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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]

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]

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]

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]

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]

Mixed-mode high-performance liquid chromatography (HPLC) is increasingly used for the analysis of ionic and highly hydrophilic drugs, which are difficult to separate by conventional single-mode HPLC. In the former case, chromatographic separation is achieved using one of the several commercially available mixed-mode stationary phases, typically combinations of reversed and ion-exchange phases. Moreover, mixed-mode stationary phases can be used as solid-phase extraction (SPE) sorbents. This review focuses on the recent applications of mixed-mode stationary phases in the chromatographic analysis of bioactive compounds, such as drugs, herbicides, and pesticides. Specifically, we briefly summarize HPLC methods utilizing mixed-mode stationary phases and SPE pretreatment procedures utilizing mixed-mode sorbents developed in the last decade, thus providing a reference work for overcoming the difficulties in analyzing ionized or hydrophilic drugs by conventional reversed-phase chromatography. [ABSTRACT FROM AUTHOR]

In the past few decades, considerable scientific strides have been made in the subject of drug analysis in human biological samples. However, the risk caused by incorrect drug plasma levels in patients still remains an important concern. This review paper attempts to investigate the advances made over the last ten years in common sample preparation techniques (SPT) for biological samples based on solid sorbents, including solid-phase extraction (SPE) and solid-phase micro-extraction (SPME), and in particular in the field of molecularly imprinted polymers (MIPs), including non-stimuli-responsive and stimuli-responsive adsorbents. This class of materials is known as 'smart adsorbents', exhibiting tailored responses to various stimuli such as magnetic fields, pH, temperature, and light. Details are provided on how these advanced SPT are changing the landscape of modern drug analysis in their coupling with liquid chromatography-mass spectrometry (LC-MS) analytical techniques, a general term that includes high-performance liquid chromatography (HPLC) and ultra-high performance liquid chromatography (UHPLC), as well as any variation of MS, such as tandem (MS/MS), multiple-stage (MSn), and high-resolution (HRMS) mass spectrometry. Some notes are also provided on coupling with less-performing techniques, such as high-performance liquid chromatography with ultraviolet (HPLC-UV) and diode array detection (HPLC-DAD) detection. Finally, we provide a general review of the difficulties and benefits of the proposed approaches and the future prospects of this research area. [ABSTRACT FROM AUTHOR]

The amount of macrolide (MAL) residues in aquatic products, including oleandomycin (OLD), erythromycin (ERM), clarithromycin (CLA), azithromycin (AZI), kitasamycin (KIT), josamycin (JOS), spiramycin (SPI), tilmicosin (TIL), tylosin (TYL), and roxithromycin (ROX), was determined using solid-phase extraction and ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS). The residues were extracted with 1% ammonia acetonitrile solution and purified by neutral alumina adsorption. Chromatographic separation was completed on an ACQUITY UPLC BEH C18 column with acetonitrile–0.1% formic acid aqueous solution as the mobile phase, and mass spectrometry detection was performed by multiple reaction monitoring scanning with the positive mode in an electrospray ion source (ESI+). Five isotopically labeled compounds were used as internal standards for quality control purposes. The findings indicated that across the mass concentration span of 1.0–100 μg/L, there was a strong linear correlation (R2 > 0.99) between the concentration and instrumental response for the 10 MALs. The limit of detection of UPLC-MS/MS was 0.25–0.50 μg/kg, and the limit of quantitation was 0.5–1.0 μg/kg. The added recovery of blank matrix samples at standard gradient levels (1.0, 5.0, and 50.0 μg/kg) was 83.1–116.6%, and the intra-day precision and inter-day precisions were 3.7 and 13.8%, respectively. The method is simple and fast, with high accuracy and good repeatability, in line with the requirements for accurate qualitative and quantitative analysis of the residues for 10 MALs in aquatic products. [ABSTRACT FROM AUTHOR]

In this study, adsorbents based on molecularly imprinted polymers (MIPs) in two solid-phase extraction application forms, pipette tip and magnetic extraction, were used for the selective extraction of coumarins. The pipette-tip solid-phase extraction reduced solvent volumes; the magnetic MIP extraction was simple and effective for phase separation. Parameters affecting extraction, such as the amount of adsorbent, type of washing solvent, volume of the elution solvent, and extraction times for magnetic extraction, were optimized. The MIP-based adsorbents displayed high selectivity and extraction efficiency, resulting in recoveries ranging from 70.3 to 102.0% (RSD % less than 5.5%) for five coumarins under study, 6,7-dihydroxycoumarin-6-β-D-glucoside, coumarin, 7-methoxycoumarin, 6-methylcoumarin, and dicoumarol. The extracts were analyzed by high-performance liquid chromatography with diode array (DAD) and fluorescence (FLD) detectors, reaching limits of quantification of 0.5 and 0.9 µg·mL−1 for coumarin and dicoumarol detected by DAD and 0.001–0.012 µg·mL−1 for the other prohibited simple coumarins when used as a fragrance (detected by FLD). The proposed method was validated and its applicability was shown for the analysis of cosmetic samples like shower gel and perfume. [ABSTRACT FROM AUTHOR]

A citric acid cross-linked β-cyclodextrin (β-CD) polymer was synthesized and loaded on micro-ceramic balls to fabricate the solid-phase adsorbents (P-MCB) for adsorption and extraction of triazole pesticides from water. The stability of β-CD polymer and P-MCB was investigated in solutions with different pH values at different temperatures. The adsorption properties and the influence of kinetics, sorbent amount, pesticide concentration, and temperature on the adsorption capacity were evaluated. The results showed P-MCB had favorable adsorption of 15.98 mg/g flutriafol in 3.5 h. The equilibrium data followed the Freundlich equation, and the adsorption of flutriafol and diniconazole followed the second-order kinetics. The recovery rate of P-MCB for triazole pesticides in water was satisfactory, and the recovery rate was still 80.1%, even at the 10th cycle. The P-MCB had good stability, with a degradation rate of 0.2% ± 0.08 within 10 days, which could ensure extraction and recycling. [ABSTRACT FROM AUTHOR]

Some South American countries have ancient traditions that may pose legal problems, such as the consumption of coca leaves, as this can provide positive results for cocaine use after the analysis of biological samples. For this reason, it is necessary to find specific markers that help differentiate legal from illegal consumption, such as tropacocaine, cinnamoylcocaine, and especially hygrine and cuscohygrine. In this work, two techniques for collecting biological samples are compared: the Quantisal® Oral Fluid collection device and passive drooling. Once the samples were collected, they were subjected to solid-phase extraction for subsequent injection into GC-MS. Different validation parameters included in international guides have been studied to evaluate whether the proposed method is valid for the defined purpose, placing special emphasis on the study of the matrix effect and little value on GC-MS analyses. With respect to this parameter, an increase in the signal was found for CUS and t-CIN, but it was not significant for the rest of the substances studied. The recoveries have varied significantly depending on the way of working, being higher when working with standardized areas. After carrying out work with the oral fluid samples collected from laboratory volunteers, the method was applied to two real samples. The results obtained support the need for further research to overcome certain limitations presented by the device. [ABSTRACT FROM AUTHOR]

Fatty acid analysis is an essential step in evaluating the potential of macroalgae for biodiesel production. An extraction method was developed to simultaneously analyze up to five types of biodiesel-fuel-related fatty acids (myristic acid, palmitic acid, cis-palmitvaccenic acid, stearic acid, and oleic acid) in macroalgae using liquid chromatography and tandem mass spectrometry (LC–MS/MS). Lypophilization and solid-phase extraction (SPE) techniques were applied to improve the extraction efficiency and effectively purify samples. The optimal conditions for SPE were set by comparing the recoveries according to the various solvent conditions for each step (loading, washing, and elution). In addition, the introduction of trimethylaminoethyl (TMAE) derivatives to the hydroxyl group of the target analyte increased the ionization efficiency and sensitivity. The derivatized samples were analyzed using the LC–MS/MS method with electrospray ionization in the positive and multiple-reaction monitoring modes. The target analytes were separated and detected within 13.5 min using a CAPCELL PAK C18 MGII S3 column. Gradient elution was performed using distilled water and acetonitrile containing 5 mM ammonium acetate. This method offers a reliable and sensitive tool for the analysis of macroalgae samples for their potential use in biodiesel production. To the best of our knowledge, this is the first report on the simultaneous determination of fatty acids in macroalgae using LC–MS/MS with TMAE derivatization. [ABSTRACT FROM AUTHOR]

Non-steroidal anti-inflammatory drugs (NSAIDs) have been recognized as a potentially serious threat to the natural environment. NSAIDs are popular painkillers, and the main pathway for them to reach natural water is via discharge from wastewater and sewage treatment plants. In order to monitor contamination caused by these drugs, as well as their impact on the environment, a new material based on Silica Gel 60, functionalized with a dendrimeric copolymer of methylamine and 1,4-butanediol diglycidyl ether (named MA-BDDE), was prepared. Initial physicochemical characterization of the MA-BDDE material was carried out using ATR FT-IR spectroscopy as well as solid-state carbon-13 NMR spectroscopy. Its effectiveness at NSAID extraction was evaluated by the application of five select drugs in dispersive solid-phase extraction (dSPE): aspirin, ketoprofen, naproxen, diclofenac and ibuprofen. This was followed by their simultaneous determination using the HPLC-UV/Vis system demonstrating good sensitivity, with limits of detection values within the 63–265 ng mL−1 range. A comparison of the sorption capacity of each pharmaceutical with unmodified base silica showed an at least tenfold increase in capacity after modification. Initial MA-BDDE application in a quick, low-waste extraction procedure of those select NSAIDs from spiked surface water samples yielded promising results for its use as a sorbent, as recovery values of analytes adsorbed from various samples were found to exceed 72%. [ABSTRACT FROM AUTHOR]

Using straightforward and cost-effective methods, persimmon leaves were converted into high-quality powder. This powder was applied as an adsorbent for the removal of Cu(II) and Cd(II) from aqueous solutions. Scanning electron microscopy (SEM) revealed the presence of particles with non-homogeneous sizes and rough textures. The biosorbent exhibited a specific surface area of approximately 0.44 ± 0.015 m2 g−1. Elemental analysis and energy-dispersive X-ray spectroscopy (EDX) confirmed the presence of elements such as sulfur, phosphorus, nitrogen, and oxygen. The results of 13C nuclear magnetic resonance (13C-NMR), obtained using the cross-polarization technique, show the presence of groups containing sulfur and oxygen. Infrared spectroscopy (FTIR) indicated the existence of amine and hydroxyl groups. The material was used in the solid-phase extraction of Cu(II) and Cd(II) in batch experiments, and its adsorption capacity was evaluated as a function of time, pH, and analyte concentration. The fraction with a diameter between 63 and 106 μm was selected for the adsorption tests. Kinetic equilibrium was reached within 5 min, and the experimental data were fitted to the pseudo-second-order kinetic model. The optimum pH for the adsorption of both metal species was approximately 5.0. The adsorption isotherms were adjusted using the modified Langmuir equation, and the maximum amount of metal species extracted from the solution was determined to be 0.213 mmol g−1 for Cu(II) and 0.215 mmol g−1 for Cd(II), with high linear correlation coefficients for both metals. Persimmon leaves are typically abundant during the growing season, and because they are seasonal, the Diospyros kaki L.f. tree undergoes the natural process of leaf abscission, ensuring the availability of leaves for application. [ABSTRACT FROM AUTHOR]

Speciation analysis is a relevant topic since the (eco)toxicity, bioavailability, bio (geo)chemical cycles, and mobility of a given element depend on its chemical forms (oxidation state, organic ligands, etc.). The reliability of analytical results for chemical species of elements depends mostly on the maintaining of their stability during the sample pretreatment step and on the selectivity of further separation step. Solid-phase extraction (SPE) is a matter of choice as the most suitable and widely used procedure for both enrichment of chemical species of elements and their separation. The features of sorbent material are of great importance to ensure extraction efficiency from one side and selectivity from the other side of the SPE procedure. This review presents an update on the application of polymeric materials in solid-phase extraction used in nonchromatographic methods for speciation analysis. [ABSTRACT FROM AUTHOR]

This study investigates electrospun fibers of metal-organic frameworks (MOFs), particularly CuBTC and ZIF-8, in polyacrylonitrile (PAN) for the solid-phase extraction (SPE) of Tamoxifen (TAM) and its metabolites (NDTAM, ENDO, and 4OHT) from human blood plasma. The focus is on the isolation, pre-concentration, and extraction of the analytes, aiming to provide a more accessible and affordable breast cancer patient-monitoring technology. The unique physicochemical properties of MOFs, such as high porosity and surface area, combined with PAN's stability and low density, are leveraged to improve SPE efficiency. The study meticulously examines the interactions of these MOFs with the analytes under various conditions, including elution solvents and protein precipitators. Results reveal that ZIF-8/PAN composites outperform CuBTC/PAN and PAN alone, especially when methanol is used as the protein precipitator. This superior performance is attributed to the physicochemical compatibility between the analytes' properties, like solubility and polarity, and the MOFs' structural features, including pore flexibility, active site availability, surface polarity, and surface area. The findings underscore MOFs' potential in SPE applications and provide valuable insights into the selectivity and sensitivity of different MOFs towards specific analytes, advancing more efficient targeted extraction methods in biomedical analysis. [ABSTRACT FROM AUTHOR]

Mycotoxins are toxic metabolites of molds which can contaminate food and beverages. Because of their acute and chronic toxicity, they can have harmful effects when ingested or inhaled, posing severe risks to human health. Contemporary analytical methods have the sensitivity required for contamination detection and quantification, but the direct application of these methods on real samples is not straightforward because of matrix complexity, and clean-up and preconcentration steps are needed, more and more requiring the application of highly selective solid-phase extraction materials. Molecularly imprinted polymers (MIPs) are artificial receptors mimicking the natural antibodies that are increasingly being used as a solid phase in extraction methods where selectivity towards target analytes is mandatory. In this review, the state-of-the-art about molecularly imprinted polymers as solid-phase extraction materials in mycotoxin contamination analysis will be discussed, with particular attention paid to the use of mimic molecules in the synthesis of mycotoxin-imprinted materials, to the application of these materials to food real samples, and to the development of advanced extraction methods involving molecular imprinting technology. [ABSTRACT FROM AUTHOR]

An analysis methodology was optimised and validated for the quantification of opium alkaloids (OAs) in ground poppy seeds. This involved ultrasound-assisted extraction (UAE) and solid-phase extraction (SPE) purification before analysis using a high-performance liquid chromatography mass spectrometry detector (HPLC-MS/MS). UAE was optimised through the design of experiments with three factors and a three-level full factorial design. For SPE optimisation, a commercial material was compared with a previously synthesised material of SBA-15 silica functionalised with sulfonic groups (SBA-15-SO3−). The synthesised material demonstrated superior efficiency with only 25 mg and proved to be reusable for up to four cycles. The methodology was properly validated in terms of linearity, limits of detection and quantification, and selectivity. Matrix effects were negligible; adequate recovery values (85–100%) and inter-day and intra-day precision (≤15%) were obtained. The greenness of the method was evaluated with the AGREEprep metric scale, being more environmentally friendly compared to OA analysis methods. Finally, the method was applied to different samples of ground poppy seeds and revealed a concentration of 140 mg/kg of morphine equivalents in one of the samples, surpassing the legislatively established limits by sevenfold. This highlights the need to analyse these types of samples to mitigate potential public health issues. [ABSTRACT FROM AUTHOR]

This paper describes a new methodology for carrying out quantitative extraction of cloxacillin from drinking and river water samples using a molecularly imprinted polymer (MIP) as a selective sorbent for solid-phase extraction (MISPE). Several polymers were synthesized via thermal polymerization using cloxacillin as a template, methacrylic acid (MAA) as a functional monomer, ethyleneglycoldimethacrylate (EGDMA) as a cross-linker and different solvents as porogens. Binding characteristics of the adequate molecularly imprinted and non-imprinted (NIP) polymers were evaluated via batch adsorption assays following the Langmuir and Freundlich isotherms and Scatchard assays. The parameters related to the extraction approach were studied to select the most appropriate polymer for cloxacillin determination. Using the optimized MIP as the SPE sorbent, a simple sample treatment methodology was combined with high-performance liquid chromatography (HPLC) to analyze cloxacillin residues in drinking and river water. Under the optimum experimental conditions, the MISPE methodology was validated using spiked samples. The linearity for cloxacillin was assessed within the limits of 0.05–1.5 µg L−1 and the recovery percentage was higher than 98% (RSD < 4%). The limits of detection and limits of quantification were 0.29 and 0.37 µg L−1 and 0.8 and 0.98 µg L−1 for drinking and river water, respectively. The selectivity of MIP against other ß-lactam antibiotics with similar structures (oxacillin, cefazoline, amoxicillin and penicillin V) was studied, obtaining a good recovery higher than 85% for all except cefazoline. The proposed MISPE-HPLC methodology was successfully applied for the detection of cloxacillin in drinking water from Canal de Isabel II (Madrid) and river water from the Manzanares River (Madrid). [ABSTRACT FROM AUTHOR]

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

In the development of bioanalytical LC-MS methods for the determination of drugs in plasma samples in a clinical setting, adequate sample preparation is of utmost importance. The main goals are to achieve the selective extraction of the analytes of interest and attain thorough matrix removal while retaining acceptable ecological properties, cost-effectiveness, and high throughput. Solid-phase extraction (SPE) offers a versatile range of options, from the selection of an appropriate sorbent to the optimisation of the washing and elution conditions. In this work, the first SPE method for the simultaneous extraction of six anticancer drugs used in novel therapeutic combinations for advanced breast cancer treatment—palbociclib, ribociclib, abemaciclib, anastrozole, letrozole, and fulvestrant—was developed. The following sorbent chemistries were tested: octylsilyl (C8), octadecylsilyl (C18), hydrophilic–lipophilic balance (HLB), mixed-mode cation-exchange (MCX and X-C), and mixed-mode weak cation-exchange (WCX), with different corresponding elution solvents. The samples were analysed using LC-MS/MS, with a phenyl column (150 × 4.6 mm, 2.5 μm). The best extraction recoveries (≥92.3%) of all analytes were obtained with the C8 phase, using methanol as the elution solvent. The optimised method was validated in the clinically relevant ranges, showing adequate precision (inter-day RSD ≤ 14.3%) and accuracy (inter-day bias −12.7–13.5%). Finally, its applicability was successfully proven by the analysis of samples from breast cancer patients. [ABSTRACT FROM AUTHOR]

Pesticides can easily enter the food chain, harming bee populations and ecosystems. Exposure of beehive products to various contaminants has been identified as one of the factors contributing to the decline in bee populations, and multiple food alerts have been reported. Despite this fact, royal jelly, a valuable bee product with nutritional and functional properties, has received less attention in this context. Pesticide residues of different chemical class can contaminate royal jelly when foraging bees collect pollen or nectar from pesticide-treated flowers, or in some cases, due to its frequent and inappropriate use in the treatment of mites in beehives. To monitor this issue and also make it more reliable, it is crucial to develop effective sample preparation methods for extracting pesticides from royal jelly for subsequent analysis. In this context, this review provides information about sample preparation methods (solid-phase extraction, solvent extraction, and QuEChERS—quick, easy, cheap, effective, rugged and safe) and analytical methods that have been validated or improved to extract and analyze pesticides, respectively, in royal jelly samples of different origins. Finally, future perspectives are discussed. With this background, we aim to provide data that can guide future research related to this topic. [ABSTRACT FROM AUTHOR]

A simple and efficient sample pretreatment technology is very important for the accurate determination of trace drug residues in foods to ensure food safety. Herein, we report a new carboxyl group-functionalized ionic liquid hybrid solid- phase adsorbent (PS-IL-COOH) for the highly efficient extraction and quantitative determination of diclofenac sodium (DS) residue in milk samples. It was found that the adsorption efficiency of PS-IL-COOH for the ppb level of DS was greater than 93.0%, the adsorption capacity was 934.1 mg/g, and the enrichment factor was 620.0, which surpass most of the previously reported values for DS adsorbents. The high concentration of salts did not interfere with the adsorption of DS. Importantly, the recovery of DS was above 90% after 16 adsorption–-regeneration cycles. The synergistic effect of the multiple interactions was found to be the main factor for the high efficiency of DS adsorption. The proposed method was applied to the extraction and detection of DS in milk samples, with the relative recovery ranging from 88.2 to 103.0%. [ABSTRACT FROM AUTHOR]

Antibiotic drug residues can adversely affect the human body. Lincomycin is a common veterinary drug that can form residues in foods of animal origin. However, the detection of trace residue levels of lincomycin residues in real samples is challenging. Here, a simple solid phase extraction (SPE) method was developed for the enrichment of lincomycin from cow milk samples before its detection by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The adsorbent used in the SPE was a Cu-based metal-organic framework (Cu-MOF) prepared by the solvothermal synthesis approach. The prepared MOFs were characterized using scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FT-IR), X-ray diffractometry (XRD), differential thermogravimetric analysis (TG-DTA), and N2 adsorption-desorption experiments. The adsorption capacity (adsorption equilibrium, extraction time, pH), and elution solvent parameters were investigated. Under the optimized conditions of the HPLC-MS/MS method, lincomycin was detected in the linear range of 10–200 g/L with a detection limit of 0.013 ng/mL. Commercial milk samples were spiked with lincomycin, and a recovery rate between 92.3% and 97.2% was achieved. Therefore, the current method can be successfully applied for the enrichment and determination of lincomycin from milk samples. [ABSTRACT FROM AUTHOR]

Here, we propose a concept of immobilized sorption-colorimetric microprobes for preconcentration and sensing of colored analytical forms. Individual particles of sorbents distributed over a small area of 1 mm × 1 mm and attached to an easy-to-made strip with an adhesive layer were considered as the probes producing colorimetric responses through preconcentration of colored analytical forms. These responses were then directly recorded with a scanner at 1200 dpi, separated from a background, and processed to obtain information about the amounts of analytes. The food dyes Fast Green FCF, and Ponceau-4R were used as the proof-of-concept colored analytes. The microprobes based on silica modified with quaternary ammonium bases and on alumina were studied. Some features of the analytes' adsorption by the probes and their scanometric sensing were found. It was shown that the proposed method is applicable for the determination of 1–7 mg L−1 of the dyes. [ABSTRACT FROM AUTHOR]

Since active pharmaceutical ingredients (APIs) are directly related to human health, monitoring and quantifying them in the environment is a crucial and challenging issue. Using capillary-zone electrophoresis (CZE), four frequently used fluoroquinolones (FQs), ciprofloxacin, sparfloxacin, moxifloxacin, and gatifloxacin, were efficiently isolated and measured in pharmaceutical industrial wastewater. Solid-phase extraction (SPE) was developed and used as an efficient sample pretreatment procedure. The capillary electrophoretic procedure's various parameters were tuned to produce the optimal separation pattern for the drugs under consideration. All of the drugs under study were quantified in a concentration range of 0.5 to 50 µg/mL. After full assay validation in compliance with ICH-Q2B criteria, real wastewater samples were subjected to effective SPE, and the proposed assay was successfully used to determine the examined FQs in real wastewater samples. [ABSTRACT FROM AUTHOR]

In this paper, an imine-based porous 3D covalent organic polymer (COP) was synthesized via solvothermal condensation. The structure of the 3D COP was fully characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, and powder X-ray diffractometry, thermogravimetric analysis, and Brunauer–Emmer–Teller (BET) nitrogen adsorption. This porous 3D COP was used as a new sorbent for the solid-phase extraction (SPE) of amphenicol drugs, including chloramphenicol (CAP), thiamphenicol (TAP), and florfenicol (FF) in aqueous solution. Factors were investigated for their effects on the SPE efficiency, including the types and volume of eluent, washing speed, pH, and salinity of water. Under the optimized conditions, this method gave a wide linear range (0.1–200 ng/mL) with a high correlation coefficient value (R2 > 0.99), low limits of detection (LODs, 0.01–0.03 ng/mL), and low limits of quantification (LOQs, 0.04–0.10 ng/mL). The recoveries ranged from 83.98% to 110.7% with RSDs ≤ 7.02%. The good enrichment performance for this porous 3D COP might contribute to the hydrophobic and π–π interactions, the size-matching effect, hydrogen bonding, and the good chemical stability of 3D COP. This 3D COP-SPE method provides a promising approach to selectively extract trace amounts of CAP, TAP, and FF in environmental water samples in ng quantities. [ABSTRACT FROM AUTHOR]

The objective of this analysis is to establish the potential of biodegradable agro-industrial waste materials as biosorbents in the solid-phase extraction (SPE) technique for sample preparation. In this regard, waste coffee husk (CH) powder was collected, washed, treated chemically, characterized, and applied as an SPE adsorbent to extract pantoprazole from the wastewater samples. Sample detection was accomplished using the UPLC-MS/MS system. The positive mode of electrospray ionization was exploited for the ionization of the sample, and quantification of the target analyte was performed by the multiple reaction monitoring modes. The precursor to product ion transition of 384.02→1380.05 and 384.02→200.05 was used as qualifiers and quantifiers, respectively. Optimization of the particle size, adsorbent dose, and contact time were evaluated to select the best combination of features. The efficiency and regeneration capability of the CH were compared with respect to a commercially available silica-based C18 SPE adsorbent, and it was found that CH possessed comparable (~50%) extraction, as well as regeneration capacity (~95%). The developed biosorbent was applied in a wastewater sample spiked with the target analyte and recovery studies were performed, which found a range of 93.0 to 102.0% with a %RSD of 3.72 to 12.7%. Thus, CH can be exploited as a 'greener' replacement for the commercially available adsorbents for the extraction/retention of active pharmaceutical ingredients present in water/wastewater samples. [ABSTRACT FROM AUTHOR]

In this work, a metal–organic framework (MOF), copper benzene dicarboxylate (Cu-MOF), was tested for the adsorptive recovery of organic dyes (Sunset Yellow FCF, Tartrazine, Orange II, and Methyl Orange) from aqueous solutions. Studies were also carried out to determine the effects of various parameters, and isothermal and kinetic models were proposed. The adsorption capacity of Cu-MOF was much higher than that of activated carbon. The experimental data are best described by the Langmuir isotherm model (R2 > 0.997) and show the ability of Cu-MOF to adsorb 435 mg/g of the dye under optimal conditions. The study of the kinetics of the dye adsorption process followed a pseudo-second-order kinetic model indicating the coexistence of physical and chemisorption, with diffusion within the particles being the rate-limiting step. Thermodynamic studies were also carried out, and they led to the conclusion that the adsorption of the dye was a feasible, spontaneous, and exothermic process (−25.53 kJ mol−1). The high organic dye recovery shows that Cu-MOF can be used as an efficient and reusable adsorbent for the extraction of dyes from aqueous solutions. These studies may lead to economic interest in this adsorbent material for environmental purposes. [ABSTRACT FROM AUTHOR]

Lupin alkaloids (LAs) represent a class of toxic secondary metabolites in plants, in particular in Lupinus spp.; they are produced as a defense mechanism due to their strong bitter taste and are very dangerous for human and animals. In this work, a sensitive and reliable high performance liquid chromatography—tandem mass spectrometry (HPLC-MS/MS) analytical method for the identification and quantification of thirteen lupin alkaloids was developed and validated according to FDA guidelines. Efficient extraction and clean-up steps, carried out by solid-phase extraction, were finely tuned on the basis of the characteristics of the analytes and lupin samples, providing good selectivity with minimized matrix interference. The effectiveness of the method was proven by the satisfactory recovery values obtained for most of the analytes and a matrix effect ≤23% for all tested levels. In addition, a sensitive and reliable determination of the target compounds was obtained; LOQs were between 1 and 25 µg Kg−1, i.e., below the requested maximum levels (<200 mg Kg−1). The method was applied to evaluate the LAs profile in different batches of raw L. albus L. samples, varying in size and across farming treatments. [ABSTRACT FROM AUTHOR]

The synthesis of an organofunctionalized mesoporous silica was accomplished by a two-step process involving (1) the co-condensation of a silylant agent at the surface of silica, followed by (2) the immobilization of Purpald (ligand) at the organic termination of the silytant agent. The characterization of the organofunctionalized material indicated the presence of NH2 groups, and the immobilization of the ligand was confirmed by 29Si- and 13C-nuclear magnetic resonance. The material's surface area was determined as 370 m2 g−1. Batch adsorption experiments enabled the determination of optimum pH conditions for the adsorption of Cu(II) and Cd(II). Under optimal pH, the pseudo-second-order kinetic model and Langmuir model provided the best correlations to describe the materials adsorption behavior, suggesting a chemisorption mechanism. When tested in continuous-flow preconcentration experiments, the flow rate and eluent concentration demonstrated to affect the removal of Cu(II) and Cd(II), while the buffer concentration had an effect only over the adsorption of Cu(II). Under optimized preconcentration conditions, it was possible both to determine the concentrations of Cu(II) and Cd(II) in samples such as mineral water, ground water, tap water and river water. Ions commonly found in drinking and natural waters (Na+, K+, Ca2+, Mg2+, Fe3+, Ba2+, Cl−, SO42−, HCO3−, and H2PO4−) did not affect the preconcentration of any of the studied analytes. Reutilization experiments indicated that the adsorbent material can withstand at least 40 adsorption/desorption preconcentration cycles with no efficiency loss. [ABSTRACT FROM AUTHOR]

In this work we investigated the synthesis and the characterization of electrospun polyacrylonitrile (PAN) and polymethyl methacrylate (PMMA) stabilized in air, made in a 5:1 ratio, used as sorbent for the solid-phase extraction of fluoroquinolones in plasma samples and the following quantification in UHPLC-PDA. Preliminary analyses of viscosity were carried out on the polymer solution to be sure about the electrospinability. Characterizations were performed on the electrospun membrane to evaluate the morphology (SEM scanning electron microscopy and AFM atomic force microscopy), the thermal degradation behavior (TGA thermogravimetric analysis), the porosity and the surface area (BET, Brunauer Emmett Teller), and the quantitative and qualitative distribution of atomic structures (FTIR infrared analysis in Fourier transform and EDX Energy Dispersive X-ray analysis). A solid-phase extraction method was developed by studying parameters such as the amount of sorbent and the pH of the sample. Finally, a UHPLC-PDA method for the analysis of fluoroquinolones was developed and validated in accordance with the guidelines and successfully applied. The use of the prepared sorbent combined with UHPLC-PDA has allowed the development of a method whose strengths are its speed, accuracy, sensitivity, and high recoveries. [ABSTRACT FROM AUTHOR]

In this work, a rapid, precise, and cost-valuable method has been established to quantify phenolic compounds in olive oil using new-based hydrophilic interaction solid-phase extraction (SPE). Boehlert's experimental design applied the determination of the optimal operating conditions. An investigation into the effects of the methanol composition (50–100%), the volume of eluent (1–12 mL), and pH (1–3) on the extraction of phenols acids and total phenols from Tunisian olive oils was performed. The results showed that the extraction conditions had a significant effect on the extraction efficiency. The experiment showed that the greatest conditions for the SPE of phenolic acids were the methanol composition at 90.3%, pH at 2.9, and volume at 7.5 mL, respectively. The optimal conditions were applied to different types of olive oils, and it could be concluded that larger concentrations of polyphenols were found in extra virgin olive oil (89.15–218), whereas the lowest levels of these compounds (66.8 and 5.1) were found in cold-pressed crude olive oil and olive pomace oil, respectively. [ABSTRACT FROM AUTHOR]

A rapid and sensitive high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS) method was developed for the quantification of Paclitaxel (PTX), 6α-hydroxypaclitaxel (6α-OHP), and p-3′-hydroxypaclitaxel (3′-OHP) in mouse plasma and tumor tissue. The analytes were separated using a C18 column (50 × 2.1 mm, 1.8 μm), and a triple-quadrupole mass spectrometry device equipped with an electrospray ionization (ESI) source was applied for their detection. PTX, 6α-OHP, and 3′-OHP were extracted from the biological samples with the solid-phase extraction cartridge. The method was fully validated according to the FDA's guidance. The method was linear over the concentration ranges of 0.5~1000.0 ng/mL for PTX and 0.25~500.0 ng/mL for 6α-OHP and 3′-OHP. The precision, accuracy, extraction recovery, and matrix effects were within acceptable limits. The present method was successfully applied to the study of the pharmacokinetics and distribution of PTX, 6α-OHP, and 3′-OHP in the tumors of post xenograft nude mice intravenously injected with PTX solution. [ABSTRACT FROM AUTHOR]

Kappa-casein-derived caseinomacropeptide (CMP)—a 64-amino-acid peptide—is released from kappa-casein after rennet treatment and is one of the major peptides in whey protein isolate (WPI). CMP has anti-inflammatory and antibacterial activities. It also has two major amino acid sequences with different modifications, including glycosylation, phosphorylation, and oxidation. To understand the potential biological role of CMP within the human body, there is a need to examine the extent to which CMP and CMP-derived fragments survive across the digestive tract, where they can exert these functions. In this study, three solid-phase extraction (SPE) methods—porous graphitized carbon (PGC), hydrophilic interaction liquid chromatography (HILIC), and C18 chromatography—were evaluated to determine which SPE sorbent is the most efficient to extract intact CMP and CMP-derived peptides from WPI and intestinal digestive samples prior to LC-MS/MS acquisition. The C18 SPE sorbent was the most efficient in extracting intact CMP and CMP-derived peptides from WPI, whereas the PGC SPE sorbent was the most efficient in extracting CMP-derived peptides from intestinal digesta samples. [ABSTRACT FROM AUTHOR]

Glutathione S-transferases (GSTs) are important type-II detoxification enzymes that protect DNA and proteins from damage and are often used as protein tags for the expression of fusion proteins. In the present work, octa-aminopropyl caged polyhedral oligomeric silsesquioxane (OA–POSS) was prepared via acid-catalyzed hydrolysis of 3-aminopropyltriethoxysilane and polymerized on the surface of graphene oxide (GO) through an amidation reaction. Glutathione (GSH) was then modified to GO–POSS through a Michael addition reaction to obtain a GSH-functionalized GO–POSS composite (GPG). The structure and characteristics of the as-prepared GPG composite were characterized using scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), thermogravity analysis, and surface charge analysis. The specific binding interactions between glutathione and GST gave GPG favorable adsorption selectivity towards GST, and other proteins did not affect GST adsorption. The adsorption behavior of GST on the GPG composite conformed to the Langmuir isotherm model, and the adsorption capacity of GST was high up to 364.94 mg g−1 under optimal conditions. The GPG-based solid-phase adsorption process was applied to the extraction of GST from a crude enzyme solution of pig liver, and high-purity GST was obtained via SDS-PAGE identification. [ABSTRACT FROM AUTHOR]

The abuse and residues of antibiotics have a great impact on the environment and organisms, and their determination has become very important. Due to their low contents, varieties and complex matrices, effective recognition, separation and enrichment are usually required prior to determination. Molecularly imprinted polymers (MIPs), a kind of highly selective polymer prepared via molecular imprinting technology (MIT), are used widely in the analytical detection of antibiotics, as adsorbents of solid-phase extraction (SPE) and as recognition elements of sensors. Herein, recent advances in MIPs for antibiotic residue analysis are reviewed. Firstly, several new preparation techniques of MIPs for detecting antibiotics are briefly introduced, including surface imprinting, nanoimprinting, living/controlled radical polymerization, and multi-template imprinting, multi-functional monomer imprinting and dummy template imprinting. Secondly, several SPE modes based on MIPs are summarized, namely packed SPE, magnetic SPE, dispersive SPE, matrix solid-phase dispersive extraction, solid-phase microextraction, stir-bar sorptive extraction and pipette-tip SPE. Thirdly, the basic principles of MIP-based sensors and three sensing modes, including electrochemical sensing, optical sensing and mass sensing, are also outlined. Fourthly, the research progress on molecularly imprinted SPEs (MISPEs) and MIP-based electrochemical/optical/mass sensors for the detection of various antibiotic residues in environmental and food samples since 2018 are comprehensively reviewed, including sulfonamides, quinolones, β-lactams and so on. Finally, the preparation and application prospects of MIPs for detecting antibiotics are outlined. [ABSTRACT FROM AUTHOR]

Cell surface proteins, including transmembrane and other surface-anchored proteins, play a key role in several critical cellular processes and have a strong diagnostic value. The development of quick and robust experimental methods remains vital for the accurate and comprehensive characterization of the cell surface subproteome of individual cells. Here we present a high-throughput technique which relies on the biotinylation of the accessible primary amino groups in the extracellular segments of the proteins, using HL60 as a model cell line. Several steps of the method have been thoroughly optimized to capture labeled surface proteins selectively and in larger quantities. These include the following: improving the efficiency of the cell surface biotinylation; reducing the endogen protease activity; applying an optimal amount of affinity column and elution steps for labeled peptide enrichment; and examining the effect of various solid-phase extraction methods, different HPLC gradients, and various tandem mass spectrometry settings. Using the optimized workflow, we identified at least 1700 surface-associated individual labeled peptides (~6000–7000 redundant peptides) from the model cell surface in a single nanoHPLC-MS/MS run. The presented method can provide a comprehensive and specific list of the cell surface available protein segments that could be potential targets in various bioinformatics and molecular biology research. [ABSTRACT FROM AUTHOR]

Polyaniline (PANI) is one of the best known and widely studied conducting polymers with multiple applications and unique physicochemical properties. Due to its porous structure and relatively high surface area as well as the affinity toward many analytes related to the ability to establish different types of interactions, PANI has a great potential as a sorbent in sample pretreatment before instrumental analyses. This study provides an overview of the applications of polyaniline and polyaniline composites as sorbents in sample preparation techniques based on solid-phase extraction, including conventional solid-phase extraction (SPE) and its modifications, solid-phase microextraction (SPME), dispersive solid-phase extraction (dSPE), magnetic solid-phase extraction (MSPE) and stir-bar sorptive extraction (SBSE). The utility of PANI-based sorbents in chromatography was also summarized. It has been shown that polyaniline is willingly combined with other components and PANI-based materials may be formed in a variety of shapes. Polyaniline alone and PANI-based composites were successfully applied for sample preparation before determination of various analytes, both metal ions and organic compounds, in different matrices such as environmental samples, food, human plasma, urine, and blood. [ABSTRACT FROM AUTHOR]

Organophosphate triesters are compounds widely used in industries and are ubiquitous in the environment, where they can be transformed into organophosphate diesters. Some organophosphate diesters are also used by industry. Several studies suggest organophosphate diesters can have toxic effects for reproduction, and hazardous and mutagenic properties. Due to the impact these compounds can have on marine biota and human beings through the consumption of fish and shellfish, it is necessary to study their presence in widely consumed seafood species. We therefore developed an analytical method for determining six of the most common organophosphate diesters in seafood. The procedure is based on the Quick, Easy, Cheap, Effective, Rugged and Safe extraction method and a solid phase extraction clean-up, followed by liquid chromatography coupled to high-resolution mass spectrometry. The method was optimised and validated for seafood with different lipid content, providing satisfactory relative recoveries (from 89 to 138%) and limits of detection (1.0–50 ng g−1 dry weight), as well as repeatability values (RSD% (n = 5, 100 ng g−1 (dry weight)) lower than 15%. Eight seafood species were analysed using this method and two organophosphate diesters were detected and quantified in all the samples, demonstrating the suitability of the method. [ABSTRACT FROM AUTHOR]

Pesticides are widely used on tea plants, and pesticide residues are of significant concern to consumers. The National Food Safety Standard Maximum Residue Limits for Pesticides in Food (GB 2763-2021) was recently amended. However, detection methods for pesticides newly added to the list of residues in beverages have not yet been established. For that reason, this study developed a solid-phase extraction (SPE) and gas chromatography–tandem mass spectrometry (GC–MS/MS) method for determining the residues of 12 pesticides, including four newly added, in black and green tea. Sample preparation processes (sample extraction, SPE clean-up, elution solvent, and elution volume) were optimized to monitor these residues reliably. Multiple reaction monitoring (MRM) was used for GC–MS/MS electron impact (EI) mode determination. Finally, satisfactory recoveries (70.7–113.0% for green tea and 72.0–99.1% for black tea) were achieved at three concentrations (10 μg/kg, 20 μg/kg, and 100 μg/kg). The LOQs were 0.04–8.69 μg/kg, and the LODs were 0.01–3.14 μg/kg. This study provides a reliable and sensitive workflow for determining 12 pesticide residues in tea, filling a gap in the newly revised National Standards. [ABSTRACT FROM AUTHOR]

Currently, among the various areas of targeted wastewater treatment, great attention is being given by researchers to the solid-phase extraction of organic dyes using metal–organic frameworks (MOFs). In this work, a mixed-ligand Zr-MOF containing terephthalic acid and 1,10-phenanthroline as linkers was used for this purpose. The limiting adsorption of the dyes Congo red and methylene blue, according to experimental data, is 40 mg/g. The influence of various parameters (time, temperature, adsorbent dosage, pH, and coexisting ions) on adsorption characteristics was studied. The sorbent was tested for the removal of dyes from drinks in water and in artificial seawater. The possibility of the separation of dyes by column chromatography using a sorbent as a filler was studied. [ABSTRACT FROM AUTHOR]

The consumption of plant-based beverages as an alternative to cow's milk has recently gained vast attention worldwide. The aim of this work is to monitor the intake of Bisphenol A (BPA), Bisphenol B (BPB) and Bisphenol S (BPS) in the Italian population through the consumption of these foodstuffs. Specifically, the development and validation of an analytical procedure for the quantitative determination of the analytes by liquid chromatography coupled to tandem mass spectrometry was reported. Thirty-four samples of plant-based beverages (soya, coconut, almond, oats and rice) of popular brands marketed in Italy were analyzed. BPA was found in 32% of the samples, while BPB was found in 3% of the samples. The risk assessment using the Rapid Assessment of Contaminant Exposure (RACE) tool demonstrated that there was no risk for all population groups, when using the current Tolerable Daily Intake (TDI) of 4 ng/kg body weight (bw)/day as a toxicological reference point. In contrast, using the new temporary TDI of 0.04 ng/kg bw/day, the existing risk was found to be real for all population groups. If this value were to become final, even more attention would have to be paid to the possible presence of BPA in food to protect consumer health. [ABSTRACT FROM AUTHOR]

A novel HPLC-ESI-MS/MS method for simultaneous gonadotropin-releasing hormone (GnRH) analogs and somatostatin analog quantitation was developed and validated. The developed method was successfully applied to pharmacokinetic studies. The sample preparation process included solid-phase extraction (SPE). Effective chromatographic separation of the analytes and internal standard (dalargin) was achieved with a C18 column, using a gradient elution with two mobile phases: 0.1% v/v formic acid (aqueous solution) and 0.1% v/v formic acid (acetonitrile solution). The linearity of the method was demonstrated within a concentration range of 0.5–20 ng/mL, with correlation coefficients between 0.998–0.999 for goserelin, buserelin, triptorelin, and octreotide, respectively. The relative standard deviation (RSD, %) values for method accuracy and precision did not exceed 20% at the lower level of quantitation (LLOQ) or 15% at other concentration levels. [ABSTRACT FROM AUTHOR]

In this study, a sensitive capillary electrophoresis (CE) method based on molecularly imprinted solid-phase extraction (MISPE) was proposed to determine histamine in foods. A molecularly imprinted polymer (MIP) synthesized by bulk polymerization was used as the MISPE adsorbent for the selective extraction of histamine. Under the optimal conditions, the MISPE-CE method possessed good linearity for histamine detection in the concentration range of 0.1–100.0 μg/L. The limit of detection and limit of quantification of the method were calculated to be 0.087 μg/L and 0.29 μg/L, respectively. The histamine in spiked rice vinegar and liquor samples were detected by the developed method with recoveries of 92.63–111.00%. The histamine contents in fish, prawn, pork, chicken breast and soy sauce samples were determined using the developed method and a high-performance liquid chromatography method, with no significant difference found between the two methods. [ABSTRACT FROM AUTHOR]

99Mo/99mTc generators are mainly produced from 99Mo of high specific activity generated from the fission of 235U. Such a method raises proliferation concerns. Alternative methods suggested the use of low specific activity (LSA) 99Mo to produce 99mTc generators. However, its applicability is limited due to the low adsorptive capacity of conventional adsorbent materials. This study attempts to investigate the effectiveness of some commercial metal oxides nanoparticles as adsorbents for LSA 99Mo. In a batch equilibration system, we studied the influence of solution pH (from 1–8), contact time, initial Mo concentration (from 50–500 mg∙L−1), and temperature (from 298–333 K). Moreover, equilibrium isotherms and thermodynamic parameters (changes in free energy ΔG0, enthalpy change ΔH0, and entropy ΔS0) were evaluated. The results showed that the optimum pH of adsorption ranges between 2 and 4, and that the equilibrium was attained within the first two minutes. In addition, the adsorption data fit well with the Freundlich isotherm model. The thermodynamic parameters prove that the adsorption of molybdate ions is spontaneous. Furthermore, some investigated adsorbents showed maximum adsorption capacity ranging from 40 ± 2 to 73 ± 1 mg Mo∙g−1. Therefore, this work demonstrates that the materials used exhibit rapid adsorption reactions with LSA 99Mo and higher capacity than conventional alumina (2–20 mg Mo∙g−1). [ABSTRACT FROM AUTHOR]

Ion-imprinted polymers (IIPs) have been widely used in different fields of Analytical Sciences due to their intrinsic selective properties. However, the success of chemical imprinting in terms of selectivity, as well as the stability, specific surface area, and absence of swelling effect depends on fully understanding the preparation process. Therefore, the proposal of this review is to describe the influence of relevant parameters on the production processes of ion-imprinted polymers, including the nature (organic, inorganic, or hybrid materials), structure, properties of the salt (source of the metal ion), ligand, crosslinking agent, porogenic solvent, and initiator. Additionally, different polymerization methods are discussed, the classification of IIPs as well as the applications of these adsorbent materials in the last years (2017–2022). [ABSTRACT FROM AUTHOR]

The optimization of solid-phase extraction (SPE) purification and chromatographic separation is usually neglected during proteomics studies. However, the effects on detection performance are not negligible, especially when working with highly glycosylated samples. We performed a comparative study of different SPE setups, including an in-house optimized method and reversed-phase chromatographic gradients for the analysis of highly glycosylated plasma fractions as a model sample for glycopeptide analysis. The in-house-developed SPE method outperformed the graphite-based and hydrophilic interaction liquid chromatography (HILIC) purification methods in detection performance, recovery, and repeatability. During optimization of the chromatography, peak distribution was maximized to increase the peptide detection rate. As a result, we present sample purification and chromatographic separation methods optimized for the analysis of hydrophilic samples, the most important of which is heavily N-glycosylated protein mixtures. [ABSTRACT FROM AUTHOR]