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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]

Illicit drug use has become a global issue, posing significant health, socioeconomic, and cultural risks. The study examined essential trace metals: selenium, zinc, and copper in blood concentrations, as well as in serum and scalp hair samples, from 240 male drug-abuse subjects/patients aged 18–45, categorized into three age groups. The study compared 45 healthy subjects of the same age group using an acid digestion method supported by a microwave oven during sample preparation. The technique of atomic absorption spectrometry was employed to identify essential and toxic elements, utilizing certified reference materials for accuracy. According to a recent study, plasma zinc and selenium concentrations in drug abusers are lower than those in referent subjects, potentially increasing vulnerability to infection due to poor nutritional status or other contaminants. [ABSTRACT FROM AUTHOR]

The Folin-Ciocalteu method is a well-established and widely used assay for measuring total (poly)phenol content in food/plant products. In recent years, there has been growing interest in applying this method to human samples due to its simplicity and efficacy. However, biological matrices such as blood and urine contain several interference substances that must be eliminated beforehand. This mini-review summarizes the current state of knowledge regarding the use of the Folin-Ciocalteu assay to measure total phenolic content in human urine and blood samples, as well as the preceding cleaning methods to remove interferences. Higher total (poly)phenol levels measured by the Folin-Ciocalteu method have been associated with a decrease in mortality and several risk variables. We focus on the application of this sustainable assay as a biomarker of poly(phenol) intake and its potential use as an anti-inflammatory biomarker in clinical laboratories. The Folin-Ciocalteu method, with a clean-up extraction step, is a reliable tool for determining total (poly)phenol consumption. Here, we also recommend using the Folin-Ciocalteu assay as means to measure anti-inflammatory activity. [ABSTRACT FROM AUTHOR]

A rapid and sensitive dispersive liquid–liquid microextraction (DLLME) method coupled with UV-Vis spectrophotometry has been developed and validated for the determination of metoclopramide in pharmaceutical and biological samples. The method is based on the formation of an ion-pair complex between metoclopramide and cobalt(II) thiocyanate under acidic conditions (pH = 3), followed by DLLME to efficiently preconcentrate the chromogenic complex. In the novel DLLME procedure, methylene chloride was used as the extraction solvent and acetonitrile acted as the dispersive solvent, generating a cloudy heterogeneous mixture upon injection into the aqueous sample. This facilitated extensive interfacial contact and partitioning of the metoclopramide-cobalt complex into the fine dispersed methylene chloride droplets within minutes. After centrifugation, the sedimented organic phase was analyzed at the maximum wavelength of 625 nm. Under optimal conditions, the method permitted quantification of metoclopramide from 0.25–45 µg/mL with high enrichment factors, and LOD of 0.078 µg/mL, LOQ of 0.258 µg/mL and high extraction recoveries in the range of 94–101% were obtained. The proposed DLLME-spectrophotometric methodology provides a simple, rapid and sensitive approach for routine therapeutic monitoring and quality control of metoclopramide in real samples. [ABSTRACT FROM AUTHOR]

A sophisticated electrochemical sensor is presented employing a glassy carbon electrode (GCE) modified with a novel composite of synthesized graphitic carbon nitride (g-C3N4) and CoNiO2 bimetallic oxide nanoparticles (g-C3N4/CoNiO2). The sensor's electrocatalytic capabilities for Sunitinib (SUNI) oxidation were demonstrated exceptional performance with a calculated detection limit (LOD) of 52.0 nM. The successful synthesis and integrity of the composite were confirmed through meticulous characterization using various techniques. FT-IR analysis affirmed the successful synthesis of g-C3N4/CoNiO2 by providing insights into its molecular structure. XRD, FE-SEM, SEM–EDX, and BET analyses collectively validated the material's structural integrity, surface morphology, and electrocatalytic performance. Optimization of key analytical parameters, such as loading volume, concentration, electrolyte solution type, and pH, enhanced the electrocatalytic sensing capabilities of g-C3N4/CoNiO2. The synergistic interaction between g-C3N4 and CoNiO2 bimetallic oxide nanoparticles executed the sensor highly effective in the electrical oxidation of SUNI. Across a concentration range of 0.1–83.8 µM SUNI, the anodic peak current exhibited a linear increase with good precision. Application of the newly developed g-C3N4/CoNiO2 system to detect SUNI in a variety of samples, including urine, human serum, and capsule dosage forms, obtained satisfactory recoveries ranging from 97.1 to 103.0%. This methodology offers a novel approach to underscore the potential of the developed sensor for applications in biological and pharmaceutical monitoring. [ABSTRACT FROM AUTHOR]

Rifampicin is a frontline antibiotic in the management of tuberculosis. Since no spectrofluorimetric methods are reported for this drug, this approach was challenged to craft a sensitive, reliable, valid, fast, and green methodology. In recent years, fluorescence spectroscopy has received a lot of interest. Its benefits include ecological greenness and analytical performance. The pharmaceutical industries greatly like this approach because of its low energy and decreased solvent usage, which make it both economical and environmentally friendly. This methodology was based on utilizing the enhanced native fluorescence of the rifampicin at 341 nm after excitation at 241 nm in a beta‐cyclodextrin micellar system. Modern developments in analytical chemistry have been applied to reduce risks to the workplace and environment by using distilled water as a dilution solvent for method application and optimization. The method was found excellent green with 97 eco‐scale and 0.86 AGREE scores besides an 89.6 overall whiteness score. The range of linearity for rifampicin raw material was 0.2–1.5 μg·mL−1, and the average recoveries for raw material and spiked plasma were 100.15% and 99.64%, respectively. The suggested technique worked well for the commercial oral syrup of Rimactane® and did not conflict with any common additives. [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.

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]

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]

In the criminal process, the evidentiary means are obtained through certain evidentiary procedures, and after performing them, evidence can be obtained regarding the commission of some crimes. The legislator has shown in the criminal procedural provisions as well as in other related special laws the ways in which the physical examination is carried out when it is presumed that a crime has been committed. This examination is performed on the suspect or defendant, on the victim or on other persons who were in the criminal field. The process of physical examination consisting of external and internal examination of a person's body, as well as taking biological samples, can lead to finding out the truth in a criminal case. [ABSTRACT FROM AUTHOR]

Analysis of biological samples containing synthetic cathinones has become a significant area of interest for researchers in recent years, because synthetic cathinones can cause adverse reactions such as delusions and hallucinations. Generally, the intricate nature of the sample matrix and exceedingly low drug concentration in biological samples present significant challenges for the determination of target substances. Accordingly, scientists were dedicated to the advancement of effective sample preparation techniques to address these difficulties. However, the current reviews involved in synthetic cathinones all focused on detection methods. A systematic review focusing on sample preparation for the quantification of synthetic cathinones is still lacking. In light of that, this paper reviewed the most commonly used sample preparation techniques for synthetic cathinones. Recent advances in sample preparation techniques for synthetic cathinones in different biological samples such as blood, urine, oral fluid and hair samples were discussed. In addition, we prospected the challenges and the future perspectives of biological sample preparation techniques for synthetic cathinones determination.

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]

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]

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.)

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]

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

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]

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]

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]

Magnetic dispersive micro solid-phase extraction as a proper and selective sample preparation was developed to extract and clean up three drugs, including Caffeine (CAF), Lidocaine (LID), and Chlorpromazine (CPZ), before determining by HPLC-DAD. Nickel-doped BiFeO3 was synthesised using the sol–gel method as a magnetic sorbent core and coated with tetraethyl orthosilicate (TEOS) to enhance the sorbent stability and the sorbent selectivity. In the extraction procedure, the sorbent was dispersed into acetonitrile as disperser solvent and sodium dodecyl sulphate (SDS) as a disperser agent before injecting into the sample solution to extract the analytes. Several influential factors in the method were evaluated using an experimental design strategy. Under the optimum conditions, the method displayed wide linearity in the concentration ranges of 20.8–365, 1.4–389, and 2.7–355 ng mL−1 to determine CAF, LID, and CPZ with a suitable R2 between 0.9963 and 0.9971, respectively. Intra-day and inter-day relative standard deviations were in the ranges of 3.5–3.8 and 3.9–4.3%. LODs and LOQs for the determination of CAF, LID, and CPZ were lower than 6.3 and 20.8 ng mL−1. The method is convenient for determining the analytes in real water and biological samples with RSD (n = 3) and recovery in the ranges of 3.0–4.3% and 87.5–96.9%, respectively. [ABSTRACT FROM AUTHOR]

AbstractLipid peroxidation occurs when substances, such as reactive oxygen species, attack lipids. Polyunsaturated fatty acids are the main targets. Several products are formed, including primary products such as lipid hydroperoxides and secondary products such as malondialdehyde (MDA), the most used lipid peroxidation biomarker. As MDA levels are elevated in several diseases, MDA is an essential indicator for assessing pathological states. The thiobarbituric acid reactive substances assay is the most widely used method for MDA determination. However, it lacks specificity. Capillary Electrophoresis (CE) is a separation technique that has been used to quantify MDA in biological samples. This technique has advantages such as the low amount of biological sample required, absence or low volume of organic solvent, short analysis time, separation of interferents, sample preparation step with only protein precipitation, and the possibility of direct detection of the MDA, without derivatization. To our knowledge, this review article is the first to show the CE background for analyzing MDA in biological samples. Therefore, given the potential of MDA in evaluating pathological states, this article demonstrates the potential of CE to become a reference method for MDA determination in clinical analysis laboratories, which will play a significant role in diagnosing and monitoring diseases. [ABSTRACT FROM AUTHOR]

Simple Summary: Biobanks belong to the highly organized infrastructures of research institutions and clinics which allow the storage of patients' biological material, thus constituting an essential tool for performing translational research aiming at the discovery of prognostic and predictive biomarkers. Although hundreds of biomarkers have been reported in the literature, only a few of them have been confirmed and validated for their specificity and sensitivity and, subsequently, have become clinically applicable. The main reason for this is the biological specimens' lack of quality, which is essential for obtaining reliable and reproducible results from their analysis. In this review, we discuss some important issues that need to be met during biobanking to enhance the contribution of biomarkers to translational and clinical cancer research. Cancer biobanks have a crucial role in moving forward the field of translational cancer research and, therefore, have been promoted as indispensable tools for advancing basic biomedical research to preclinical and clinical research, ultimately leading to the design of clinical trials. Consequently, they play an essential role in the establishment of personalized oncology by combining biological data with registries of detailed medical records. The availability of complete electronic medical reports from individualized patients has led to personalized approaches for diagnosis, prognosis, and prediction. To this end, identifying risk factors at early time points is important for designing more effective treatments unique for each patient. Under this aspect, biobanking is essential for accomplishing improvements in the field of precision oncology via the discovery of biomarkers related to cellular and molecular pathways regulating oncogenic signaling. In general terms, biological samples are thought to reflect the patient's disease biology, but under certain conditions, these may also represent responses to various biological stresses. Divergent collection, handling, and storage methods may significantly change biosamples' inherent biological properties. The alteration or loss of biological traits post-collection would lead to the discovery of nonreliable biomarkers and, consequently, to irreproducible results, thus constituting a formidable obstacle regarding the successful translation of preclinical research to clinical approaches. Therefore, a necessary prerequisite for successful biobanking is that the stored biological samples retain their biological characteristics unchanged. The application of quality standards for biospecimen collection and storage could be useful for generating encouraging preclinical data leading to the successful translation to clinical treatment approaches. Herein, we aim to comprehensively review the issues linked to biobank implementation for promoting cancer research. [ABSTRACT FROM AUTHOR]

Bio-SELEX is a revolutionary method for the discovery of novel biomarkers within biological samples, offering profound insights into diagnosing both infectious and non-infectious diseases. This innovative strategy involves three crucial steps: Traditional SELEX, Pull Down, and mass spectrometry. Firstly, Traditional SELEX involves the systematic selection of specific nucleic acid sequences (aptamers) that bind to the target molecules of interest. These aptamers are generated through iterative rounds of selection, amplification, and enrichment, ultimately yielding highly selective ligands. Secondly, the Pull-Down phase employs these aptamers to capture and isolate the target biomarkers from complex biological samples. This step ensures the specificity of the selected aptamers in binding to their intended targets. Lastly, mass spectrometry is utilized to identify and quantify the captured biomarkers, providing precise information about their presence and concentration in the sample. These quantitative data are invaluable in disease diagnosis and monitoring. Bio-SELEX's significance lies in its ability to discover biomarkers for a wide range of diseases, spanning infectious and non-infectious conditions. This approach holds great promise for early disease detection, personalized medicine, and the development of targeted therapies. By harnessing the power of aptamers and mass spectrometry, Bio-SELEX advances our understanding of disease biology and opens new avenues for improved healthcare. [ABSTRACT FROM AUTHOR]

Cancer biobanks have a crucial role in moving forward the field of translational cancer research and, therefore, have been promoted as indispensable tools for advancing basic biomedical research to preclinical and clinical research, ultimately leading to the design of clinical trials. Consequently, they play an essential role in the establishment of personalized oncology by combining biological data with registries of detailed medical records. The availability of complete electronic medical reports from individualized patients has led to personalized approaches for diagnosis, prognosis, and prediction. To this end, identifying risk factors at early time points is important for designing more effective treatments unique for each patient. Under this aspect, biobanking is essential for accomplishing improvements in the field of precision oncology via the discovery of biomarkers related to cellular and molecular pathways regulating oncogenic signaling. In general terms, biological samples are thought to reflect the patient’s disease biology, but under certain conditions, these may also represent responses to various biological stresses. Divergent collection, handling, and storage methods may significantly change biosamples’ inherent biological properties. The alteration or loss of biological traits post-collection would lead to the discovery of nonreliable biomarkers and, consequently, to irreproducible results, thus constituting a formidable obstacle regarding the successful translation of preclinical research to clinical approaches. Therefore, a necessary prerequisite for successful biobanking is that the stored biological samples retain their biological characteristics unchanged. The application of quality standards for biospecimen collection and storage could be useful for generating encouraging preclinical data leading to the successful translation to clinical treatment approaches. Herein, we aim to comprehensively review the issues linked to biobank implementation for promoting cancer research.

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.