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Antibiotic contamination in polluted rivers is well recognized as an environmental and public health challenge. In this study, the occurrence, distribution, and ecological risk assessment of three commonly used antibiotics (amoxicillin, ciprofloxacin, and azithromycin) were assessed in the Litani River, the most important and highly polluted river in Lebanon. Physicochemical and microbiological water quality parameters including the antibiotic-resistant ones were in parallel determined in the same sites. Water samples from five sites stretching across the river upper basin were analyzed for the antibiotics under study using high-performance liquid chromatography, with both fluorometric and UV detectors post-extraction using a solid-phase method with a hydrophilic-lipophilic balance cartridges. The disc diffusion method and standardized water quality methods were used for antibiotic-resistant bacteria and water quality assessment, respectively. Amoxicillin and ciprofloxacin were found at concentrations of 250 ng/L and 107.2 ng/L, while azithromycin was not detected in any of the sites under study. Varying levels of antibiotic resistance were detected with the isolated Escherichia coli (E. coli) and Pseudomonas aeruginosa (P. aeruginosa) while the total coliforms showed resistance to multiple antibiotics. COD, TP, PO43-, TN, NO3-, NH4 + , E. coli, total coliform, P. aeruginosa, and Cd levels surpassed permissible levels. Correlation analysis with water quality parameters (COD, total phosphate, phosphate, total nitrogen, and cadmium) showed a significant positive correlation with ciprofloxacin (r > 0.5, p value < 0.05). Also, the resistant P. aeruginosa showed a significant positive correlation with cadmium (r > 0.5, p value < 0.05) while the resistant E. coli was positively correlated with total nitrogen, nitrate, and lead levels (r > 0.5, p value < 0.05). The ecological risk assessment revealed that all the tested antibiotics pose low risks (ecological risk quotient RQ < 0.1) except ciprofloxacin, which could pose a medium risk (0.1 < RQ < 1). Future research concerning the long-term assessment of antibiotics' residues and the identification of resistance genes in the river is recommended. [ABSTRACT FROM AUTHOR]

Introduction: 2,5-diketopiperazines are the simplest forms of cyclic dipeptides (CDPs) and have diverse frameworks with chiral side chains that are useful for drug development. Previous research has investigated the antimicrobial properties of proline-linked CDPs and their combinations in the culture filtrate (CF) of Lactobacillus plantarum LBP-K10 using anion exchange chromatography (AEC). However, the quantity of CDPs showcasing notable anti-influenza virus activity derived from AECs was generally lower than those originating from Lactobacillus CF.Methods: To address this issue, the study aims to propose a more efficient method for isolating CDPs and to introduce the antiviral combinations of CDPs obtained using a new method. The study employed a novel technique entailing high-throughput C18-based solid-phase extraction with a methanol gradient (MeSPE). The MeSPE method involved increasing the methanol concentration from 5% to 50% in 5% increments.Results: The methanol SPE fractions (MeSPEfs) eluted with methanol concentrations between 35% and 45% evinced substantial efficacy in inhibiting the influenza A/H3N2 virus via plaque-forming assay. MeSPEf-45, the 45% MeSPEf, exhibited exceptional efficacy in preventing viral infections in Madin-Darby kidney cells, surpassing both individual CDPs and the entire set of MeSPEfs. To identify the specific antiviral components of MeSPEf-45, all MeSPEfs were further fractionated through preparative high-performance liquid chromatography (prep-HPLC). MeSPEf-45 fractions S8 and S11 presented the highest activity against multidrug-resistant bacteria and influenza A/H3N2 virus among all MeSPEfs, with 11 common fractions. Antiviral fractions S8 and S11 were identified as proline-based CDPs, specifically cis-cyclo(L-Leu-L-Pro) and cis-cyclo(L-Phe-L-Pro), using gas chromatography-mass spectrometry. The combination of MeSPEf-45 fractions S8 and S11 displayed superior antibacterial and anti-influenza virus effects compared to the individual fractions S8 and S11.Discussion: High-throughput MeSPE-derived MeSPEfs and subsequent HPLC-fractionated fractions presents an innovative approach to selectively purify large amounts of potent antimicrobial CDPs from bacterial CF. The findings also show the effectiveness of physiologically bioactive combinations that utilize fractions not containing CDP. This study provides the initial evidence demonstrating the antimicrobial properties of CDPs acquired through high-throughput SPE techniques.

Abstract Dissolved organic carbon (DOC) in the global oceans is an important long‐term carbon sink. Connections between molecular size, reactivity, and isotopic characteristics show that DOC exists on a continuum from biologically reactive to recalcitrant. The driving mechanisms behind the creation and persistence of recalcitrant DOC remain unknown. We show mean recalcitrant DOC (isolated via solid‐phase extraction; SPE‐DOC) δ13C values are 1.3 ± 0.6‰ lower than mean total DOC δ13C between depth ranges 0–200 m and 2–4 km on three GO‐SHIP Repeat Hydrography cruises. Lowest observed δ13C values correlate with low ∆14C and proximity to deep ocean hydrothermal systems. These data support the hypothesis that reworking of DOC through the microbial carbon pump is a key driver of the ocean's long‐term carbon sink. Mass‐balance modeling shows deep‐ocean DOC not captured by SPE is enriched in 13C, highlighting the need for continued research on non‐retained DOC to predict mechanisms that drive ocean carbon storage.

Solid-phase extraction (SPE) coupled with capillary electrophoresis (CE) for the determination of macrolide antibiotics (azithromycin, clarithromycin, roxithromycin, tylosin) and tiamulin in water samples was described in this article. These compounds were extracted with different types of sorbents ( Oasis HLB, C18, C8, SDB, and Strata-X) and different masses of sorbents (60 mg, 200 mg, and 500 mg) using different organic solvents (methanol, ethanol, and acetonitrile) and different pH values of water samples (pH 7.00, 8.00, and 9.00). It was found that the highest extraction efficiency of the studied compounds was obtained with 200 mg/3 mL C18 cartridges with methanol as eluent at pH 9.00 of the water sample. The developed SPE-CE method for macrolide antibiotics and tiamulin was validated for linearity, precision, repeatability, the limit of detection (LOD), the limit of quantification (LOQ), and recovery. Good linearity was obtained in the range of 0.3–30 mg L−1 depending on the drug, with correlation coefficients higher than 0.9958 in all cases except clarithromycin (0.9873). Expanded measurement uncertainties were calculated for each pharmaceutical, accounting for 20.31 % (azithromycin), 38.33 % (tiamulin), 28.95 % (clarithromycin), 26.99 % (roxithromycin), and 21.09 % (tiamulin). Uncertainties associated with precision and calibration curves contributed the most to the combined measurement uncertainty. The method was successfully applied to the analysis of production waste-water from the pharmaceutical industry.

In recent decades, micro-pollutants like estrogen hormones have been considered due to adverse health effects on humans and the environment despite very low concentrations of 0.1–20 ng/L. In the present study, drinking water was sampled from the six areas of Tehran in summer (August 2020), autumn (November 2020), winter (February 2021), and spring (May 2021) to evaluate natural and synthetic estrogen hormones (estrone (E1), 17-beta-estradiol (E2), estriol (E3), and 17-alpha-ethinyl estradiol (EE2)). The samples were transferred to the laboratory and the solid-phase extraction (SPE) method was used to extract the hormones, and the type and amount of hormones were examined by gas chromatography–mass spectrometry. According to the results, the highest concentrations were related to E1 and E2 compounds at 1.96 and 2.13 ng/L, respectively, in summer and autumn (device detection limit = 0.5 ng/L). In addition, concentrations of compounds E1 and E2 were lower than the detection limit in spring and winter in all samples, and compounds E3 and EE2 were not identified in any samples or seasons. Commonly, the concentration of steroid hormones increased in the dry seasons (summer and autumn), while in the spring and winter concentrations were less than the device detection limit because of rainfall. HIGHLIGHTS Endocrine-disrupting hormones were evaluated in the drinking water of Tehran city; E1 and E2 were detected only in summer and autumn.; E1 and E2 were not detected in spring and winter.; E3 and EE2 were not detected in any region or any season.;

Abstract Background In-hospital therapeutic drug monitoring (TDM) requires a suitable quantification method for target drugs from the viewpoint of precision, throughput, and testing costs. We previously developed a practical HPLC-UV platform for quantification of serum levels of various drugs. In this report, the platform was effectively applied to the quantification of patient serum levels of five different drugs by clinical professionals in our hospital during their daily work. Methods The residual sera of patients receiving carbamazepine (CBZ), phenytoin (PHT), lamotrigine (LTG), vancomycin (VCM), or voriconazole (VRCZ) were used in the present clinical study. The quantification method for each drug consisted of rapid solid-phase extraction (SPE) of each drug in the patient serum, followed by optimized HPLC-UV analysis of the drug in the SPE eluate. Furthermore, patient serum levels of PHT, CBZ, and VCM were also measured by ligand-binding assay using a cobas® analyzer in our hospital, and those of LTG and VRCZ were measured by HPLC-MS/MS at an outsourced provider. Passing–Bablok regression analysis and Bland–Altman analysis were employed to analyze the agreement of drug levels in patient sera, which was separately quantified using two different methods—our HPLC-UV platform and the cobas analyzer, or HPLC-UV and HPLC-MS/MS. Results All analytical conditions of the present method using our HPLC-UV platform were well optimized for each target drug quantification in the patient’s serum, and the quantification method for each drug was fully validated for accuracy, precision and reproducibility. Furthermore, Passing–Bablok regression analysis and Bland–Altman analysis revealed that patient serum levels of PHT, CBZ, and VCM quantified by our HPLC-UV platform were closely correlated with those quantified by the cobas® analyzer, and the levels of LTG and VRCZ quantified by our HPLC-UV platform were also correlated with those quantified by HPLC-MS/MS. Conclusions Our HPLC-UV platform can be performed without requiring special analytical techniques. This platform is expected to be used for the measurement of blood levels of multiple drugs for in-hospital routine TDM.

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.

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.

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.

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.

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%).

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.

为清除合成乳化剂硬脂酰乳酸钠（SSL）对铜皂络合比色技术测定油脂酸价过程的正向干扰，开发了一种固相萃取（SPE）清除SSL的技术。用含2%异丙醇的环己烷为固相萃取流动相和油脂样品溶解液，通过离子排斥色谱检测油脂皂化水解后释放的游离乳酸的含量，间接评估SPE净化处理前后油脂中的SSL含量,并结合铜皂络合比色技术测定的酸价变化，评价所建立的SPE技术对去除油脂中SSL的效果。结果表明：SPE技术可有效去除油脂中的SSL，明显消除油脂中SSL对铜皂络合比色法测定酸价的干扰，不会导致油脂样品脂肪酸含量损失。对于含SSL的食用油脂试样，经SPE技术净化处理后，铜皂络合比色法测定酸价过程的干扰明显降低。To eliminate the positive interference of synthetic emulsifier sodium stearyl lactate (SSL) in the determination of acid value by cupric-pyridine colorimetric method,a solid-phase extraction (SPE) technique for cleaning SSL was developed. Using cyclohexane containing 2% isopropyl alcohol as mobile phase of SPE and oil sample solution, the content of SSL in oils before and after SPE was indirectly evaluated by detecting the content of free lactic acid released after saponification and hydrolysis of oils by ion exclusion chromatography. The effect of the established SPE technique on the removal of SSL from oils was evaluated by combining the acid value change measured by cupric-pyridine colorimetric method.The results showed that the SPE method could effectively remove SSL from oil, and obviously eliminate the interference of SSL on the determination of acid value by cupric-pyridine colorimetric method, without causing the loss of fatty acid content in oil samples.After purification by SPE, the interference of the acid value determination by cupric-pyridine colorimetric method is significantly reduced for the samples containing SSL edible oils.

Heavy metals' contamination of water resources is a global environmental issue due to their detrimental effects on human health. To safeguard humans and the environment, toxic heavy metals must be removed from contaminated water because they cannot be broken down. Diverse technologies are employed to reduce the levels of heavy metals in wastewater. However, these technologies suffer from being either costly or ineffective, particularly when the effluent has extremely low residual amounts. This review outlines the main accomplishments and promising future directions for solvent extraction as one of the potential methods of extracting heavy metals from water, utilizing literature reports. In addition to reviewing some of the commercial chelating reagents now in use, this article also discusses some of the obnoxious effects on human health that are associated with exposure to heavy metals. HIGHLIGHTS Water pollution by heavy metals is a global issue.; Some heavy metals are toxic to plants and human life.; Chelation extraction of heavy metals is a potential technology for remediation of heavy-metal polluted water.; Chelation extraction is potentially more efficient and selective.; With respect to green chemistry principles such as solvent-free technique, functionalization of mesoporous silica is a promising alternative.;

Objective Cow urine possesses several bioactive properties but the responsible components behind these bioactivities are still far from identified. In our study, we tried to identify the possible components behind the antimicrobial activity of cow urine by exploring the peptidome and metabolome. Methods We extracted peptides from the urine of Sahiwal cows belonging to three different physiological states viz heifer, lactation, and pregnant, each group consisting of 10 different animals. The peptides were extracted using the solid phase extraction technique followed by further extraction using ethyl acetate. The antimicrobial activity of the aqueous extract was evaluated against different pathogenic strains like Staphylococcus aureus, Escherichia coli, and Streptococcus agalactiae. The safety of urinary aqueous extract was evaluated by hemolysis and cytotoxicity assay on the BuMEC cell line. The urinary peptides were further fractionated using high-performance liquid chromatography (HPLC) to identify the fraction(s) containing the antimicrobial activity. The HPLC fractions and ethyl acetate extract were analyzed using nLC-MS/MS for the identification of the peptides and metabolites. Results A total of three fractions were identified with antimicrobial activity, and nLC-MS/MS analysis of fractions resulted in the identification of 511 sequences. While 46 compounds were identified in the metabolite profiling of organic extract. The urinary aqueous extract showed significant activity against E. coli as compared to S. aureus and S. agalactiae and was relatively safe against mammalian cells. Conclusion The antimicrobial activity of cow urine is a consequence of the feeding habit. The metabolites of plant origin with several bioactivities are eliminated through urine and are responsible for their antimicrobial nature. Secondly, the plethora of peptides generated from the activity of endogenous proteases on protein shed from different parts of tissues also find their way to urine. Some of these sequences possess antimicrobial activity due to their amino acid composition.

Quantitative information on blood metabolites can be used in developing advanced medical strategies such as early detection and prevention of disease. Monitoring bioactive lipids such as steroids, bile acids, and PUFA metabolites could be a valuable indicator of health status. However, a method for simultaneously measuring these bioactive lipids has not yet been developed. Here, we report a LC/MS/MS method that can simultaneously measure 144 bioactive lipids, including steroids, bile acids, and PUFA metabolites, from human plasma, and a sample preparation method for these targets. Protein removal by methanol precipitation and purification of bioactive lipids by solid-phase extraction improved the recovery of the targeted compounds in human plasma samples, demonstrating the importance of sample preparation methods for a wide range of bioactive lipid analyses. Using the developed method, we studied the plasma from healthy human volunteers and confirmed the presence of bioactive lipid molecules associated with sex differences and circadian rhythms. The developed method of bioactive lipid analysis can be applied to health monitoring and disease biomarker discovery in precision medicine.

AbstractGastrodia elata is a well-known Asian traditional herb with gastrodin (GAS; p-hydroxymethylbenzene-β-d-glucopyranoside) as its active ingredient. It is a challenging task to efficiently separate the active ingredient gastrodin from Gastrodia elata by simple procedure. The results of computer molecular simulation & UV-vis spectroscopy showed that water-soluble 1-vinyl-3-tetradecylimidazole bromide([C14VIM+] [Br-]) was selected as the best ionic liquid functional monomer compared with methacrylic acid(MAA), acrylic acid(AA), 3-(2-carboxyethyl)-1-vinylimidazolium bromide ionic liquid (imidazole propionate, [COOHpvimBr]), and dehydroabietic acid [2-(acryloyloxy)ethyl] ester (DAAEE). The force between [C14VIM+] [Br-] and GAS (with multiple hydroxyl groups) is stronger than other monomers with more polar groups. The molecular imprinted polymers (MIPs) and non- molecular imprinted polymers (NIPs) with high selectivity to gastrodin were synthesized utilizing ([C14VIM+] [Br-]) as a novel functional monomer. The polymer was characterized by infrared spectrum, scanning electron microscope, specific surface area tester and thermosgravimetric analyser(TGA). The adsorption performance of the polymer was investigated by adsorption kinetics experiment and static adsorption experiment. Among different eluents, the content of gastrodin in eluent (70% ethanol) significantly increased compared with it in plant extract by the MIPs-solid phase extraction (SPE)-HPLC. The recoveries of the spiked samples for the GAS were 97.75–103.43%, with relative standard deviation values lower than 2.88%. This novel [C14VIM+] [Br-]-based MIP was a potential separation material for gastrodin. The graphical abstract was shown below. [ABSTRACT FROM AUTHOR]

In this work, is proposed an analytical method for the determination of nickel in natural water and sediment samples using solid-phase extraction with a mini-column of bamboo fibres modified with 5-Br-PADAP and determination by flame atomic absorption spectrometry. Applying the characterisation techniques of fresh bamboo fibre aimed to define the morphology of the fibre and its physical characteristics. Turning to the optimisation of the variables for the adsorptive process of nickel. The system allows the determination of nickel with a limit of detection (LOD) of 0.75 μg L−1 and a limit of quantitation (LOQ) of 2.50 μg L−1. The precision was expressed as a relative standard deviation (RSD) of 3.4 and 3.8% for a nickel concentration of 20.0 and 50.0 μg L−1 respectively. The value of 78.0 was determined as the value for the enrichment factor. The accuracy was confirmed with spike tests with recuperations varying from 91% to 106% and 93% to 104% for water and sediment samples, respectively, and by comparison with the certified sample. The procedure was applied for nickel determination in natural water and sediment samples. The achieved concentrations varied from 4.0–53.2 and 3.7–55.8 µg L−1 for water and sediment samples, respectively. [ABSTRACT FROM AUTHOR]

AbstractIn this work, sulfide-modified magnetic titanium dioxide microparticles (magnetic TiO2-µPs@S) were synthesized and studied for adsorption-based removal and extraction of Cd(II), Co(II), Cu(II), Mn(II), and Ni(II) ions in aqueous solutions before FAAS analysis. The magnetic TiO2-µPs@S was well characterized by UV-vis, FTIR, XRD, SEM, and EDS techniques, and the material was well functionalized, pure, and had a slightly rod-like morphology. Under optimized conditions, initial concentration of 10 mg/L, sample solution pH of 7, adsorbent dose of 0.5 g/L, agitation speed of 200 rpm, and contact time of 45 min, the magnetic TiO2-µPs@S exhibited an adsorption capacity of 24.0, 34.9, 37.6, 38.5, and 27.9 mg/g for Cd(II), Co(II), Cu(II), Mn(II), and Ni(II), respectively. Then after, the desorption experiment was conducted using 5 mL of 0.2 M HNO3 as an eluting solvent. The method showed excellent linearity (R2 ≥ 0.998) in 0.05–10 mg/L concentration range. The limits of detection and quantification of the developed method were found to be in the range of 0.14–0.81 and 0.47–2.73 µg/L, consecutively, indicating high sensitivity of the proposed method, and <3% RSD was obtained. Furthermore, its practical applicability was assessed on tap water, lake water, and wastewater samples, and satisfactory percent recovery values, 84.5–114%, were acquired. These results indicate the potential applicability of the developed method. In general, the magnetic TiO2-µPs@S can be used as an effective adsorbent for removing heavy metals, and the adsorbent-based solid-phase extraction can be considered a promising technique for extracting and enriching heavy metals from aqueous solutions. [ABSTRACT FROM AUTHOR]

Adsorption isotherms of N,N,N',N'-tetraoctyldiglycolamide (TODGA) on three brands of hypercrosslinked polystyrene (HCP) in a medium of supercritical CO2 were constructed using the gravimetric analysis method. It was shown that, under similar conditions (T = 313 K, P = 20 MPa), HCP marks MN200 and MN202 adsorb up to 0.55 and 0.59 mmol/g TODGA, respectively, which allows their use as a carrier of the ligand under consideration. The adsorption of TODGA on MN270 under similar conditions did not exceed 0.07 mmol/g. The effect of temperature and density of the medium on the adsorption of TODGA on MN200 was assessed. It was shown that a decrease in CO2 density under isothermal conditions leads to an increase in the maximum adsorption of TODGA. The solid extractant obtained on the basis of MN200 and TODGA showed noticeable extraction properties for Nd3+ compounds. The solid extractant based on MN202 turned out to be inactive in extraction, which is probably because the pore size of the matrix is too small for the complex to form. [ABSTRACT FROM AUTHOR]

In this study, an effective and selective approach for determining methamphetamine by magnetic nanoparticles coated with poly(3-thienylboronic acid) (Fe3O4@P3Th) as a new magnetic solid-phase extraction adsorbent (MSPE) in the biological environment was developed. Synthesis of Fe3O4@P3Th magnetic nanoparticles (MNPs) was approved by Fourier transform infrared (FT-IR) spectroscopy, vibrating sample magnetometer (VSM), thermal gravimetric analysis (TGA), scanning electron microscopy (SEM), powder X-ray diffraction (XRD), and Elemental mapping and EDX analysis. The main factors influencing extraction efficiency, including the amount of nano adsorbent (20-60 mg), type and amount of organic extraction solvent (water-ethanol %), temperature (25-35 °C), pH (3-9), and extraction time (5-210 min), were investigated and optimized using a Support-vector machine. The low mean squared error (Mse) and high correlation coefficient (close to 1) for train, validation, and test data indicate successful and accurate machine backup vector predictions. Adsorption efficiency of 88.9 ± 0.42% was obtained for nano adsorbent in ethanol at the optimal condition (pH: 7, temperature: 35 °C, time: 210 min, and for 60 mg of nano adsorbent). Methamphetamine exhibited good linearity in the concentration range from 100 to 5000 ng/mL under optimal extraction conditions. The results of adsorption showed high chemical stability and adsorption capacity of nano adsorbents due to the presence of P3Th. Therefore, Fe3O4@P3Th magnetic nanoparticles (MNPs) could be used as a new MSPE in clinical and forensic laboratories to determine the materials used in the urinary environment. [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]

To improve the efficiency and accuracy of drug residue detection in agricultural products, this paper develops an automated sample preparation platform suitable for various sample matrices and preprocessing methods. The platform integrates functions such as oscillatory extraction, ultrasonic extraction, homogenization extraction, solid-phase extraction, liquid-liquid extraction, dispersive solid-phase extraction, nitrogen concentration, and calibration curve configuration. Simultaneously, it utilizes optimized salting modules, centrifuge-assisted positioning structures, and pendulum-type oscillation to achieve the automation of the sample preparation process. Experimental validation demonstrates that the system can efficiently process different samples, with average recovery rates for 22 pesticides and 12 veterinary drugs ranging from 75.4% to 115.0%, and relative standard deviations between 1.06% and 12.10%, meeting the requirements of GB/T 27404--2008. This automated sample preparation platform possesses broad applicability and has the potential to drive the automation of agricultural testing. [ABSTRACT FROM AUTHOR]

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In the present work, the herb (Poria cocos (Schw.) Wolf) residue, as an environmentally friendly and renewable biomass source, was converted into novel biochar. Biochar/sodium alginate mixed matrix membrane was fabricated. On this basis, a biochar/sodium alginate mixed matrix membrane‐based in‐syringe solid‐phase extraction was developed combined with ultra‐high performance liquid chromatography‐tandem mass spectrometry to determine nitroimidazoles in water samples. The factors including times of exaction, type, and volume of elution solvent, and sample solution pH were thoroughly optimized. Then the correlation coefficient was 0.9995–0.9997. The limit of detection of four analytes was between 0.006 and 0.014 ng/mL, and the recovery was between 79.02% and 99.1%. Consequently, the established method would provide a new perspective on monitoring nitroimidazoles in water samples. [ABSTRACT FROM AUTHOR]

In this study, a new thermosensitive surface imprinted polymer based on palygorskite was successfully synthesised by a surface imprinting technique and used as an intelligent selective recognition adsorbent for the adsorption of Cu(II) ions from aqueous solution. Scanning electron microscopy (SEM), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR) measurements results demonstrated that Cu(II)-imprinted polymer was successfully synthesised. The separation and preconcentration characteristics of Cu(II)-imprinted polymer for Cu(II) were researched by batch and column procedures. optimal intelligent recognition temperature for adsorption is 35°C and intelligent identification and elution of Cu(II) can be achieved by adjusting the temperature. The maximum static adsorption capacity of the ion-imprinted and non-imprinted sorbents for Cu(II) was 35.55 and 9.78 mg g−1, respectively. The relative selectivity factor values (ar) of Cu(II)/Zn(II), Cu(II)/Ni(II), Cu(II)/Co(II) and Cu(II)/Pb(II) were 111.48, 85.37, 98.31 and 73.85 respectively, which were all greater than 1. The Cu(II)-imprinted polymer offered fast kinetics for the adsorption and desorption of Cu(II). Under the optimised conditions (pH-5, temperature-35°C, shaking time-15 min), a detection limit of 0.21 μg L−1 with a relative standard deviation (RSD) of 2.5% for Cu(II) was obtained. Based on Cu(II)-imprinted polymer packed columns, a highly selective pre-concentration method for Cu(II) was established. The accuracy of the method has been certified using national reference materials (GBW 08301). This method has also been successfully used for the determination of Cu (II) in locally collected water samples. [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]

A rapid and simple method was optimized through experimental design and validated for the separation of chromium and manganese with magnetic sorbent of Fe3O4@Ag and 2-(2-thiazolylazo)-p-cresol ligand from the effluent of a steel factory. The adsorbed metals on the magnetic sorbent were simply separated using a magnet and collected on filter paper to measure with an X-ray fluorescence device. The infrared spectroscopy, ultraviolet–visible spectroscopy, field emission scanning electron microscopy, and wavelength-dispersive X-ray spectroscopy were used to characterize and follow the steps of the constructed sorbent synthesis. The surface response methodology was used to achieve better figures of merit and more accuracy. Optimal values for the three effective parameters of the response pH, sorbent amount, and sample solution volume were obtained to be 6.0, 4.0 mg, and 50.0 mL, respectively. Under optimum conditions, the detection limits of 0.5 µg mL−1 and 1.6 µg mL−1 for chromium and manganese ions were achieved, respectively. The acceptable linear range of 2.0–100.0 and 5.0–100.0 µg mL−1 was obtained for chromium and manganese, respectively. To show the efficiency of the method, the heavy metals of chromium (20.0 µg mL−1) and manganese (30.0 µg mL−1) were measured with a high accuracy (n = 3), and the recovery was 98% and the relative standard deviation was 2.1% in the real samples of the effluent of a steel factory. [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]

In this work, the synthesis of thin-layer, pH-sensitive molecularly imprinted membrane using methacrylic acid and maleic acid as functional monomers, ethylene glycol dimethacrylate as cross-linker, 2,2′-azobisisobutyronitrile as initiator, poly (vinylidene fluoride) as porous membrane, and celecoxib as a target molecule have been reported. Different technique analyses characterized the membrane product. A novel molecularly imprinted membrane-solid phase extraction method was used for the extraction of celecoxib and concentrating it prior to be analyzed in the human plasma and urine matrix. High-performance liquid chromatography with ultraviolet detection was used and validated for the analysis of celecoxib which was extracted from biological fluids. The molecularly imprinted membrane showed selective performance for the template, and extraction recoveries of the drug by the membrane from human plasma and urine samples were between 96.2 and 97.3%. The obtained results showed that the detection and quantification limits of the drug were 0.12 and 0.40 ng mL−1, respectively. The adsorption capacity of 4.95 mg g−1 was obtained from the fitting by the Langmuir model. The molecularly imprinted membrane can be easily regenerated eight times with sustained efficiency. Therefore, the developed method can be a good candidate for the separation and detection of celecoxib in biological samples. [ABSTRACT FROM AUTHOR]

An NH2‐MIL‐53(Al)‐DES(ChCl‐Urea) nanocomposite was synthesized for extraction and determination of Rhodamine (Rh) 6G from environmental and cosmetic samples. The deep eutectic solvent (DES) was prepared by mixing choline chloride and urea in a mole ratio of 1:2. NH2‐MIL‐53(Al)‐DES(ChCl‐Urea) nanocomposite was synthesized using the impregnation method at a ratio of 60:40 (w/w). The optimum conditions were determined after NH2‐MIL‐53(Al)‐DES(ChCl‐Urea) characterization was performed. The optimum conditions were determined as pH 8, adsorbent amount of 15 mg, total adsorption‐desorption time of 6 min, and enrichment factor of 20. The recovery values of the solid‐phase extraction method for water and cosmetic samples under optimum conditions were between 95% and 106%. NH2‐MIL‐53(Al)‐DES(ChCl‐Urea) nanocomposite was an economically advantageous adsorbent because of its reusability of 15 times. All analyses were performed using the ultraviolet‐visible spectrophotometer. The linear range, limit of detection, and limit of quantification of the method were 100–1000, 9.80, and 32.68 μg/L, respectively. The obtained results showed that the synthesized nanocomposite is a suitable adsorbent for the determination of Rh 6G in water and cosmetic samples. The real sample applications were verified with the high‐performance liquid chromatography system. [ABSTRACT FROM AUTHOR]

Today's environment is under the influence of numerous substances and most of them are not covered by current national and international regulations. Substances that are classified as contaminants of emerging concern, CECs, are not regulated nor systematically controlled in the environment, and they belong to the different chemical classes such as pesticides in current use, pharmaceutically active compounds (PhACs), personal care products, illicit drugs, hormones, micro- and nano-plastics, per- and poly-fluoroalkyl substances (PFAS), and many others. Once released CECs end up in surface water where they can be either accumulated or transported to the other environmental compartments, i.e. soil (by irrigation), underground water, or drinking water. The aim of the research was to investigate the efficiency of different selected solid-phase extraction (SPE) cartridges for preparation of water samples for simultaneous analysis of several CECs. For this purpose, a model mix solution of selected CECs in concentration relevant to environmental appearance was used. The selected CECs (14 PhACs, 11 pesticides in current use, and 4 PFAS) represented emerging contaminants with different properties, including polarities, and varying adverse effect on the environment and human health. Different types of sorbents were investigated: (i) commercial single-layer HLB, (ii) homemade multi-layer I: HLB plus a mix of WAX, WCX, and PPL, and (iii) multi-layer II: mix of WAX, WCX, and PPL plus HLB. The results revealed that the single-layer sorbent showed better efficiency in extraction of the analyzed CECs. Multi-layer sorbent should be further investigated to elucidate the possible reason for the poor extraction of some compounds, as development of a balanced extraction for a wider range of contaminants with different polarities, especially for non-target analysis of chemical residues, is required in order to capture the occurrence of the full profile of micropollutants. [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]

Objective： A method based on high-performance liquid chromatography-mass spectrometry was developed for the simultaneous determination of bisphenol A and nonylphenol in food packaging material. Methods: The extraction solvent and extraction method were investigated. Solid-phase extraction （SPE） conditions were optimized. The effects of solid phase extraction column, loading solvent, eluting solvent and elution solvent on the purification effect were systematically analyzed. The samples were ultrasonic extracted with dichloromethaneand cleaned up on a solid-phase extraction （SPE） cartridge equipped with packing material of silicone. The separation was performed on a Venusil MP C18（2）（100 mm×2.1 mm,2.6 μm）by gradient elution with 0.1% ammonia solution and methanol as mobile phase. The analytes were determined with multiple reaction monitoring （MRM） mode under electrospray negative ionization mode and quantified by an internal standard method. Results: The results indicated that good linearities was obtained for bisphenol A and nonylphenol both within the concentration range of 1.0~200.0 μg/L. The average recoveries of each analyte at three spiked levels of 1.0, 10.0, 200.0 μg/kg were in the range of 89.2%~101.2%, with relative standard deviations （RSD） of 3.1%~6.2%. The limits of detection （LODs） and limits of quantification （LOQs） were 0.5 μg/kg and 1.0 μg/kg, respectively. Conclusion: The method was proved to be a simple, accurate and sensitive method and was successfully applied to detect bisphenol A and nonylphenol in food packaging material. It can also provide reference for the determination of bisphenol A and nonylphenol in food.

Flavonoids have attracted considerable attention due to their health benefits. This study aimed to investigate the flavonoid profiles and antioxidant activity of Paeonia lactiflora petal flavonoid extract (PPF). The UHPLC-ESI-Q-Exactive HF MS/MS method was established for characterization, and 21 predominant flavonoid compounds were tentatively identified in PPF. Among them, isoscutellarein-7-(6′-acetylallosyl-(1->2)-glucoside) and scutellarin methylester were discovered in PPF for the first time. Pretreatment with PPF significantly reduced H2O2-induced cell damage, ROS accumulation, and malondialdehyde content and increased the activity of SOD, CAT, and GSH-Px in buffalo rat liver 3A (BRL3A) cells. Moreover, the expression of nuclear Factor E2-related factor (Nrf2) was upregulated by PPF, whose expression trend was consistent with that of heme oxygenase-1 (HO-1), glutamate-cysteine ligase catalytic subunit (GCLC), and NAD(P)H quinone oxidoreductase-1 (NQO1). These findings suggested that herbaceous peony flavonoids can be used as a natural bioactive agent to prevent oxidative stress.

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.

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.

The sorption properties of Na-modified Ukrainian Transcarpathian clinoptilolite towards neodymium aqueous solutions under dynamic conditions have been investigated. The sorption capacity of the Na-from of Transcarpathian clinoptilolite towards Nd(III) significantly depends on the concentration of neodymium salt, the pH of the solution, and the heat treatment temperature of the sorbent. Nd(III) is most efficiently sorbed from slightly alkaline solutions (pH 8.5), mainly by adsorption of neutral hydrolyzed forms of Nd(OH)3 on the surface of Na-clinoptilolite samples preheated at 75 °C. During the passage of an Nd(III) solution with a concentration of 1 μg mL−1 through the sorbent at a rate of 3 mL min−1 under optimal conditions, the sorption capacity of Na-clinoptilolite is 7.2 mg g−1, which is in 4 and 2.3 times higher than that of natural and acid-modified forms of this zeolite. It is shown that under the experimental conditions with an increase in the flow rate, the thickness of the stationary surface layer decreases, which leads to a decrease in the sorption capacity of Na-clinoptilolite. The best Nd(III) desorbents are solutions of mineral acids and acidified solutions of alkali metal salts (except NaCl), which provide 93–98 % extraction of lanthanide from the zeolite matrix. The method for neodymium trace amounts preconcentration from aqueous solutions in a solid-phase extraction mode with a further determination of this rare earth element by a spectrophotometric method was developed. The detection limit of this method is 0.75 ng mL−1 and the linearity was evaluated in the range of 2.5–500 ng mL−1.

In this research, the magnesium ferrite/zinc oxide (MgFe2O4/ZnO) nanocomposite has been utilized as an effective adsorbent in the ultrasound-assisted dispersive solid-phase extraction (USA-DSPE) coupled to a spectrophotometric method for preconcentration of methylene blue (MB) and safranin O (SO) dyes. X-Ray diffraction (XRD), vibrating sample magnetometer (VSM), transmission electron microscopy (TEM), and field emission scanning electron microscopy (FESEM) analyses were performed to characterize and confirm the properties of the synthesized MgFe2O4/ZnO nanocomposite. Box-Behnken design (BBD) based on response surface methodology (RSM) was utilized to optimize the variables. The results of this research showed that the maximum extraction efficiency was obtained at pH = 7, eluent volume of 140 µL, adsorbent amount of 1.53 mg, and ultrasonic time of 8 min. After optimization by RSM and using the Quadratic model, the extraction efficiency for MB and SO was 98.60% and 97.23%, respectively. The analysis of variance (ANOVA) showed that the data obtained from the experiment were consistent with the predicted model. Under optimal conditions, the calibration curve was linear in the range of 5–1000 µg/L (coefficient of determination of 0.9884) for MB and 10–1100 µg/L (coefficient of determination of 0.9973) for SO. The limit of detections (LOD) of the proposed method for MB and SO were determined as 1.5 µg/L and 3 µg/L, respectively. The relative standard deviations (RSD, n = 5) for MB and SO were obtained as 1.1% and 2.1%, respectively. The results of adsorbent recovery revealed that MgFe2O4/ZnO nanocomposite could be used several times without a significant adsorbent efficiency loss. Furthermore, the findings of interference studies revealed that the presence of different ions does not cause substantial interference with the extraction of dyes. The environmental water samples analysis showed that the extraction efficiency for dyes was in the range of 93.74–99.11%.

Background: In-hospital therapeutic drug monitoring (TDM) requires a suitable quantification method for target drugs from the viewpoint of precision, throughput, and testing costs. We previously developed a practical HPLC-UV platform for quantification of serum levels of various drugs. In this report, the platform was effectively applied to the quantification of patient serum levels of five different drugs by clinical professionals in our hospital during their daily work. Methods: The residual sera of patients receiving carbamazepine (CBZ), phenytoin (PHT), lamotrigine (LTG), vancomycin (VCM), or voriconazole (VRCZ) were used in the present clinical study. The quantification method for each drug consisted of rapid solid-phase extraction (SPE) of each drug in the patient serum, followed by optimized HPLC-UV analysis of the drug in the SPE eluate. Furthermore, patient serum levels of PHT, CBZ, and VCM were also measured by ligand-binding assay using a cobas® analyzer in our hospital, and those of LTG and VRCZ were measured by HPLC-MS/MS at an outsourced provider. Passing–Bablok regression analysis and Bland–Altman analysis were employed to analyze the agreement of drug levels in patient sera, which was separately quantified using two different methods—our HPLC-UV platform and the cobas analyzer, or HPLC-UV and HPLC-MS/MS. Results: All analytical conditions of the present method using our HPLC-UV platform were well optimized for each target drug quantification in the patient's serum, and the quantification method for each drug was fully validated for accuracy, precision and reproducibility. Furthermore, Passing–Bablok regression analysis and Bland–Altman analysis revealed that patient serum levels of PHT, CBZ, and VCM quantified by our HPLC-UV platform were closely correlated with those quantified by the cobas® analyzer, and the levels of LTG and VRCZ quantified by our HPLC-UV platform were also correlated with those quantified by HPLC-MS/MS. Conclusions: Our HPLC-UV platform can be performed without requiring special analytical techniques. This platform is expected to be used for the measurement of blood levels of multiple drugs for in-hospital routine TDM. [ABSTRACT FROM AUTHOR]

Coffee is one of the most consumed beverages in the world. Coffee provides to the consumer special sensorial characteristics, can help to prevent diseases, improves physical performance and increases focus. In contrast, coffee consumption supplies a significant source of substances with carcinogenic and genotoxic potential such as furan, hydroxymethylfurfural (HMF), furfural (F), and acrylamide (AA). The present review addresses the issues around the presence of such toxic substances formed in Maillard reaction (MR) during thermal treatments in food processing, from chemical and, toxicological perspectives, occurrences in coffee and other foods processed by heating. In addition, current strategies advantages and disadvantages are presented along with application of molecular imprinting technology (MIT) and poly (ionic liquid) s (PIL) as an alternative to reduce the furan, HMF, F and AA content in coffee and other foods. [ABSTRACT FROM AUTHOR]

Polymer monoliths are promising materials for sample preparation due to their high porosity, pH stability, and simple preparation. The use of melamine formaldehyde foams has been reported as an effective support to prepare highly robust silica and polymer monoliths. Herein, divinylbenzene monoliths based on a 50:50 (%, w/w) crosslinker/porogen ratio have been nested within a melamine‐formaldehyde sponge, resulting in monoliths with a surface area higher than 400 m2/g. The extraction performance of these monoliths was evaluated for the extraction of endocrine‐disrupting bisphenols from aqueous solutions. We evaluated for the first time the versatility of sponge‐nested polymer monoliths by comparing three different extraction modes (vortex mixing, magnetic stirring, and orbital shaking). Vortex mixing showed a comparable recovery of bisphenols (39%–81%) in a shorter extraction time (30 min, instead of 2 h). In addition, the robustness of the sponge‐nested polymer monoliths was demonstrated for the first time by reshaping a larger monolithic cube (0.125 cm3) into four smaller pieces (4 × 0.03125 cm3) leading to a 16%–21% increase in extraction efficiency. This effect was attributed to an increase in the effective contact area with the sample, obtaining a higher analyte extraction capacity. [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.)