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The complexity of the drug market and the constant updating of drugs have been challenging issues for drug regulatory authorities. With the emergence of new psychoactive substances (NPS) and the nonmedical use of prescription drugs, forensic and toxicology laboratories have had to adopt new drug screening methods and advanced instrumentation. Using high‐performance liquid chromatography coupled with Orbitrap mass spectrometry, we developed a screening method for common NPS and other drugs. Two milliliters of mixed solvent of n‐hexane and ethyl acetate (1:1, v:v) were added to 500 μL of blood or urine sample for liquid–liquid extraction, and methanol extraction was used for hair samples. The developed method was applied to 3897 samples (including 332 blood samples, 885 urine samples, and 2680 hair samples) taken from drug addicts in a province of China during 2019–2021. For urine and blood samples, the limits of detection (LODs) ranged from 1.68 pg/mL to 10.7 ng/mL. For hair samples, the LODs ranged from 3.30 × 10−5 to 4.21 × 10−3 ng/mg. The matrix effects of urine, blood, and hair samples were in the range of 47.6%–121%, 39.8%–139%, and 6.35%–118%, respectively. And the intra‐day precision was 3.5%–6.0% and the inter‐day precision was 4.18%–9.90%. Analysis of the actual samples showed an overall positive detection rate of 58.9%, with 5.32% of the samples indicating the use of multiple drugs. [ABSTRACT FROM AUTHOR]

A green reversed‐phase liquid chromatography method was developed to determine caffeine (CF), theobromine (TB), theophylline (TP), and paraxanthine (PX). The stationary phase was a silica‐based C18 monolithic column (100 × 3.0 mm2 i.d.), eluted with a gradient from 6% to 10% (v/v) of ethanol in water, at a flow rate of 0.75 mL/min (35°C) and UV detection at 272 nm. The compounds were separated in less than 6 min, with a total time of 10 min for column reconditioning. The effect of gradient composition, flow rate, injection volume, and column temperature was evaluated in the separation efficiency, especially regarding the critical pair PX/TP, for which the best resolution was 1.37. The linear range was between 0.5 and 100 µg/mL. The LODs were 0.065, 0.057, 0.040, and 0.044 mg/mL for TP, TB, PX, and CF, respectively. The method was applied to green tea and yerba mate infusions, soft drinks, energy drinks, and soluble coffee. Urine samples were analyzed before and after solid‐phase extraction. The accuracy was evaluated by the spiking/recovery strategy standing in the 79.6% to 116.4% range. The separation performance and the mobile phase consumption were compared to those of another method using a gradient of methanol in water. [ABSTRACT FROM AUTHOR]

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

Copyright of Chinese Journal of Inorganic Analytical Chemistry / Zhongguo Wuji Fenxi Huaxue is the property of Beijing Research Institute of Mining & Metallurgy Technology Group 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.)

Phytoestrogens, natural compounds with structural similarity to 17-β-estradiol, are known to have potential health benefits, including in hormone-dependent malignancies. The therapeutic interest and some safety concerns observed triggered the need to develop accurate methods to assess their level in different matrices. This narrative review examines the existing analytical methods used to isolate, quantify, and characterize phytoestrogens and their metabolites in plants, foods, and biological samples. Different conventional and modern extraction techniques, such as ultrasonication-assisted extraction, supercritical fluid extraction, or enzyme-assisted extraction, were presented and compared. The advantages and limitations of the existing analytical methods, such as high-performance liquid chromatography using different sensitive detectors, gas chromatography often coupled with mass spectrometry, and immunoassay methods, are highlighted, along with the need for ongoing research to improve the sensitivity and selectivity of the analysis. [ABSTRACT FROM AUTHOR]

Over the years, monitoring the quality of the environment, food, and human health has emerged as a fundamental objective of scientific investigation. Various analytical techniques have been devised and continually refined to ensure a high standard of living. Among these methods, dispersive liquid–liquid microextraction (DLLME) stands out as a widely used approach to conduct analytical evaluations and pre-concentrations of chemical compounds. This review provides an account of the evolution of DLLME over the past five years (2018–2023). The Scopus search engine was used to search for scientific articles. The selection of relevant articles was carried out according to the criteria described below. Emphasis was placed on the evolution that DLLME has undergone over the years by integrating it with other pre-concentration methods in order to amplify the concentration factor and improve analytical precision. Factors such as solvent dispersion and extraction, dispersion formation, and the recovery of the solvent containing the extracted analytes were examined. Additionally, derivatization systems were evaluated to refine both qualitative and quantitative analysis. These efforts aim to introduce methods that are safe for operators, environmentally friendly, and economical. This review evaluates the advantages and disadvantages displayed by the evolution of this technique in the phases before, during, and after its application. [ABSTRACT FROM AUTHOR]

This research aims to address the need for monitoring the behavior of organic and inorganic materials in hypergravity conditions. To fulfill this objective, a container with specific features was designed. The container has a box with a lid, measuring 10×10×10 cm, conforming to the 1U volume of the CubeSat standard. It includes four cylindrical spaces to accommodate the sample wells. The container was 3D printed using polylactic acid (PLA) wire. For the electronic components, four ESP32-CAM modules were utilized, with two programmed to capture and upload photos to the cloud, and the other two programmed to capture and store photos on a micro SD memory card. Additionally, four light emitting diodes (LEDs) were incorporated to illuminate the well spaces. The total weight of the container is 450 grams, and it has a maximum wireless upload distance of 10 meters to the cloud. The storage capacity of the SD memory card determines the number of images that can be saved. [ABSTRACT FROM AUTHOR]

During the commission of crimes, traces of biological origin are left on the objects of the environment, tools, clothing, and the body of the participants. To conduct an identification study, an expert needs to compare the traces of the crime with biological samples of the person being tested. Criteria for determining biological samples are proposed. The biological criterion means that the samples reflect the internal and external properties of a person as a biological organism. The informational criterion is that the samples meet certain requirements: undoubted origin, required quantity, proper quality, compatibility with traces of crime. The identification criterion establishes that the human properties reflected by the samples are individual, stable, cannot be deliberately altered by a person and are suitable for identification. The procedural criterion means that biological samples must be collected in a lawful manner. Based on these criteria, biological samples for examination include: body parts; secretions as products of human activity; imprints of the skin relief of the human body. The mandatory participants in the collection of biological samples as a procedural action are: persons from whom biological samples are collected; officials who conduct the collection of samples and are responsible for its legality and validity; a specialist or expert; witnesses; employees of the relevant law enforcement agencies (in the case of compulsory collection of biological samples). Optional participants are a defence counsel, legal representative, representative, lawyer, doctor at their request. During the compulsory collection of biological samples, in order to ensure the legality, objectivity, reliability of the objects of expert research, preservation of health and observance of human rights, it is necessary to comply with legal, ethical, medical and forensic conditions. The author proposes a general algorithm for the tactics of obtaining biological samples for examination at the stage of pre-trial investigation, which includes the preparatory, working and final stages.

The levels of the MMPs in the biological samples of confirmed patients with gastric cancer are significantly elevated compared to those found in healthy people. Therefore, a novel 3D stochastic microsensor based on graphene oxide, modified with gold nanoparticles and (Z)-N-(pyridin-4-yl-methyl) octadec-9-enamide (namely N2-AuNP/GO), was designed for the determination of MMP-2 in biological samples, and validated for the screening tests of biological samples in order to be used for the early diagnosis of gastric cancer. The proposed sensor presents a low limit of quantification (1.00 × 10−22 g mL−1), high sensitivity (1.84 × 107 s−1 g−1 mL), and a wide working concentration range (1.00 × 10−22–1.00 × 10−7 g mL−1). Recovery values higher than 99.15% were recorded for the assay of MMP-2 in whole blood, gastric tissue tumors, saliva, and urine samples. [ABSTRACT FROM AUTHOR]

AbstractReducing monosaccharides and their phosphates are critical metabolites in the central carbon metabolism pathway of living organisms. Variations in their content can indicate abnormalities in metabolic pathways and the onset of certain diseases, necessitating their analysis and detection. Reducing monosaccharides and their phosphates exhibit significant variations in content within biological samples and are present in many isomers, which makes the accurate quantification of reducing monosaccharides and their phosphates in biological samples a challenging task. Various analytical methods such as spectroscopy, fluorescence detection, colorimetry, nuclear magnetic resonance spectroscopy, sensor-based techniques, chromatography, and mass spectrometry are employed to detect monosaccharides and phosphates. In comparison, chromatography and mass spectrometry are highly favored for their ability to simultaneously analyze multiple components and their high sensitivity and selectivity. This review thoroughly evaluates the current chromatographic and mass spectrometric methods used for detecting reducing monosaccharides and their phosphates from 2013 to 2023, highlighting their efficacy and the advancements in these analytical technologies. [ABSTRACT FROM AUTHOR]

Benchtop NMR provides improved accessibility in terms of cost, space, and technical expertise. In turn, this encourages new users into the field of NMR spectroscopy. Unfortunately, many interesting samples in education and research, from beer to whole blood, contain significant amounts of water that require suppression in 1H NMR in order to recover sample information. However, due to the significant reduction in chemical shift dispersion in benchtop NMR systems, the sample signals are much closer to the water resonance compared to those in a corresponding high‐field NMR spectrum. Therefore, simply translating solvent suppression experiments intended for high‐field NMR instruments to benchtop NMR systems without careful consideration can be problematic. In this study, the effectiveness of several popular water suppression schemes was evaluated for benchtop NMR applications. Emphasis is placed on pulse sequences with no, or few, adjustable parameters making them easy to implement. These fall into two main categories: (1) those based on Pre‐SAT including Pre‐SAT, PURGE, NOESY‐PR, and g‐NOESY‐PR and (2) those based on binomial inversion including JRS and W5‐WATERGATE. Among these schemes, solvent suppression sequences based on Pre‐SAT offer a general approach for easy solvent suppression for samples with higher analyte concentrations (sucrose standard and Redbull™). However, for human urine, binomial‐like sequences were required. In summary, it is demonstrated that highly efficient water suppression approaches can be implemented on benchtop NMR systems in a simple manner, despite the limited spectral dispersion, further illustrating the potential for widespread implementation of these approaches in education and research. [ABSTRACT FROM AUTHOR]

Flavonoids are a prominent group of plant phenolics (polyphenol group) extensively present in the human diet and associated with health promotion. Flavonoids are essential in various pharmaceutical, nutraceutical, and cosmetic applications. To collect and categorize these compounds, we comprehensively assessed High-performance liquid chromatography (HPLC) techniques published to analyze flavonoids in various matrices. Most documented methods employed liquid chromatography with ultraviolet detection (HPLC-UV) and tandem mass spectrometry (LC-MS/MS) methods. Among chromatographic techniques, reversed-phase liquid chromatography remains the predominant and efficient method for separating various analytes. This review explores the primary chromatographic methods used to separate and quantify flavonoids in herbs, fruits, and biological samples. This article examines recent literature on applying liquid chromatography with different detection methods for analyzing flavonoids. To examine recent literature on applying liquid chromatography with different detection methods for analyzing flavonoids. It offers valuable insights to researchers as they prepare to develop quantification methods. [ABSTRACT FROM AUTHOR]

This work discusses ceramic filter materials used as substrates to study biological objects by electron microscopy. The composition, structure, pore sizes, and morphology of ceramic substrates made of foamed silicate prior to and following the application of inverse silicon oxide opals were evaluated by x-ray diffraction analysis and SEM method. Adescription of the use of the obtained filtering substrates in an experiment with biological objects is given. The substrates seem promising for electron microscopy, since they can be used for sample preparation of biological objects with the use of metal spraying or ionic liquid. This technique, together with the filtering porous material and the technical capabilities of the microscope, preserves the physical characteristics of biological objects. [ABSTRACT FROM AUTHOR]

We developed a novel electrochemical sensor for the detection of alfuzosin (AFZ), a drug used to treat benign prostatic hyperplasia, using a double-shelled Co3O4/NiCo2O4 nanocomposite-modified electrode. The nanocomposites were synthesized using a template-assisted approach, with zeolitic imidazole framework-67 (ZIF-67) as the sacrificial template, involving the formation of uniform ZIF-67/Ni-Co layered double hydroxide (LDH) hollow structures followed by calcination to achieve the final nanocomposite. The nanocomposite was characterized by various techniques and showed high porosity, large surface area, and good conductivity. The nanocomposite-modified electrode exhibited excellent electrocatalytic activity towards AFZ oxidation, with a wide linear range of 5–180 µM and a low limit of detection of 1.37 µM. The sensor also demonstrated good repeatability, reproducibility, and stability selectivity in the presence of common interfering substances. The sensor was successfully applied to determine the AFZ in pharmaceutical tablets and human serum samples, with satisfactory recoveries. Our results suggest that the double-shelled Co3O4/NiCo2O4 nanocomposite is a promising material for the fabrication of electrochemical sensors for AFZ detection. [ABSTRACT FROM AUTHOR]

Proton magnetic resonance spectroscopy (1H MRS) presents a powerful tool for revealing molecular-level metabolite information, complementary to the anatomical insight delivered by magnetic resonance imaging (MRI), thus playing a significant role in in vivo/in vitro biological studies. However, its further applications are generally confined by spectral congestion caused by numerous biological metabolites contained within the limited proton frequency range. Herein, we propose a pure-shift-based 1H localized MRS method as a proof of concept for high-resolution studies of biological samples. Benefitting from the spectral simplification from multiplets to singlet peaks, this method addresses the challenge of spectral congestion encountered in conventional MRS experiments and facilitates metabolite analysis from crowded NMR resonances. The performance of the proposed pure-shift 1H MRS method is demonstrated on different kinds of samples, including brain metabolite phantom and in vitro biological samples of intact pig brain tissue and grape tissue, using a 7.0 T animal MRI scanner. This proposed MRS method is readily implemented in common commercial NMR/MRI instruments because of its generally adopted pulse-sequence modules. Therefore, this study takes a meaningful step for MRS studies toward potential applications in metabolite analysis and disease diagnosis. [ABSTRACT FROM AUTHOR]

AbstractOvarian cancer, which affects the female reproductive organs, is one of the most common types of cancer. Since this type of cancer has a high mortality rate from gynaecological cancers, the scientific community shows great interest in studies on its treatment. Chemotherapy, radiotherapy, and surgical treatment methods are used in its treatment. In the absence of targeted treatments in these treatment methods, side effects occur in patients, and patients show resistance to the drug. In addition, the underlying causes of ovarian cancer are still not fully known. The scientific world thinks that genetic factors, environmental conditions, and consumed foods may cause this cancer. The most important factor in the treatment of ovarian cancer is early diagnosis. Therefore, the drugs used in the treatment of ovarian cancer are platinum-based anticancer drugs. In addition to these drugs, the most preferred treatment method recently is targeted treatment approaches using poly(adenosine diphosphate ribose) polymerase (PARP) inhibitors. In this review, studies on the sensitive analysis of the treatment methods of these new-generation drugs used in the treatment of ovarian cancer have been comprehensively examined. In addition, the basic features, structural aspects, and biological data of analytical methods used in treatments with new-generation drugs are explained. Analytical studies carried out in the literature in recent years aim to show future developments in how these new-generation drugs are used today and to guide future studies by comprehensively examining and explaining the structure-activity relationship, mechanism of action, toxicity, and pharmacokinetic studies. Finally, in this study, the methods used in the analysis of drugs used in the treatment of ovarian cancer and the studies conducted between 2015 and 2023 were discussed in detail. [ABSTRACT FROM AUTHOR]

For the simultaneous determination of monoamine neurotransmitters (NTs) like dopamine, serotonin, noradrenaline, and epinephrine, and their metabolites (metanephrine, normetanephrine, 3-methoxytyramine, vanillylmandelic acid, 3,4-dihydroxyphenylacetic acid, homovanillic acid, and 5-hydroxyindoleacetic acid), a robust liquid chromatography method coupled with tandem mass spectrometry (LC–MS/MS) was introduced as the analytical method. This analytical method proved to be accurate for the simultaneous measurement of the amounts of 11 NTs and their metabolites in biological samples. The method proved to be more efficient and better than the previously reported method in terms of precision, recovery, sample requirement, and extraction procedure. The reported method requires only 100 μL of blood and 200 μL of urine, and the extraction procedure requires acetonitrile precipitation, filtration, drying, and reconstitution in water. The separation of all analytes was performed on an C18 column (4.6 mm × 150 mm and 1.8 μm). A 10 min gradient elution program with a mobile phase consisting of phase A (0.2% formic acid in water) and phase B (methanol) was used. The positive ionization mode was used for the detection of all analytes in multiple reaction monitoring (MRM). The proposed method was validated with an internal standard and yielded lower limits of detection and quantification ranges of 0.0182–0.0797 ng/mL and 0.0553–0.2415 ng/mL, respectively, with a good linearity (R2) between 0.9959 and 0.9994. The recoveries ranged from 73.37% to 116.63% in blood and from 80.9% to 115.33% in urine. For the NTs and metabolites, the intra- and interday % CV were 0.24–9.36 and 0.85–9.67, respectively. The developed LC–MS/MS method was successfully used for the determination of trace amounts of endogenous compounds in human blood and urine samples. [ABSTRACT FROM AUTHOR]

Background Atomic force microscopy (AFM) is one of the main techniques used to characterize the mechanical properties of soft biological samples and biomaterials at the nanoscale. Despite efforts made by the AFM community to promote open-source data analysis tools, standardization continues to be a significant concern in a field that requires common analysis procedures. AFM-based mechanical measurements involve applying a controlled force to the sample and measure the resulting deformation in the so-called force-distance curves. These may include simple approach and retract or oscillatory cycles at various frequencies (microrheology). To extract quantitative parameters, such as the elastic modulus, from these measurements, AFM measurements are processed using data analysis software. Although open tools exist and allow obtaining the mechanical properties of the sample, most of them only include standard elastic models and do not allow the processing of microrheology data. In this work, we have developed an open-source software package (called PyFMLab, as of python force microscopy laboratory) capable of determining the viscoelastic properties of samples from both conventional force-distance curves and microrheology measurements. Methods PyFMLab has been written in Python, which provides an accessible syntax and sufficient computational efficiency. The software features were divided into separate, self-contained libraries to enhance code organization and modularity and to improve readability, maintainability, testability, and reusability. To validate PyFMLab, two AFM datasets, one composed of simple force curves and another including oscillatory measurements, were collected on HeLa cells. Results The viscoelastic parameters obtained on the two datasets analysed using PyFMLab were validated against data processing proprietary software and against validated MATLAB routines developed before obtaining equivalent results. Conclusions Its open-source nature and versatility makes PyFMLab an open-source solution that paves the way for standardized viscoelastic characterization of biological samples from both force-distance curves and microrheology measurements.

Given the high contagiousness and rapid spread of the rinderpest virus, timely and accurate diagnosis plays a key role in preventing epidemics and taking measures to control the disease. The study aims to evaluate the efficiency of using multiplex primers in the polymerase chain reaction method for the detection of rinderpest virus ribonucleic acid. The study included the analysis of samples such as blood serum and conjunctival swabs from 50 animals with clinical manifestations of the disease. The experiment involved the collection of clinical samples such as blood serum and conjunctival washings. The results demonstrate the high specificity of the developed primers. These primers stand out because they use two pairs of the same gene region with different variable sequences that are specific for all strains of the rinderpest virus. In the polymerase chain reaction, both pairs of primers are used simultaneously at equal concentrations and under the same conditions. An additional polymerase chain reaction performed using these primers at the optimal annealing temperature confirmed the successful amplification and specificity of the primers. The absence of dimers and nonspecific products in the negative control confirmed the purity and reliability of the results. Thus, these results demonstrate that the use of these multiplex polymerase chain reaction primers allows for the efficient detection of the ribonucleic acid of the rinderpest virus of different strains. The developed multiplex primers represent an innovative method for the diagnosis of rinderpest virus with the potential for use in veterinary practice and animal disease control

One-carbon folate metabolites and one-carbon-related amino acids play an important role in human physiology, and their detection in biological samples is essential. However, poor stability as well as low concentrations and occurrence in different species in various biological samples make their quantification very challenging. The aim of this study was to develop a simple, fast, and sensitive ultra-high-performance liquid chromatography MS/MS (UHPLC–MS/MS) method for the simultaneous quantification of various one-carbon folate metabolites (folic acid (FA), tetrahydrofolic acid (THF), p-aminobenzoyl-L-glutamic acid (pABG), 5-formyltetrahydrofolic acid (5-CHOTHF), 5-methyltetrahydrofolic acid (5-CH3THF), 10-formylfolic acid (10-CHOFA), 5,10-methenyl-5,6,7,8-tetrahydrofolic acid (5,10-CH+-THF), and 4-α-hydroxy-5-methyltetrahydrofolate (hmTHF)) and one-carbon-related amino acids (homocysteine (Hcy), methionine (Met), S-ade-L-homocysteine (SAH), and S-ade-L-methionine (SAM)). The method was standardized and validated by determining the selectivity, carryover, limits of detection, limits of quantitation, linearity, precision, accuracy, recovery, and matrix effects. The extraction methods were optimized with respect to several factors: protease–amylase treatment on embryos, deconjugation time, methanol precipitation, and proteins' isoelectric point precipitation on the folate recovery. Ten one-carbon folate metabolites and four one-carbon-related amino acids were detected using the UHPLC–MS/MS technique in various biological samples. The measured values of folate in human plasma, serum, and whole blood (WB) lay within the concentration range for normal donors. The contents of each analyte in mouse plasma were as follows: pABG (864.0 nmol/L), 5-CH3THF (202.2 nmol/L), hmTHF (122.2 nmol/L), Met (8.63 μmol/L), and SAH (0.06 μmol/L). The concentration of each analyte in mouse embryos were as follows: SAM (1.09 μg/g), SAH (0.13 μg/g), Met (16.5 μg/g), 5,10-CH+THF (74.3 ng/g), pABG (20.6 ng/g), and 5-CH3THF (185.4 ng/g). A simple and rapid sample preparation and UHPLC–MS/MS method was developed and validated for the simultaneous determination of the one-carbon-related folate metabolites and one-carbon-related amino acids in different biological samples. [ABSTRACT FROM AUTHOR]

This study focused on the development of chitosan and CNTs enhanced glassy carbon electrodes (CS/CNT/GCE) as a methadone electrochemical biosensor and its application to athlete doping testing in biological and food samples. SEM, FTIR, and XRD analysis results indicated the successful synthesis of CS/CNT-modified GCE. An electrochemical study of modified electrodes using the methods of cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and differential pulse voltammetry (DPV) revealed an improvement in the sensitivity, stability, and selectivity of the CS/CNT/GCE within methadone determination due to a synergistic effect between CS and CNT. The CS/CNT/GCE showed a robust and broad linear range of 40 to 1000 µM, a sensitivity of 0.03204 µA/µM, and a detection limit of 0.019 µM for methadone detection. In this investigation, genuine pear samples and blood serum samples from five athletes were utilized to examine the application of the created methadone sensor, and the results showed substantial recovery values (above 96.00%) and good precision (RSD value less than 4.76%). These results demonstrated that the CS/CNT/GCE sensor was dependable and precise for measuring methadone concentrations in biological and food samples. [ABSTRACT FROM AUTHOR]

Genetic expertise is a judicial procedure and aims to establish DNA, which is a molecule that contains the unique genetic code of each person, and by applying molecular biology techniques, genetic data can be obtained from the reference profile with those highlighted in the unknown genetic profile or with genetic characteristics of another person. The presentation will show the legal provisions in the matter, the method of carrying out the forensic genetic expertise, its probative value, as well as the storage of the genetic profile. [ABSTRACT FROM AUTHOR]

Copyright of Baghdad Science Journal is the property of Republic of Iraq Ministry of Higher Education & Scientific Research (MOHESR) 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.)

Organophosphorous (OP) pesticides can cause many human diseases. In this study, the separation and determination of two organophosphorous pesticides (diazinon and methyl-parathion) in biological samples using solid-phase extraction method prior to their measurements by high‐performance liquid chromatography (HPLC) were investigated. Herein, a new functionalized cerium-based metal–organic framework (MOF) bearing oxime moiety, denoted here UiO-66(Ce)-MO, was synthesized through two-synthetic steps from the pristine UiO-66(Ce) and then applied as an efficient porous adsorbent for the extraction of pesticides from biological samples. Various techniques including Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), and Brunauer–Emmett–Teller (BET) analysis were used for the description of adsorbent. The optimization of variables was performed by Box–Behnken design combined with response surface methodology. The factors' effects including pH, eluent volume (EV), sample flow rate (SF) and eluent flow rate (EF) were also examined. The optimum conditions for both compounds were pH 5.5, eluent volume 0.6 mL, SF 2 mL min−1, and EF 0.2 mL min−1, leading to 97.1% and 96.0% removal of diazinon and methyl-parathion, respectively. Under the optimum conditions, the maximum adsorption capacity was obtained 454.5 mg g−1 for methyl-parathion and 476.2 mg g−1 for diazinon. The limit of detection (LOD) was found to be 0.04 μgL−1 for diazinon and 0.06 μgL−1 for methyl-parathion. Sensitivity analysis showed that pH plays a significant role on the efficiency of both organic pollutants. Remarkably, the results showed that this adsorbent outperforms the other UiO-66(Ce) samples and is suitable for separation and determination of these organic materials from water and biological real samples (blood plasma and urine). A porous oxime-functionalized Ce-MOF, UiO-66(Ce)-MO, was synthesized and applied for efficient extraction and determination of trace amounts of methyl-parathion and diazinon from water and biological samples. [ABSTRACT FROM AUTHOR]

Understanding and comparing the applicability of electromembrane extraction (EME) and liquid‐phase microextraction (LPME) is crucial for selecting an appropriate microextraction approach. In this work, EME and LPME based on supported liquid membranes were compared using biological samples, including whole blood, urine, saliva, and liver tissue. After optimization, efficient EME and LPME of clozapine from four biological samples were achieved. EME provided higher recovery and faster mass transfer for blood and liver tissue than LPME. These advantages were attributed to the electric field disrupting clozapine binding to interfering substances. For urine and saliva, EME demonstrated similar recoveries while achieving faster mass transfer rates. Finally, efficient EME and LPME were validated and evaluated combined with liquid chromatography‐tandem mass spectrometry (LC‐MS/MS). The coefficient of determination of all methods was greater than 0.999, and all methods showed acceptable reproducibility (≤14%), accuracy (90%–110%), and matrix effect (85%–112%). For liver and blood with high viscosity and complex matrices, EME‐LC‐MS/MS provided better sensitivity than LPME‐LC‐MS/MS. The above results indicated that both EME and LPME could be used to isolate non‐polar basic drugs from different biological samples, although EME demonstrated higher recovery rates for liver tissue and blood. [ABSTRACT FROM AUTHOR]

Dimetridazole (DMZ) is a derivative of nitroimidazole and is a veterinary drug used as an antibiotic to treat bacterial or protozoal infections in poultry. The residues of DMZ cause harmful side effects in human beings. Thus, we have constructed a superior electrocatalyst for DMZ detection. A copper (Cu)-integrated poly(aniline) (PANI) electrocatalyst (PANI-Cu@BSA) was prepared by using a one-step method of biomimetic mineralization and polymerization using bovine serum albumin (BSA) as a stabilizer. Then, the synthesized PANI-Cu@BSA was encapsulated with reduced graphene oxide (rGO) using an ultrasonication method. The PANI-Cu@BSA/rGO nanocomposite had superior water dispersibility, high electrical conductivity, and nanoscale particles. Moreover, a PANI-Cu@BSA/rGO nanocomposite-modified, screen-printed carbon electrode was used for the sensitive electrochemical detection of DMZ. In phosphate buffer solution, the PANI-Cu@BSA/rGO/SPCE displayed a current intensity greater than PANI-Cu@BSA/SPCE, rGO/SPCE, and bare SPCE. This is because PANI-Cu@BSA combined with rGO increases fast electron transfer between the electrode and analyte, and this synergy results in analyte–electrode junctions with extraordinary conductivity and active surface areas. PANI-Cu@BSA/rGO/SPCE had a low detection limit, a high sensitivity, and a linear range of 1.78 nM, 5.96 μA μM−1 cm−2, and 0.79 to 2057 μM, respectively. The selective examination of DMZ was achieved with interfering molecules, and the PANI-Cu@BSA/rGO/SPCE showed excellent selectivity, stability, repeatability, and practicability. [ABSTRACT FROM AUTHOR]

In the current project, the National Institute of Standards (NIS), Egypt, initiated a preliminary investigation to create a certified reference material for certain elements, including Fe, Mg, Mn, Al, Cu, and Zn, in human hair. This reference material would be a quality control sample for trace element determination. This paper studied homogeneity and short-term stability as critical parameters for producing certified reference materials. ICP-OES and AAS were used to measure human hair powder samples, and the data was statistically evaluated for normality and outliers, which resulted in the measurement results being normal after removing the outliers. Also, sample homogeneity was evaluated and assessed using analysis of variance (ANOVA), which revealed that the human hair samples produced were homogenous and stable during transportation. This CRM mainly intends to develop methods and check instrumental performance, analytical trueness, and accuracy related to trace element analysis in human hair and similar matrices. [ABSTRACT FROM AUTHOR]

Cytokines are compounds that belong to a special class of signaling biomolecules that are responsible for several functions in the human body, being involved in cell growth, inflammatory, and neoplastic processes. Thus, they represent valuable biomarkers for diagnosing and drug therapy monitoring certain medical conditions. Because cytokines are secreted in the human body, they can be detected in both conventional samples, such as blood or urine, but also in samples less used in medical practice such as sweat or saliva. As the importance of cytokines was identified, various analytical methods for their determination in biological fluids were reported. The gold standard in cytokine detection is considered the enzyme‐linked immunosorbent assay method and the most recent ones have been considered and compared in this study. It is known that the conventional methods are accompanied by a few disadvantages that new methods of analysis, especially electrochemical sensors, are trying to overcome. Electrochemical sensors proved to be suited for the elaboration of integrated, portable, and wearable sensing devices, which could also facilitate cytokines determination in medical practice. HIGHLIGHTS: Cytokines are signaling molecules involved in numerous medical conditions, therefore their detection is essential;Various biological samples are used to detect cytokines thus it is necessary to correlate between the detected levels. There are numerous analytical methods applied for cytokine analysis;Electrochemical methods offer new perspectives for cytokine determination;Electrochemical sensors are suitable for miniaturization and portable devices fabrication [ABSTRACT FROM AUTHOR]

This study aimed to develop a fast, accurate, and precise high‐performance liquid chromatography with UV detection method for simultaneous analysis of underivatized phenylalanine (Phe) and tyrosine (Tyr) in biological samples. Separation of the analytes was accomplished using a Discovery HS F5‐3 column, which offered better retention and peak symmetry for the tested analytes. Chromatographic conditions were optimized using central composite experimental design, and three factors were investigated: the concentration of ammonium acetate (A), the acetonitrile proportion in the mobile phase (B) and the column oven temperature (C). The approach was verified using β‐expectation tolerance intervals for total error measurement that did not exceed 15%. Optimal settings were A = 50 mm, B = 24% and C = 28°C. The method applicability was determined using human plasma from 75 volunteers. The limits of detection and quantification of the technique were satisfactory at 9 and 29 μm for Phe and 4 and 13 μm for Tyr. The mean analytical bias in spiking levels was acceptable, ranging from −1.649 to +1.659% for both substances, with RSD <5% in all instances. The suggested approach was successfully used to analyze Phe and Tyr in human blood samples and calculate the Phe/Tyr ratio. [ABSTRACT FROM AUTHOR]

Phytoestrogens, natural compounds with structural similarity to 17-β-estradiol, are known to have potential health benefits, including in hormone-dependent malignancies. The therapeutic interest and some safety concerns observed triggered the need to develop accurate methods to assess their level in different matrices. This narrative review examines the existing analytical methods used to isolate, quantify, and characterize phytoestrogens and their metabolites in plants, foods, and biological samples. Different conventional and modern extraction techniques, such as ultrasonication-assisted extraction, supercritical fluid extraction, or enzyme-assisted extraction, were presented and compared. The advantages and limitations of the existing analytical methods, such as high-performance liquid chromatography using different sensitive detectors, gas chromatography often coupled with mass spectrometry, and immunoassay methods, are highlighted, along with the need for ongoing research to improve the sensitivity and selectivity of the analysis.

Aim of this study stands in the evaluation of a carbon nanotubes-based polymerized high internal phase emulsion composite (CNT/polyHIPE) as sorptive phase in biological sample preparation. A micro-solid-phase extraction procedure (µSPE) was developed for trace fluoroquinolone (FQ) antimicrobials, namely Ciprofloxacin, Levofloxacin, Lomefloxacin, Moxifloxacin, Norfloxacin and Sparfloxacin, in human urine samples. PolyHIPEs modified by incorporation of different concentrations of nanotubes (0.2–0.8 wt %) were one-pot synthesized and applied in the packed-cartridge setting. The sorption affinity for the drugs was investigated in tap water and buffered aqueous solutions, demonstrating the key role of the nanotubes embedded in the polymer. The 0.5 wt % CNT composite was selected to develop a straightforward µSPE procedure directly in raw urine (1 mL sample), followed by HPLC-MS/MS. Targets were retained on the sorbent at near neutral pH and, after an aqueous washing (0.1 % v/v formic acid), eluted in a single-step with 4 % v/v ammonia aqueous solution (15 % v/v acetonitrile), thus combining extraction and clean-up. The method allowed accurate quantification of FQs, as evidenced by the recoveries (74–116 %, n = 3) obtained on blank pooled urine samples spiked with 40, 75, 150 µg L−1, accompanied by good inter-day precision (RSD

The transport of temperature-sensitive biological samples (blood, medicines, patient samples, vaccines, organs, etc.) to hard-to-reach places remains a challenge. This is especially true in places where infrastructure is limited, for which the use of unmanned aerial vehicles (UAVs) is an attractive solution. In this project, a cooling system compatible with on-board drone applications for the delivery of samples that require cold temperature storage and transportation was built, tested, and characterized. Specifically, a miniature polystyrene cooling unit with Peltier coolers was designed and built, enabling temperatures as low as −10 °C within the unit to be achieved. Further, passive and active cooling control strategies including the use of active feedback-control were explored to achieve a consistent temperature range between 2 °C and 8 °C. Finally, calculations of on-board power and battery weight required to achieve target cooling performance as a function of ambient environmental conditions are presented. Overall, this study presents an important step towards the design and development of drone-based technologies for temperature-sensitive sample delivery.

The levels of the MMPs in the biological samples of confirmed patients with gastric cancer are significantly elevated compared to those found in healthy people. Therefore, a novel 3D stochastic microsensor based on graphene oxide, modified with gold nanoparticles and (Z)-N-(pyridin-4-yl-methyl) octadec-9-enamide (namely N2-AuNP/GO), was designed for the determination of MMP-2 in biological samples, and validated for the screening tests of biological samples in order to be used for the early diagnosis of gastric cancer. The proposed sensor presents a low limit of quantification (1.00 × 10−22 g mL−1), high sensitivity (1.84 × 107 s−1 g−1 mL), and a wide working concentration range (1.00 × 10−22–1.00 × 10−7 g mL−1). Recovery values higher than 99.15% were recorded for the assay of MMP-2 in whole blood, gastric tissue tumors, saliva, and urine samples.

Proton magnetic resonance spectroscopy (1H MRS) presents a powerful tool for revealing molecular-level metabolite information, complementary to the anatomical insight delivered by magnetic resonance imaging (MRI), thus playing a significant role in in vivo/in vitro biological studies. However, its further applications are generally confined by spectral congestion caused by numerous biological metabolites contained within the limited proton frequency range. Herein, we propose a pure-shift-based 1H localized MRS method as a proof of concept for high-resolution studies of biological samples. Benefitting from the spectral simplification from multiplets to singlet peaks, this method addresses the challenge of spectral congestion encountered in conventional MRS experiments and facilitates metabolite analysis from crowded NMR resonances. The performance of the proposed pure-shift 1H MRS method is demonstrated on different kinds of samples, including brain metabolite phantom and in vitro biological samples of intact pig brain tissue and grape tissue, using a 7.0 T animal MRI scanner. This proposed MRS method is readily implemented in common commercial NMR/MRI instruments because of its generally adopted pulse-sequence modules. Therefore, this study takes a meaningful step for MRS studies toward potential applications in metabolite analysis and disease diagnosis.

One-carbon folate metabolites and one-carbon-related amino acids play an important role in human physiology, and their detection in biological samples is essential. However, poor stability as well as low concentrations and occurrence in different species in various biological samples make their quantification very challenging. The aim of this study was to develop a simple, fast, and sensitive ultra-high-performance liquid chromatography MS/MS (UHPLC–MS/MS) method for the simultaneous quantification of various one-carbon folate metabolites (folic acid (FA), tetrahydrofolic acid (THF), p-aminobenzoyl-L-glutamic acid (pABG), 5-formyltetrahydrofolic acid (5-CHOTHF), 5-methyltetrahydrofolic acid (5-CH3THF), 10-formylfolic acid (10-CHOFA), 5,10-methenyl-5,6,7,8-tetrahydrofolic acid (5,10-CH+-THF), and 4-α-hydroxy-5-methyltetrahydrofolate (hmTHF)) and one-carbon-related amino acids (homocysteine (Hcy), methionine (Met), S-ade-L-homocysteine (SAH), and S-ade-L-methionine (SAM)). The method was standardized and validated by determining the selectivity, carryover, limits of detection, limits of quantitation, linearity, precision, accuracy, recovery, and matrix effects. The extraction methods were optimized with respect to several factors: protease–amylase treatment on embryos, deconjugation time, methanol precipitation, and proteins’ isoelectric point precipitation on the folate recovery. Ten one-carbon folate metabolites and four one-carbon-related amino acids were detected using the UHPLC–MS/MS technique in various biological samples. The measured values of folate in human plasma, serum, and whole blood (WB) lay within the concentration range for normal donors. The contents of each analyte in mouse plasma were as follows: pABG (864.0 nmol/L), 5-CH3THF (202.2 nmol/L), hmTHF (122.2 nmol/L), Met (8.63 μmol/L), and SAH (0.06 μmol/L). The concentration of each analyte in mouse embryos were as follows: SAM (1.09 μg/g), SAH (0.13 μg/g), Met (16.5 μg/g), 5,10-CH+THF (74.3 ng/g), pABG (20.6 ng/g), and 5-CH3THF (185.4 ng/g). A simple and rapid sample preparation and UHPLC–MS/MS method was developed and validated for the simultaneous determination of the one-carbon-related folate metabolites and one-carbon-related amino acids in different biological samples.

Dimetridazole (DMZ) is a derivative of nitroimidazole and is a veterinary drug used as an antibiotic to treat bacterial or protozoal infections in poultry. The residues of DMZ cause harmful side effects in human beings. Thus, we have constructed a superior electrocatalyst for DMZ detection. A copper (Cu)-integrated poly(aniline) (PANI) electrocatalyst (PANI-Cu@BSA) was prepared by using a one-step method of biomimetic mineralization and polymerization using bovine serum albumin (BSA) as a stabilizer. Then, the synthesized PANI-Cu@BSA was encapsulated with reduced graphene oxide (rGO) using an ultrasonication method. The PANI-Cu@BSA/rGO nanocomposite had superior water dispersibility, high electrical conductivity, and nanoscale particles. Moreover, a PANI-Cu@BSA/rGO nanocomposite-modified, screen-printed carbon electrode was used for the sensitive electrochemical detection of DMZ. In phosphate buffer solution, the PANI-Cu@BSA/rGO/SPCE displayed a current intensity greater than PANI-Cu@BSA/SPCE, rGO/SPCE, and bare SPCE. This is because PANI-Cu@BSA combined with rGO increases fast electron transfer between the electrode and analyte, and this synergy results in analyte–electrode junctions with extraordinary conductivity and active surface areas. PANI-Cu@BSA/rGO/SPCE had a low detection limit, a high sensitivity, and a linear range of 1.78 nM, 5.96 μA μM−1 cm−2, and 0.79 to 2057 μM, respectively. The selective examination of DMZ was achieved with interfering molecules, and the PANI-Cu@BSA/rGO/SPCE showed excellent selectivity, stability, repeatability, and practicability.

• Electrochemical sensor was fabricated based on Au@Ce 2 Sn 2 O 7 /MXene nanocomposite. • Au@Ce 2 Sn 2 O 7 /MXene was synthesized by simple hydrothermal and ultrasonication methods. • Differential pulse voltammetry technique was utilized for metol detection. • Developed sensor showed high sensitivity and low limit of detection (5.63 nM). • The practicability of the developed sensor was estimated in various real samples. Metol (MTL) is a highly significant organic compound that plays a crucial role in numerous applications as a monochromatic material. It has an impact on humans, plants, and animals and it raises serious environmental concerns. The present scenario necessitates the development a rapid, cost-effective, precise, and specific method for detecting metol in environmental and biological samples. In this study, the electrochemical sensor was developed using a modified electrode based on the Au@Ce 2 Sn 2 O 7 /MXene nanocomposite. The nanocomposite was thoroughly examined through phase composition analysis, elemental analysis, and morphological studies. The modified electrode exhibits exceptional selectivity, cyclic stability, storage stability, and reproducibility. The proposed sensor shows a wide linearity range (0.00125 to 1021.96 μM), low detection limit (5.63 nM), and high sensitivity (0.403 μA·μM–1·cm–2). The suggested sensor's consistency was confirmed by real-time monitoring of MTL in several environmental and biological samples with a high percentage of recovery. [ABSTRACT FROM AUTHOR]

[Display omitted] • The spectrofluorimetric approach is based on the quenching of Acid red 87 at an acidic medium. • The approach is compatible with green chemistry criteria. • The technique was applied successfully for the assay of eletriptan in dosage form assay and plasma. • The approach was validated in concordance with ICH directives. Eletriptan (ETR), a selective pharmaceutical agent agonist of the 5-hydroxytryptamine1 receptor subtype, are primarily used to treat acute migraine attacks. ETR is a triptan-class medication that works by narrowing cerebral blood vessels and reducing chemicals that produce headache pain, light and sound sensitivity, and nausea. Due to its effectiveness in reducing migraine symptoms, it is a worthwhile choice for those looking for quick and efficient treatment. A green, raid, one-pot and straightforward fluorescence spectrometric method was employed to evaluate ETR in tablets and biological samples. By introducing the ETR drug and the fluorescent ligand, Acid red 87, in an acidic buffer, a quenching of the ligand native fluorescent was promptly produced. The quenching action was simply attributed to the selective ion-pair complex generation between the cationic target and the selected ligand. An increase in ETR concentration was linearly proportional to the quenching response in the 50.0 – 500.0 ng/mL range. The optimal configurations for adjusting the system's variable parameters were determined by examining the ETR–Acid red 87 system's response. Additionally, the sensor that was developed met the standards set by the International Council for Harmonisation of Technical Requirements of Pharmaceuticals for Human Use. The sensitivity thresholds of the approach were 13.8 and 42.0 ng/mL for the detection and quantification parameters, respectively, LOD and LOQ. This approach proficiently evaluated the pharmaceutical and biological samples of ETR. Finally, the proposed approach not only simplifies the analysis process but also limits the bad impact on the environment, making it a promising technique for analytical applications. [ABSTRACT FROM AUTHOR]

There is widespread interest in the design of portable electrochemical sensors for the selective monitoring of biomolecules. Dopamine (DA) is one of the neurotransmitter molecules that play a key role in the monitoring of some neuronal disorders such as Alzheimer's and Parkinson's diseases. Facile synthesis of the highly active surface interface to design a portable electrochemical sensor for the sensitive and selective monitoring of biomolecules (i.e., DA) in its resources such as human fluids is highly required. The designed sensor is based on a three-dimensional phosphorous and sulfur resembling a g-C 3 N 4 hornet's nest (3D-PS-doped CNHN). The morphological structure of 3D-PS-doped CNHN features multi-open gates and numerous vacant voids, presenting a novel design reminiscent of a hornet's nest. The outer surface exhibits a heterogeneous structure with a wave orientation and rough surface texture. Each gate structure takes on a hexagonal shape with a wall size of approximately 100 nm. These structural characteristics, including high surface area and hierarchical design, facilitate the diffusion of electrolytes and enhance the binding and high loading of DA molecules on both inner and outer surfaces. The multifunctional nature of g-C 3 N 4 , incorporating phosphorous and sulfur atoms, contributes to a versatile surface that improves DA binding. Additionally, the phosphate and sulfate groups' functionalities enhance sensing properties, thereby outlining selectivity. The resulting portable 3D-PS-doped CNHN sensor demonstrates high sensitivity with a low limit of detection (7.8 nM) and a broad linear range spanning from 10 to 500 nM. The portable DA sensor based on the 3D-PS-doped CNHN/SPCE exhibits excellent recovery of DA molecules in human fluids, such as human serum and urine samples, demonstrating high stability and good reproducibility. The designed portable DA sensor could find utility in the detection of DA in clinical samples, showcasing its potential for practical applications in medical settings. A portable electrochemical sensor based on the surface functional and activity of 3D-PS-doped CNHN was designed to detect the low levels of dopamine (DA) molecules in human fluids such as human serum and urine samples. The 3D-PS-doped CNHN surface functionality leads to facile binding to the DA molecules and fast redox transfer. These functionalities provide a stable signaling of DA with high sensitivity and selectivity in complex mixtures such as human fluids. The designed sensor could be used widely for monitoring of some neuronal diseases such as Alzheimer's and Parkinson's diseases. [Display omitted] • Controlled synthesis of a novel g-C 3 N 4 structure with facile doping of phosphorous and sulfur atoms was assigned. • A portable electrochemical sensor based on the highly active surface of 3D-PS-doped CNHN was designed. • The surface morphology and chemical composition of 3D-PS-doped CNHN outmost the surface interface functionality. • A sensitive and selective biosensing dopamine assay was designed based on 3D-PS-doped CNHN. • The 3D-PS-doped CNHN shows a highly stable and reproducible portable electrochemical sensor for DA screening in human fluids. [ABSTRACT FROM AUTHOR]

• Sol–gel ionic liquid/Carbowax 20M-based absorbent was fabricated and characterized. • The composite sorbent reduces the necessity of the matrix pH adjustment. • The capsule phase microextraction device was found to be reusable at least 25 times. • The green character of the developed method was assessed. • Urinary analysis of sildenafil after oral administration of the drug-containing formulation. Capsule phase microextraction (CPME) is an efficient bioanalytical technique that streamlines the sample preparation by integrating the filtration and stirring mechanism directly into the device. A novel composite sorbent designed to be selective towards the target analytes consisting of mixed-mode sorbent chemistry synthesized by sol–gel technology is found promising and superior to the conventional C 18 sorbents. Herein we describe the encapsulation of an ionic liquid (IL)/Carbowax 20M-functionalized sol–gel sorbent (sol–gel IL/Carbowax 20 M) in the lumen of porous polypropylene tubes for the capsule phase microextraction of three phosphodiesterase-5 inhibitors namely avanafil, sildenafil, and tadalafil in human serum and urine samples. The CPME device was characterized by Scanning Electron Microscopy (SEM) and Fourier-Transform Infrared Spectroscopy (FT-IR). The experimental parameters of CPME procedure (e.g. sample pH and ionic strength, extraction time, stirring rate, elution solvent and volume) were carefully optimized to achieve the highest possible extraction efficiency for the analytes. Method validation was conducted in terms of precision, linearity, accuracy, matrix effect, lower limits of quantification, and limits of detection (LOD). The method linearity was investigated in the range of 50–1000 ng mL−1 for all analytes while the precision was less than 11.8 % in all cases. For all analytes, the LOD values were 17 ng mL−1. The IL/CW 20M-functionalized microextraction capsules could be reused at least 25 times both for urine and serum samples. The green character and the applicability of the proposed method were evaluated using the ComplexGAPI and BAGI indexes. The optimized CPME protocol exhibited reduced consumption of organic solvent and generation of waste, cost-effectiveness, and simplicity. Finally, the proposed method was successfully applied to the analysis of sildenafil in human urine after administration of drug-containing formulation. [Display omitted] [ABSTRACT FROM AUTHOR]