiled at 100 ℃ for 5 min, and the dosage of Z. bungeanum could be controlled at less than 2 g to reduce the bitter flavor. Z. bungeanum oil was recommended to be fried at 105~120 ℃ for 10~30 min, and the amount of Z. bungeanum could be added moderately to keep the bitter flavor low. The main bitter substances in Z. bungeanum water might be quercetin-3-rhamnose gentiobioside, quercetin-3,7-di-O-β-D-glucopyranoside, quercetin-3-O-robinobioside, and nuciferine, while the primary bitter compounds in Z. bungeanum oil were hydroxy-α-sanshool and hydroxy-β-sanshool. This study provides data reference and theoretical basis for the processing, quality control, and bitterness reduction of Z. bungeanum.

Abstract Indacaterol, a β2 agonist prescribed for long-term management of patients with chronic obstructive pulmonary disease and asthma. In this study the first MISPE cartridges was developed using indacaterol as a template for its selective extraction from rat lung tissues, enabling precise pharmacokinetic evaluation at the drug’s site of action. A molecular imprinting polymer was synthesized using indacaterol as a template, methacrylic acid as a functional monomer and ethylene glycol dimethacrylate as a cross-linker with a molar ratio (1: 4: 20). The polymer was characterized by a high binding capacity of 9840 ± 0.86 and high selectivity with an imprinting factor of 4.53 ± 0.12. The synthesized polymer was utilized as a sorbent in solid-phase extraction to purify and extract indacaterol from lung tissue matrix. The optimum molecularly imprinted solid-phase extraction (MISPE) conditions were 20.0 mg of molecular imprinting polymer and non-imprinting polymer, acetonitrile as the loading solvent, acetonitrile: water (20: 80; by volume) as the washing solvent, and methanol: acetic acid (90: 10; by volume) as the eluting solvent. A pharmacokinetic study was performed for indacaterol in rat lungs using the synthesized and optimized MISPE cartridge as a tool for sample purification. These parameters were determined in the lung tissues of rats emphasizing the local exposure of indacaterol to its target organ. The Cmax and Tmax were 51.020 ± 2.810 µg mL− 1 and 0.083 ± 0.001 h, respectively. The AUC 0−24 and AUC0 − inf were 175.920 ± 1.053 and 542.000 ± 5.245 µg h mL− 1, respectively. The elimination rate constant was 0.014 ± 0.00012 h− 1 and the half-life time was 48.510 ± 0.012 h. This study successfully developed and optimized MISPE cartridges using indacaterol as a template, enabling precise pharmacokinetic evaluation in rat lung tissues. The cartridges demonstrated high binding capacity and selectivity, providing crucial insights into the local exposure of indacaterol at its site of action.

Abstract Background Wastewater can contain a complex mixture of organic micropollutants, with both chemical analysis and effect-based methods needed to identify relevant micropollutants and detect mixture effects. Solid-phase extraction (SPE) is commonly used to enrich micropollutants prior to analysis. While the recovery and stability of individual micropollutants by SPE has been well studied, few studies have optimized SPE for effect-based methods. The aim of the current study was to develop and evaluate two standard operating procedures (SOPs) for the enrichment of micropollutants in preparation for chemical analysis and bioanalysis, one covering a broad range of chemicals and the other selective for estrogenic chemicals. Results Pristine surface water spiked with > 600 micropollutants was used to develop a generic extraction method for micropollutants with a wide range of physiochemical properties, while water spiked with estrogenic chemicals was used to identify a selective extraction method. Three different SPE sorbents were tested, with recoveries of individual chemicals and effect in assays indicative of mutagenicity, estrogenic activity, and fish embryo toxicity assessed. The sorbent HRX at pH 7 was selected for the generic extraction method as it showed the best recovery of both individual chemicals and effect in the bioassays. The sorbent HLB at pH 3 showed optimal recovery of estrogenic chemicals and estrogenic activity. The two optimal SPE methods were applied to spiked and unspiked wastewater effluents, with the concentrations of detected chemicals and observed effects similar to those of previous studies. The long-term storage of both extracts and SPE cartridges for estrogens and estrogenic activity after extraction with the HRX and HLB methods were evaluated, with estrogenic effectiveness close to 100% after 112 days when HLB was used. Conclusions HRX is recommended for generic extraction, while HLB is optimal for the selective extraction of estrogenic micropollutants. However, if a laboratory only wants to use a single SPE sorbent, HLB can be used for both generic and selective extraction as it yielded similar chemical and effect recovery as HRX for a wide range of micropollutants. This paper is supplemented by the final SOP that includes a variant for generic extraction and one for the extraction of estrogenic chemicals.

Phosphatidylcholine (PC), phosphatidyl ethanolamine (PE), phosphatidylserine (PS), and phosphatidylinositol (PI) are the four major phospholipids in Antarctic krill. In this study, the composition of these phospholipids was analyzed by hydrophilic interaction ultra-high performance liquid chromatography-tandem mass spectrometry (HILIC-UPLC-MS/MS) after purification by solid-phase extraction (SPE) using titania-coated fibrous silica (TiO2/KCC-1) nanoparticles, which had been prepared in our laboratory. The results showed that under the optimal conditions, 291 phospholipids including 75 PCs, 120 PEs, 54 PIs and 42 PSs were detected, which were nearly twice as many as those detected by a previously reported method. Phospholipids containing monounsaturated and polyunsaturated fatty acid chains accounted for 54.73% and 26.17% of the total phospholipids, respectively. PC (40:6) (41.63%), PE (36:0) (39.77%), PI (38:3) (80.05%), and PS (36:1) (81.62%) were found to be the most abundant in the four phospholipids. Multivariate statistical analysis showed significant differences in the types of phospholipids before and after SPE treatment. TiO2/KCC-1 nanoparticles exhibited a significant enrichment capacity for phospholipids, especially PC (18:0/18:0), PE (16:0/18:1), and PI (16:0/18:2). The detection limit was 0.05 μg/g for PC, PE and PS, and 0.01 μg/g for PI. The relative standard deviations (RSDs) for the four major phospholipids were in the range of 0.89% to 5.05%, and the recoveries were 87%–112%. This method demonstrated high specificity, extraction efficiency, sensitivity, precision and accuracy. Therefore, it has broad application prospects for the extraction, purification, and analysis of phospholipids in biological samples.

Background: Wastewater can contain a complex mixture of organic micropollutants, with both chemical analysis and effect-based methods needed to identify relevant micropollutants and detect mixture effects. Solid-phase extraction (SPE) is commonly used to enrich micropollutants prior to analysis. While the recovery and stability of individual micropollutants by SPE has been well studied, few studies have optimized SPE for effect-based methods. The aim of the current study was to develop and evaluate two standard operating procedures (SOPs) for the enrichment of micropollutants in preparation for chemical analysis and bioanalysis, one covering a broad range of chemicals and the other selective for estrogenic chemicals. Results: Pristine surface water spiked with > 600 micropollutants was used to develop a generic extraction method for micropollutants with a wide range of physiochemical properties, while water spiked with estrogenic chemicals was used to identify a selective extraction method. Three different SPE sorbents were tested, with recoveries of individual chemicals and effect in assays indicative of mutagenicity, estrogenic activity, and fish embryo toxicity assessed. The sorbent HRX at pH 7 was selected for the generic extraction method as it showed the best recovery of both individual chemicals and effect in the bioassays. The sorbent HLB at pH 3 showed optimal recovery of estrogenic chemicals and estrogenic activity. The two optimal SPE methods were applied to spiked and unspiked wastewater effluents, with the concentrations of detected chemicals and observed effects similar to those of previous studies. The long-term storage of both extracts and SPE cartridges for estrogens and estrogenic activity after extraction with the HRX and HLB methods were evaluated, with estrogenic effectiveness close to 100% after 112 days when HLB was used. Conclusions: HRX is recommended for generic extraction, while HLB is optimal for the selective extraction of estrogenic micropollutants. However, if a laboratory only wants to use a single SPE sorbent, HLB can be used for both generic and selective extraction as it yielded similar chemical and effect recovery as HRX for a wide range of micropollutants. This paper is supplemented by the final SOP that includes a variant for generic extraction and one for the extraction of estrogenic chemicals. [ABSTRACT FROM AUTHOR]

A simple, fast, and low-cost pre-concentration methodology based on the application of solid-phase extraction coupled to layered double hydroxides (LDHs) and capillary electrophoresis was developed for the determination of naproxen (NPX), diclofenac (DFC), and ibuprofen (IBP) in environmental sample waters. A systematic study of the LDH composition was designed, including the effects of interlayer anions (NO3−, Cl−, CO32−, BenO−, and SDS−) and the effect of molar ratio (Mg:Al). The optimal composition of MgAl/Cl−-LDH (Mg:Al; 1.5:1.0) was coupled to an SPE system: pH (neutral pH), LDH amount (15 mg), and extraction capacity ranged from 79.71 to 83.11% for the three anti-inflammatory non-steroidal agents analyzed. A recovery rate of up to 80.87% was obtained when 0.01 M chloride acid in methanol was used as the eluent and 50 mL of sample was used. Under optimal conditions, the linear range of the calibration curve ranges from 18.02 to 200 μg L−1, with limits of detection ranging from 6.03 to 18.02 μg L−1 for the three NSAIDs. The precision of the methodology was evaluated in terms of inter- and intra-day repeatability, with %RSD < 10% in all cases. The proposed method was applied to analyze environmental water samples (bottle, tap, cistern, well, and river water samples). The developed method is a robust technique capable of combining with other analytical methods to quantitatively determine anti-inflammatory non-steroidal agents. [ABSTRACT FROM AUTHOR]

The global rise of new psychoactive substances (NPSs) poses challenges for their analysis in biological matrices due to their complex chemistries and short market lifespan. A comparative study for the simultaneous extraction, separation, and detection of 19 NPSs was conducted. Six solid-phase extraction (SPE) methods and one supported liquid extraction method (SLE) were compared for the extraction of analytes from blood, serum, plasma, and urine. Comparisons of four derivatization agents were conducted, at four temperatures and two incubation times. Extraction methods were assessed by precision, sensitivity, and extraction efficiency. Derivatizing agents were assessed on their selectivity and sensitivity, and a three-way ANOVA was conducted to determine statistical significance. CSDAU SPE cartridges were shown to be the most efficient when extracting analytes from blood, serum, and plasma, whereas Xcel I cartridges performed the strongest when extracting analytes from urine. SPE extraction efficiencies, when utilizing the best-performing cartridges, ranged from 49 to 119%. SLE successfully extracted all analytes from all matrices (ranging from 22 to 120%). Pentafluoropropionic anhydride: ethyl acetate was the most successful derivatizing agent, allowing all analytes to be detected, with the highest peak area responses and more unique spectra. The optimum temperature for incubation was 37 °C, with no statistical difference found between the two incubation times. [ABSTRACT FROM AUTHOR]

As a result of their toxicity, ease of analysis, and environmental occurrence, 16 polycyclic aromatic hydrocarbons (PAHs) were chosen as priority pollutants by the USEPA. Few studies have been conducted to assess the levels of PAHs in South Africa, especially KwaZulu Natal province, and no work has been done in the selected study area. Therefore, this study aimed to evaluate the levels of such PAHs in river water and wastewater samples and evaluate their source and ecological risk. The status of these PAHs in the South African environment has not been investigated fully, which is a gap this study intended to fill. The PAHs were determined using solid‐phase extraction (SPE) and dispersive liquid–liquid microextraction (DLLME) methods. The optimization and validation of these methods indicated that both methods can be used for the extraction of PAHs in liquid samples. This is because of the acceptable %recovery of 72.1%–118% for SPE and 70.7%–88.4% for DLLME with a %RSD less than 10% (indicating high precision) that was obtained. The limit of detection and limit of quantification ranged from 5.0 to 18 ng/L and 6.0–20 ng/L for SPE and from 10 to 44 ng/L and 11 to 63 ng/L for DLLME. These results demonstrated that SPE is more accurate and sensitive than DLLME, which was also confirmed by statistical analysis. The PAH concentration levels ranged from not detected (nd) to 1046 ng/L in river water and nd to 778 ng/L in wastewater samples with naphthalene demonstrating dominance over all other PAHs in both water matrices. The PAHs were found to be of petrogenic origin and posed low ecological risk on average. Integr Environ Assess Manag 2024;20:1598–1610. © 2024 The Authors. Integrated Environmental Assessment and Management published by Wiley Periodicals LLC on behalf of Society of Environmental Toxicology & Chemistry (SETAC). Key Points: The river exhibited higher levels of polycyclic aromatic hydrocarbons (PAHs) contamination than the wastewater and naphthalene dominating both environments.The PAHs in the investigated areas are a result of petrogenic sources.All PAHs demonstrated a low ecological risk to the surrounding environment except for acenaphthylene and fluorene in College Road (CR) and anthracene in all the sampling sites.The outcome of this study encourages the need for regulatory control over the PAHs. [ABSTRACT FROM AUTHOR]

A novel doxorubicin hydrochloride liposome injection was prepared to reduce toxicity and side effects, as well as extend plasma half-life in the treatment of breast cancer. In this study, a rapid and sensitive bioanalytical method was developed and validated to characterize the pharmacokinetic profile of total and free doxorubicin in plasma of 3 Chinese patients after intravenous infusion of this injection. Plasma samples were prepared by protein precipitation for the determination of total doxorubicin, while solid phase extraction was used to determine free doxorubicin. After plasma sample pre-treatment, total and free concentrations were quantified individually using a validated LC-MS/MS method. The calibration curves were found to be linear in the range of 0.20–500.0 ng mL−1 for total doxorubicin and in the range of 1.00–1,000 ng mL−1 for free doxorubicin. The free concentrations in plasma were only one sixth to one quarter of the total levels. Liposomal doxorubicin had a longer apparent half-life (>50 h) than the non-targeted drug (<10 h) reported in the reference. and a lower volume of distribution. This novel injectable formulation steadily released free doxorubicin from liposomes over a long period of time to reduce cardiac toxicity and side effects, while ensuring a clinical curative effect. [ABSTRACT FROM AUTHOR]

In this study, amino-modified micro-mesoporous silica (NH2-MMS) with hierarchical pores was prepared by modifying micro-mesoporous silica ZSM-5 with 3-aminopropyltriethoxysilane and used as an adsorbent in solid-phase extraction to analyze free fatty acids (FFAs) in krill oil during storage for an initial time. The Brunner Emmet Teller adsorption experiment and Fourier transform infrared spectroscopy demonstrate that NH2-MMS, with a hierarchical pore structure, was successfully synthesized. The adsorption experiments, especially static adsorption, indicate that the absorption ability of the prepared NH2-MMS, with a hierarchical pore structure, toward FFAs was better than that of traditional amino-modified mesoporous silica (SBA-15) with a mesoporous structure at all temperature and concentrations. Fairly low limits of detection (0.06–0.15 μg g−1), acceptable recoveries (85.16–94.31%), and precision (0.08–5.26%) were attained under ideal circumstances. Moreover, NH2-MMS has the advantages of easy preparation and being environmentally friendly. As a result, this method offers an alternative to the current method for determining FFAs in different kinds of oil specimens. [ABSTRACT FROM AUTHOR]

UV spectrophotometric determination of salicylic acid in several multicomponent drugs using an ethylcellulose-based sorbent for solid-phase extraction (SPE) for sample preparation was shown to be selective. Selective binding of the analyte to sorbent active sites and stepwise elution successively with purified water and NaOH solution (0.1 M) during SPE eliminated interference of other active pharmaceutical ingredients of multicomponent drugs during identification and quantitation of salicylic acid by UV spectrophotometry. Use of the ethylcellulose sorbent made it possible to improve the metrological parameters and decrease systematic error of the quantitative procedure by an average of 47%. [ABSTRACT FROM AUTHOR]

This work focuses on the development of a hybrid material based on SBA-15 silica with a molecularly imprinted polymer (MIP), using spiramycin (SPI) as a template, for use as sorbent in solid-phase extraction (SPE). Characterization techniques such as nitrogen gas adsorption–desorption isotherms, infrared spectroscopy and scanning electron microscopy confirmed the structure and properties of the SBA-15@MIP-SPI material. SPE conditions using SBA-15@MIP-SPI as sorbent were optimized, which allowed us to demonstrate the high selectivity and adsorption capacity of SPI on the synthesized material. The best conditions were 50 mg of sorbent, loading with 1 mL of standard solution or sample of cow milk previously extracted in acetonitrile and eluting with 3 mL of methanol with 1% acetic acid. After the optimization process, the material demonstrated recovery percentages of 81 ± 3% in SPI standard solutions and showed its potential in cow milk samples (71 ± 6%). The novelty of the research consists of the combination of MIPs with SBA-15, which could offer important advantages in terms of specific surface area and porous structure, thus improving performance and reducing the amount of sorbent compared to other traditional methods. [ABSTRACT FROM AUTHOR]

To determine the paclitaxel-related substances in a paclitaxel injection (albumin-bound), it is necessary to remove human blood albumin from the sample via solid-phase extraction and subsequently perform high-performance liquid chromatography analysis. The pre-processing operation is complicated, the duration of analysis is long, and much human power and material resources are needed in the sample testing process. Thus, the purpose of this study was to develop a quick two-dimensional liquid chromatography method that requires less consumables and possesses high sensitivity. Samples were directly injected into one-dimensional solid-phase extraction columns to remove human blood albumin. Paclitaxel and its related substances in the solid-phase extraction columns were then eluted into two-dimensional analytical columns through valve switching technology. The sample pretreatment step can be omitted in this method, which allows for the analysis of paclitaxel and its related substances to be completed more quickly, within only 15 min, under the developed two-dimensional elution conditions. The established method had good linearity (R2 = 0.9994), limit of detection (0.25 μg·mL−1), limit of quantification (0.5 μg·mL−1), precision (RSD = 0.5%), and accuracy (102.53–107.97%). [ABSTRACT FROM AUTHOR]

For the first time, a highly permeable nanoporous carbon derived from melamine-based polybenzoxazine (NPC-PBZ-m) was used as the solid-phase extraction sorbent for trace analysis of atrazine (ATZ) herbicide in environmental water samples as a pre-treatment to enhance detection for high-performance liquid chromatography. Extraction performance was investigated using an agricultural field matrix-water sample. The parameters affecting the solid-phase extraction efficiency were carefully investigated. The optimisation conditions were determined as 200.0 mg of sorbent with an adsorption flow rate of 10.0 mL min−1, an elution flow rate of 1.0 mL min−1, and an elution volume of 3.0 mL. Moreover, it was not necessary to adjust the pH of the sample. Under these optimised extraction conditions, good linearity between 5.00 and 30.0 µg L−1 was achieved along with a limit of detection (LOD) of 1.25 µg L−1 and a limit of quantification (LOQ) of 3.79 µg L−1. Furthermore, the reusability of the NPC-PBZ-m column was found up to 8 cycles making it a new cost-effective material for herbicide enrichment. Finally, this developed method was successfully applied to analyse ATZ in water samples from rice fields, fish farms, and natural canal water, with 98–117% relative recoveries. These results indicate that NPC-PBZ-m with our proposed method is feasible and demonstrates its potential application as an effective adsorbent for herbicide enrichment. [ABSTRACT FROM AUTHOR]

The aim of this study was to develop a high‐performance liquid chromatography–tandem mass spectrometry method for the determination of 6‐cyanodopamine, 6‐nitrodopamine, 6‐nitrodopa, 6‐nitroadrenaline and 6‐bromodopamine in human plasma samples. Strata‐X 33 μm solid‐phase extraction cartridges were used for the extraction of the catecholamines from human plasma samples. The catecholamines were separated in a 150 × 3 mm Shim‐pack GIST C18‐AQ column with 3 μm particle size, placed in an oven at 40°C and perfused with 82% mobile phase A (acetonitrile–H2O; 90:10, v/v) + 0.4% acetic acid and 18% mobile phase B (deionized H2O) + 0.2% formic acid at a flow rate of 340 μl/min in isocratic mode. The injected volume was 4 μl and the run lasted 4 min. The method was linear from 0.1 to 20 ng/ml and the lower limit of quantification was 0.1 ng/ml for all analytes. The method was applied to evaluate the plasma levels of catecholamines in plasma of patients with chronic kidney disease and allowed the detection for the first time of circulating levels of the novel catecholamines 6‐bromodopamine and 6‐cyanodopamine. [ABSTRACT FROM AUTHOR]

Copyright of Journal of Food Safety & Quality is the property of Journal of Food Safety & Quality Editorial Department and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

Copyright of Shipin Kexue/ Food Science is the property of Food Science Editorial Department and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

In this work, we test metal–organic frameworks (MOFs) as sorbents in the solid-phase extraction (SPE) technique to determine chemical warfare agents (CWAs) and their related compounds in water samples. During this study, we used 13 target compounds to test the selectivity of MOFs thoroughly. Three MOFs were used: MIL-100(Fe), ZIF-8(Zn), and UiO-66(Zr). The obtained materials were characterized using FT-IR/ATR, SEM, and XRD. CWA's and related compounds were analyzed using gas chromatography coupled with tandem mass spectrometry (GC-MS/MS). The effect of the type of elution solvent and the amount of sorbent (MOFs) in the column on the efficiency of the conducted extraction were verified. The LOD ranged from 0.04 to 7.54 ng mL−1, and the linearity range for the analytes tested extended from 0.11/22.62 (depending on the compound) to 1000 ng mL−1. It was found that MOFs showed the most excellent selectivity to compounds having aromatic rings in their structure or a "spread" spatial structure. The best recoveries were obtained for DPAA, CAP, and malathion. Environmental water samples collected from the Baltic Sea were analyzed using an optimized procedure to verify the developed method's usefulness. [ABSTRACT FROM AUTHOR]

Neonicotinoids (NEOs), highly selective toward insect nicotinic acetylcholine receptors, are extensively used due to their effectiveness against pests and relative non‐toxicity to vertebrates. However, their prolonged persistence in soil and water has led to frequent detection in food and environmental samples, posing significant environmental and health concerns. Recent research indicates these pesticides infiltrate aquatic ecosystems, threatening aquatic life and human health. Here, we improved the ultra‐performance liquid chromatography‐mass spectrometry method for detecting NEOs in water samples, increasing its sensitivity to fulfill forthcoming detection needs. This approach enables the simultaneous quantification of eight NEOs and five NEO metabolites in diverse water sources, including tap, surface, groundwater, sewage, and seawater. Our method achieves remarkably low detection limits for direct injection (0.78–1.7 ng/L) and solid‐phase extraction methods (0.13–0.25 ng/L). Critically, our findings reveal that boiling domestic drinking water doesn't degrade NEOs; instead, it increases their concentration due to water evaporation. A 6‐min boiling period can amplify pesticide concentration by 4–5 times, presenting a significant hazard in culinary practices of specific regions where prolonged cooking could lead to alarmingly high levels of these insecticides. This research underscores the importance of monitoring and mitigating NEO contamination in water sources to safeguard environmental and public health. [ABSTRACT FROM AUTHOR]

This study presents a method based on acid transesterification and the purification by solid-phase extraction (SPE) coupled with gas chromatography–tandem mass spectrometry for quantifying 3- and 2-monochloropropanediol esters (3-MCPDE, 2-MCPDE) and glycidyl esters (GE) in nutritional foods. The fat was extracted by liquid–liquid extraction with petroleum ether and diethyl ether after the sample was hydrolysed with ammonia. Then the extract was purified by a SPE cartridge filled with the aminopropyl sorbents. It was demonstrated that the optimal elution volume for 3-MCPDE, 2-MCPDE and GE greatly depended on the sample matrix and varied from 6 to 12 mL for four different kinds of food matrices. All three analytes in the sample solution could be fully collected in the first 10–12 mL of eluate. By this way, monoacylglycerols commonly present in the samples were fully removed. Therefore, the overestimation of GE quantification was effectively eliminated. The modified analytical procedure was fully validated in a single laboratory and has been recommended as a Chinese Food Safety National Standard. In addition, two derivatisation agents, heptafluorobutyrylimidazole and phenylboronic acid, were proved to be equivalent in method accuracy and precision for the quantification of three analytes. [ABSTRACT FROM AUTHOR]

Background: The analysis of vitamins in baby food is a challenging task given the complexity of the food matrix, vitamin stability, and strict regulations of the European Union regarding permissible deviations from declared values. Vitamins in food exist in different concentrations and forms and have different stabilities; thus, the preparation of samples for a reliable analysis using the same procedure is not straightforward. Therefore, significant attention has been devoted to optimizing sample preparation in the analysis of vitamins. Methods: This study aims to determine which of the sample preparation and extraction methods is the most efficient for the simultaneous determination of vitamins A, D, E, and K in milk and baby food using high-performance liquid chromatography (HPLC). Different samples of baby food were prepared in seven different ways based on four methods (saponification, enzymatic hydrolysis, solvent extraction, and solid-phase extraction). Results and Conclusions: According to the validation parameters, the optimal preparation method proved to be solid-phase extraction with a C18 stationary phase, with recoveries of 97.4%, 96.1%, 98.3%, and 96.2% for vitamins A, D, E, and K, respectively, and HPLC with a UV–Vis detector was identified as a sufficiently sensitive technique for the identification and quantification of fat-soluble vitamins in milk and baby food. [ABSTRACT FROM AUTHOR]

Food analysis plays an important role in preserving the integrity and quality of food. Despite these noble goals, most official methods for the analysis of nutrients (vitamins, carotenoids, etc.) antioxidants (polyphenols, etc.), and contaminants (pesticides, veterinary drugs, mycotoxins etc.) still rely on time-consuming, complex, and polluting procedures of sample preparation. To solve this discrepancy, the scientific community has frantically been working to make extraction procedures faster and safer, resorting to miniaturization, automation, low-energy consumption, and solvents/sorbents from renewable resources. This review provides an overview of the most sustainable extraction methods in food analysis, developed over the last ten years (2014–2024), including relevant examples of both liquid phase and sorbent-based techniques. Particular emphasis is placed on solutions aimed at improving the method sustainability such as smart devices, neoteric solvents, and composite sorbents, discussing the latest advancements and future trends in this sector.

Solid-phase analytical derivatization is a versatile sample preparation technique that enhances analysis accuracy, efficiency, reproducibility, and sensitivity. The technique combines the advantages of analytical derivatization and solid-phase extraction, providing a versatile approach for analysing analytes with various functional groups in complex matrices. Analytical derivatization is a technique used for functional group analysis that involves modifying the structure of an analyte to enhance sensitivity and specificity. Solid-phase analytical derivatization is a one-pot procedure that combines analytical derivatization and extraction. In the presence of acids, it can derivatize phenols, carboxylic acids, and other analytes. Furthermore, solid-phase analytical derivatization increases the reaction rate of carbonyl compounds, making it easier to extract aldehydes and ketones rapidly. This technique utilises electrophoresis, chromophores, fluorophores, and functional groups for detection and extraction. It initially began as a batch procedure but has now developed into an automated, microextraction, and derivatization method. Solid-phase analytical derivatization is highly efficient due to the significant excess of the derivatizing reagent relative to the analyte, along with the pre-impregnation of derivatizing reagents, which can speed up the process compared to traditional solution-based derivatization. This tutorial aims to provide detailed insights into the practical aspects of implementing solid-phase analytical derivatization in analytical method development and discuss the prospects and future trends.

Abstract Nucleic acid (NA) testing at the point‐of‐care requires efficient NA extraction followed by post‐NA amplification to achieve necessary detection sensitivity. Nanofibers (NFs) are demonstrated to be an ideal solid surface in an NA extraction process but necessitate harsh conditions that interfere with the subsequent NA amplification process. It is demonstrated that novel, pH tunable, zwitterionic NFs composed of uncharged nylon doped with the weakly basic, cationic polyallylamine hydrochloride and the weakly acidic anionic polycarboxylic acid to address the issue. Unlike the other cationic polymers investigated, e.g. polybrene and polyaniline, these polymers allow efficient NA extraction in Tris‐ethylenediamine tetra‐acetic acid buffer under mild conditions (pH 4.5 containing 0.1% Tween 20 for adsorption, and pH 10 with 50 mM NaCl for elution). Adsorption and elution yields over 95% and 70%, respectively, are achieved. It also discovered a correlation between material morphologies and the NA extraction suggests that the combination of polymer chemistries and nanofiber morphologies facilitates efficient NA extraction at low concentrations (ng range) within a short time period (

This work showcases a novel application of biochar for analytical sample treatment. The carbonaceous material, obtained by pyrolysis of orange peel waste (550°C) without any post-synthesis treatment or functionalization, was thoroughly characterized and easily immobilized on the inner wall of sampling tubes in order to perform a sort of “in-vial” solid-phase extraction (SPE). The as-obtained device was tested for the extraction of seven sexual steroids, as probe water pollutants, from tap, lake, river water and wastewater treatment plant effluent samples spiked with 0.2-5 µg L−1 of each compound. The sorption kinetics profiles showed quantitative uptake from the sample (25 mL) in 20 min contact time, followed by complete elution in pure ethanol (2 mL, 15 min), thanks to the proper balance between sorption affinity and ease of elution. Under the selected conditions, recovery was in the range 60-123 %, with good inter-day precision (RSD 10-18 %, n=3). As evidence of the excellent reproducibility, an overall RSD below 15 % was observed from inter-day inter-batch recovery tests on three individually prepared sampling tubes. The procedure, carried out on a roller mixer, allows 10 samples to be extracted simultaneously, improving the sample throughput. Moreover, reusability tests showed that the same device maintains its efficiency for 10 consecutive sorption/desorption cycles. The greenness assessment, carried out by two dedicated software, further supported the sustainability of this biochar-based sample preparation as an alternative SPE.

Rapid analysis of multiple food allergens is required to confirm the appropriateness of food allergen labelling in processed foods. This study aimed to develop a rapid and reliable method to simultaneously detect trace amounts of seven food allergenic proteins (wheat, buckwheat, milk, egg, crustacean, peanut, and walnut) in processed foods using LC-MS/MS. Suspension-trapping (S-Trap) columns and on-line automated solid-phase extraction were used to improve the complex and time-consuming pretreatment process previously required for allergen analysis using LC-MS/MS. The developed method enabled the simultaneous detection of selected marker peptides for specific proteins derived from seven food ingredients in five types of incurred samples amended with trace amounts of allergenic proteins. The limit of detection values of the method for each protein were estimated to be