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Synthetic cannabinoid receptor agonists (SCRAs) are a class of synthetic drugs that mimic and greatly surpass the effect of recreational cannabis. Acute SCRA intoxications are in general difficult to assess due to the large number of compounds involved, differing widely in both chemical structure and pharmacological properties. The rapid pace of emergence of unknown SCRAs hampers on one hand the timely availability of methods for identification and quantification to confirm and estimate the extent of the SCRA intoxication. On the other hand, lack of knowledge about the harm potential of emerging SCRAs hampers adequate interpretation of serum concentrations in intoxication cases. In the present study, a novel comparative measure for SCRA intoxications was evaluated, focusing on the cannabinoid activity (versus serum concentrations), which can be measured in serum extracts with an untargeted bioassay assessing ex vivo CB1 activity. Application of this principle to a series of SCRA intoxication cases (n = 48) allowed for the determination of activity equivalents, practically entailing a conversion from different SCRA serum concentrations to a JWH-018 equivalent. This allowed for the interpretation of both mono- (n = 34) and poly-SCRA (n = 14) intoxications, based on the intrinsic potential of the present serum levels to exert cannabinoid activity (cf. pharmacological/toxicological properties). A non-distinctive toxidrome was confirmed, showing no relation to CB1 activity. The JWH-018 equivalent was partly related to the poison severity score (PSS) and causality of the clinical intoxication elicited by the SCRA. Altogether, this equivalent concept allows to comparatively and timely interpret (poly-)SCRA intoxications based on CB1 activity. [ABSTRACT FROM AUTHOR]

The toxicologist ascertains drug assumptions in case of paediatric intoxications and death for overdose. The analytical approach consists of initially screening and consequently confirming drug positivity. We developed a toxicological screening method and validated its use comparing the results with a LC–MS/MS analysis. The method identifies 751 drugs and metabolites (704 in positive and 47 in negative mode). Chromatographic separation was achieved eluting mobile phase A (10 mM ammonium formate) and B (0.05% formic acid in methanol) in gradient on Kinetex Phenyl-Hexyl (50 × 4.6 mm, 2.6 μm) with 0.7 mL/min flow rate for 11 min. Multiple Reaction Monitoring (MRM) was adopted as survey scan and, after an Information-Dependent Analysis (IDA) (threshold of 30,000 for positive and 1000 cps for negative mode), the Enhanced Product Ion (scan range: 50–700 amu) was triggered. The MS/MS spectrum generated was compared with one of the libraries for identification. Data processing was optimised through creation of rules. Sample preparation, mainly consisting of deproteinization and enzymatic hydrolysis, was set up for different matrices (blood, urine, vitreous humor, synovial fluid, cadaveric tissues and larvae). Cut-off for most analytes resulted in the lowest concentration tested. When the results from the screening and LC–MS/MS analysis were compared, an optimal percentage of agreement (100%) was assessed for all matrices. Method applicability was evaluated on real paediatric intoxications and forensic cases. In conclusion, we proposed a multi-targeted, fast, sensitive and specific MRM-IDA-EPI screening having an extensive use in different toxicological fields. [ABSTRACT FROM AUTHOR]

Abstract Recently, phytochemicals play an important role in cancer management. Curcumin (CUR), a natural phytochemical, has been co-administered with widespread chemotherapeutic agents such as doxorubicin (DOX) due to its excellent antitumor activity and the ability to lower the adverse reactions and drug resistance cells associated with DOX use. The present study aims to determine DOX and CUR utilizing a label-free, selective, sensitive, and precise synchronous spectrofluorimetric method. The obvious overlap between the emission spectra of DOX and CUR prevents simultaneous estimation of both analytes by conventional spectrofluorimetry. To solve such a problem, synchronous spectrofluorimetric measurements were recorded at Δλ = 20 nm, utilizing ethanol as a diluting solvent. Curcumin was recorded at 442.5 nm, whereas DOX was estimated at 571.5 nm, each at the zero-crossing point of the other one. The developed method exhibited linearity over a concentration range of 0.04–0.40 μg/mL for CUR and 0.05–0.50 μg/mL for DOX, respectively. The values of limit of detection (LOD) were 0.009 and 0.012 µg/mL, while the values of limit of quantitation (LOQ) were 0.028 and 0.037 µg/mL for CUR and DOX, respectively. The adopted approach was carefully validated according to the guidelines of ICH Q2R1. The method was utilized to estimate CUR and DOX in laboratory-prepared mixtures and human biological matrices. It showed a high percentage of recoveries with minimal RSD values. Additionally, three different tools were utilized to evaluate the greenness of the proposed approach.

Recently, phytochemicals play an important role in cancer management. Curcumin (CUR), a natural phytochemical, has been co-administered with widespread chemotherapeutic agents such as doxorubicin (DOX) due to its excellent antitumor activity and the ability to lower the adverse reactions and drug resistance cells associated with DOX use. The present study aims to determine DOX and CUR utilizing a label-free, selective, sensitive, and precise synchronous spectrofluorimetric method. The obvious overlap between the emission spectra of DOX and CUR prevents simultaneous estimation of both analytes by conventional spectrofluorimetry. To solve such a problem, synchronous spectrofluorimetric measurements were recorded at Δλ = 20 nm, utilizing ethanol as a diluting solvent. Curcumin was recorded at 442.5 nm, whereas DOX was estimated at 571.5 nm, each at the zero-crossing point of the other one. The developed method exhibited linearity over a concentration range of 0.04–0.40 μg/mL for CUR and 0.05–0.50 μg/mL for DOX, respectively. The values of limit of detection (LOD) were 0.009 and 0.012 µg/mL, while the values of limit of quantitation (LOQ) were 0.028 and 0.037 µg/mL for CUR and DOX, respectively. The adopted approach was carefully validated according to the guidelines of ICH Q2R1. The method was utilized to estimate CUR and DOX in laboratory-prepared mixtures and human biological matrices. It showed a high percentage of recoveries with minimal RSD values. Additionally, three different tools were utilized to evaluate the greenness of the proposed approach. [ABSTRACT FROM AUTHOR]

A novel graphene-modified molecularly imprinted polymer-based electrochemical sensor (MIP/RGO-GCE) was developed for the sensitive and selective detection of sibutramine in sports doping control. The sensor was fabricated by electropolymerizing o-phenylenediamine on a reduced graphene oxide-modified glassy carbon electrode in the presence of sibutramine as the template molecule. Under optimized conditions, the MIP/RGO-GCE sensor exhibited a wide linear range (0.05 to 20 μM), low detection limit (0.02 μM), high sensitivity (1.27 μA/μM), good precision (RSD < 2.7%), and long-term stability (93.5% retention after two weeks). The sensor's applicability was successfully demonstrated by analyzing spiked human urine and serum samples, with recoveries ranging from 95.8 to 103.2% and good agreement with the reference HPLC method. Furthermore, the sensor showed a rapid response time of 5 s and excellent reproducibility with an RSD of 1.5% for repeated measurements. The proposed sensor offers a rapid, cost-effective, and reliable alternative to traditional chromatographic methods for sibutramine detection in sports doping control. [ABSTRACT FROM AUTHOR]

Essential trace minerals are vital for general human health and athletic performance. Zinc (Zn) plays critical roles in several biochemical processes in exercise physiology, especially during intense physical exercise. This research aimed to analyze erythrocyte, platelet, plasma and urine Zn concentrations among men's and female soccer players over a sports season. A total of 22 male soccer players (20.61 ± 2.66 years; 71.50 ± 5.93 kg) and 24 female soccer players (23.37 ± 3.95 years; 59.58 ± 7.17 kg) participated in this longitudinal quasi-experimental study. Three assessments were carried out over the season: 1st evaluation: first week of training (August); 2nd assessment: middle of the season, between the end of the first and second round (January) and 3rd assessment: last week of training (May/June). In all evaluations extracellular (plasma and urine) and intracellular (erythrocytes and platelets) Zn concentrations were determined, as well as physical fitness and several blood parameters. Inductively coupled plasma mass spectrometry was used to measure Zn concentrations. Plasma and urinary concentrations were higher among male soccer players (p < 0.05) while erythrocyte and platelet Zn concentrations were higher in the female soccer players (p < 0.05). Additionally, variations in urinary and platelet Zn concentrations were observed over the season. The differences could be related to muscle mass, muscle damage or the specific sport's physical demands. [ABSTRACT FROM AUTHOR]

AbstractPsychoactive substances pose significant challenges and dangers to society due to their impact on perception, mood, and behavior, leading to health and life disturbances. The consumption of these substances is largely influenced by their legal status, cultural norms, and religious beliefs. Continuous development and chemical modifications of psychoactive substances complicate their control, detection, and determination in the human body. This paper addresses the terminological distinctions between psychoactive and psychotropic substances and drugs. It provides a comprehensive review of analytical methods used to identify and quantify 25 psychoactive substances in various biological matrices, including blood, urine, saliva, hair, and nails. The analysis categorizes these substances into four primary groups: stimulants, neuroleptics, depressants, and hallucinogens. The study specifically focuses on chromatographic and spectrophotometric methods, as well as other novel analytical techniques. Methodology includes a review of scientific articles containing validation studies of these methods and innovative approaches to psychoactive substance determination. Articles were sourced from the PubMed database, with most research originating from the twenty first century. The paper discusses the limits of detection and quantitation for each method, along with current trends and challenges in the analytical determination of evolving psychoactive substances. [ABSTRACT FROM AUTHOR]

This study examined levels of lead (Pb), cadmium (Cd), chromium (Cr), copper (Cu), mercury (Hg), and arsenic (As) in blood, hair, and nails of 18 brick kiln workers from three brick kiln units located around a metropolitan city, Lahore, Pakistan. All the trace elements except Hg and As were detected in the studied matrices of Brick kiln workers. In general, brick kiln workers reflect the highest concentration of Pb, followed by Cd, Cr, and Cu. Of the pollutants analyzed, Pb has the highest mean (min–max) concentrations at 0.35 (0.09–0.65) in blood (μg/mL), 0.34 (0.14–0.71) in hairs (μg/g), and 0.44 (0.32–0.59) in nails (μg/g) of brick kiln workers. Following Pb, the trend was Cd 0.17 (0.10–0.24), Cu 0.11(0.03–0.27), and Cr 0.07 (0.04–0.08) in blood (μg/mL), followed by Cr 0.11(0.05–0.20), Cd 0.09 (0.03–0.13), and Cu 0.08 (0.04–0.16) in hairs (μg/g) and Cu 0.16 (0.05–0.36), Cd 0.13 (0.11–0.17), and Cr 0.10 (0.05–0.14) in nails (μg/g) respectively. Relatively higher concentrations of metals and other trace elements in blood depicts recent dietary exposure. The difference of trace elements except Pb was non-significant (P > 0.05) among studied matrices of workers as well as between Zigzag and traditional exhaust-based brick kilns. The concentrations of Pb, Cd and Cr in blood of brick kilns workers are higher than the values reported to cause health problems in human populations. It is concluded that chronic exposure to metals and other trace elements may pose some serious health risks to brick kiln workers which needs to be addressed immediately to avoid future worst-case scenarios. [ABSTRACT FROM AUTHOR]

In 2023, hexahydrocannabinol (HHC) attracted the attention of international agencies due to its rapid spread in the illegal market. Although it was discovered in 1940, less is known about the pharmacology of its two naturally occurring epimers, 9(R)-HHC and 9(S)-HHC. Thus, we aimed to investigate the disposition of hexahydrocannabinol epimers and their metabolites in whole blood, urine and oral fluid following a single controlled administration of a 50:50 mixture of 9(R)-HHC and 9(S)-HHC smoked with tobacco. To this end, six non-user volunteers smoked 25 mg of the HHC mixture in 500 mg of tobacco. Blood and oral fluid were sampled at different time points up to 3 h after the intake, while urine was collected between 0 and 2 h and between 2 and 6 h. The samples were analyzed with a validated HPLC-MS/MS method to quantify 9(R)-HHC, 9(S)-HHC and eight metabolites. 9(R)-HHC showed the highest Cmax and AUC0–3h in all the investigated matrices, with an average concentration 3-fold higher than that of 9(S)-HHC. In oral fluid, no metabolites were detected, while they were observed as glucuronides in urine and blood, but with different profiles. Indeed, 11nor-9(R)-HHC was the most abundant metabolite in blood, while 8(R)OH-9(R) HHC was the most prevalent in urine. Interestingly, 11nor 9(S) COOH HHC was detected only in blood, whereas 8(S)OH-9(S) HHC was detected only in urine. [ABSTRACT FROM AUTHOR]

This review aims to bring together the works on pesticide analysis in alternative biological matrices, such as hair, breast milk, meconium, and placenta. Much is known about the harmful effects of the use and indirect consumption of pesticides; however, the assessment of long-term contamination is still unclear. In this sense, the use of hair as an alternative biological matrix has some advantages, such as segmentation, which makes it possible to assess the presence of xenobiotics to which individuals have been exposed over the years, and possibly relate this exposure to symptoms or diseases that may affect them. Complementarily, the other matrices discussed are able to provide information about the exposure of mothers and newborn children, who may have been indistinctly exposed to pesticides while in the womb. Through the analysis of studies already performed, it can be observed that organochlorine pesticides (OCPs) are the most likely to be found within the biological matrices discussed here, due to the lipophilic characteristics of these compounds. For the other classes, biotransformation products are more easily detected. [ABSTRACT FROM AUTHOR]

Recently, the scope, regulation, legislation, and metrology of the analytical chemistry of engineered nanomaterials (ENMs) have been reviewed in the Part 1 of the IUPAC Technical Report. Chemical analysis of nanomaterials in complex sample matrices presents a substantial challenge for analytical science and regulatory agencies. The purpose of the present Part 2 is to discuss the detection, characterization, and quantification of nanomaterials in samples of complex matrices including methods for sample preparation and fitness for purpose. Analytical methods applied to analysis in matrices of environmental samples, food, cosmetics, and biological samples as well as those used to monitor the fate of ENMs in the environment and biological systems are reported. Tables of numerous recently published works on analyses of typical ENMs with detailed protocols and conclusive comments are presented. There is a rapid development in the field mostly in the stage of accumulation of factual material. The single-particle inductively coupled plasma mass spectrometry is already widely used at the chemical analysis of metal-containing nanoparticles. [ABSTRACT FROM AUTHOR]

Benzodiazepines (BDZs) are used in clinics for anxiolysis, anticonvulsants, sedative hypnosis, and muscle relaxation. They have high consumptions worldwide because of their easy availability and potential addiction. They are often used for suicide or criminal practices such as abduction and drug-facilitated sexual assault. The pharmacological effects of using small doses of BDZs and their detections from complex biological matrices are challenging. Efficient pretreatment methods followed by accurate and sensitive detections are necessary. Herein, pretreatment methods for the extraction, enrichment, and preconcentration of BDZs as well as the strategies for their screening, identification, and quantitation developed in the past five years have been reviewed. Moreover, recent advances in various methods are summarized. Characteristics and advantages of each method are encompassed. Future directions of the pretreatment and detection methods for BDZs are also reviewed.

Per- and polyfluoroalkyl substances (PFAS) present interesting features for several applications and have great commercial relevance. However, PFAS bioaccumulate, persist in the environment, and are toxic, so regulating and controlling their use and evaluating the risks of human exposure to them is vital. Liquid chromatography with tandem mass spectrometry (LC–MS/MS) has been employed to analyze PFAS, especially in biomonitoring studies. Unfortunately, these studies have been met with challenges, such as the low PFAS concentrations in the samples, small sample amount, contamination of labware and reagents, and signal suppression due to the sample matrix. A suitable sample preparation method could preconcentrate PFAS in the sample and remove the matrix before chromatographic analysis, thereby helping to overcome these challenges. Moreover, the right sample preparation method could reduce the analysis time and enhance the selectivity and sensitivity achieved with HPLC–MS/MS and other correlated techniques. Solid Phase Extraction (SPE) is the most common sample preparation technique. SPE is usually employed with protein precipitation (PPT) in multistep sample preparation methods. Nevertheless, depending on the sample type and composition, presence of contaminants, and analytes, other sample preparation techniques may be relevant. In this paper, we provide a critical review of the sample preparation techniques applied for PFAS analysis in biological matrices. We exploit the benefits, challenges, and future perspectives of these techniques.

Depression is one of the most prevalent but severe of mental disorders, affecting thousands of individuals across the globe. Depression, in its most extreme form, may result in self-harm and an increased likelihood of suicide. Antidepressant drugs are first-line medications to treat mental disorders. Unfortunately, these medications are also prescribed for other in- and off-label conditions, such as deficit/hyperactivity disorders, attention disorders, migraine, smoking cessation, eating disorders, fibromyalgia, pain, and insomnia. This results in an increase in the use of antidepressant medications, leading to clinical and forensic overdose cases that could be either accidental or deliberate. The findings revealed that people who used antidepressants had a 33% greater chance of dying sooner than expected, compared to those who did not take the medications. Analytical techniques for precisely identifying and detecting antidepressants and their metabolic products in a variety of biological matrices are greatly needed to be developed and made available. Hence, this study attempts to discuss various analytical techniques used to identify and determine antidepressants in various biological matrices, which include urine, blood, oral fluid (saliva), and tissues, which are commonly encountered in clinical and forensic science laboratories. [ABSTRACT FROM AUTHOR]

Knowledge of the stability of analytes in solvents and biological matrices is of high importance in the field of forensic toxicology. This is particularly true where quantitative analysis is undertaken; degradation of analytes will result in under-estimation of concentrations, whereas the production of analytes/ metabolites will lead to over-estimation. Although stability is included as part of method validation, this typically focuses on processed sample stability, and the impact of freeze/thaw cycles upon analytes. Although beneficial for method evaluation, this does not assist laboratory analysts with the short- and long-term storage of samples prior to this step and does not consider the impact the biological matrix may have on the degradation or production of the analyte in question. The timeframe for these studies is also relatively short (typically 72 h), which does not cover the time frame between sample receivership and analysis for many forensic cases. This review collects previously published work on long-term stability studies, grouping compounds into their associated drug classes and matrices. Research shows that the majority of compounds are more stable at lower storage temperatures, and that analysis should be completed as quickly as possible. It is advised that analyte stability be considered prior to any interpretation of concentrations in a forensic setting. This article is categorized under: Toxicology > Analytical Toxicology > Drug Analysis Toxicology > Drug Stability [ABSTRACT FROM AUTHOR]

Benzodiazepines (BDZs) are used in clinics for anxiolysis, anticonvulsants, sedative hypnosis, and muscle relaxation. They have high consumptions worldwide because of their easy availability and potential addiction. They are often used for suicide or criminal practices such as abduction and drug-facilitated sexual assault. The pharmacological effects of using small doses of BDZs and their detections from complex biological matrices are challenging. Efficient pretreatment methods followed by accurate and sensitive detections are necessary. Herein, pretreatment methods for the extraction, enrichment, and preconcentration of BDZs as well as the strategies for their screening, identification, and quantitation developed in the past five years have been reviewed. Moreover, recent advances in various methods are summarized. Characteristics and advantages of each method are encompassed. Future directions of the pretreatment and detection methods for BDZs are also reviewed. [Display omitted] • Progress on BDZ pretreatments regarding new technologies and materials was emphasized. • Pros and cons of preprocessing procedures for BDZs were summarized. • HRMS methods for BDZs detections were presented. • Future trends in BDZs pretreatments and detections were discussed. [ABSTRACT FROM AUTHOR]

The treatment of biological samples, especially from complex matrices, has consistently challenged analytical operators. The classic problems to be faced for any analysis, regardless of the origin of the sample, such as for example contamination and loss of analyte, in biological samples, are particularly emphasized. In particular, the main cause of the error is due to the degradation of the analyte which in several cases due to biological interaction. Many factors can influence the stability of drugs, chief among them the physicochemical properties of the drug, characteristics of the matrix, the tendency to conjugation/deconjugation, sample collection procedure, container characteristics (e.g., oxidation, adsorption), and the use of preservatives or other additives. The problem is severe in the toxicological and forensic fields, especially for analyzes considered ''non-repeatable.'' In this review, we will explore all the major problems in the pre-extraction phase for the chemical-analytical aspect in the pharmacotoxicological and forensic fields.

One of the most discussed topics concerns the sample preparation before the analysis and, therefore, all the operations necessary to eliminate the interferents, clean up the specimens, and extract the analytes of interest, reducing the matrix effect. This review highlights the fundamental steps in the treatment of postmortem samples used in forensic analysis. Through critical literature research, it was possible to choose among the countless works that could provide a general overview of the state-of-the-art in this field. Different biological matrices have been considered; blood and urine (the traditional biological fluids) are used to investigate the presence of substances that may have caused death, whilst other body fluids, such as bile and oral fluids, are still under discussion for their usability (and suitability). In the second part of the review, all the solid matrices obtained after autopsy were further divided into conventional and unconventional matrices to facilitate proper understanding. The choice of literature was also made according to the most widely used pretreatment techniques and the most representative innovative techniques. [ABSTRACT FROM AUTHOR]

Celecoxib, a cyclooxygenase-2 inhibitor (COX-2), is attracting considerable interest owing to its potential anticancer activity. The repurposing strategy of this drug, however, requires preclinical assessment involving the use of increasingly improved analytical methods. In this work, a rapid, accurate, precise, and sensitive reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed for the quantification of celecoxib in five mouse matrices (plasma, brain, spleen, liver, and kidney). Chromatographic separation was achieved within 8 min on a reversed-phase C18 column at 35 °C using a mixture of acetonitrile and 2% (v/v) acetic acid (50:50) as mobile phase, at a flow rate of 0.6 mL/min. Celecoxib and curcumin, as the internal standard, were analyzed at 425 nm and 250 nm, respectively. Linearity was observed (r2 ≥ 0.996) in the concentration ranges selected for celecoxib. Overall precision was below 14.9%, and accuracy was between −14.9% and 13.2%. The acceptance criteria specified in FDA and EMA guidelines were met. Celecoxib was reproducibly recovered (≥84%) and showed stability in all biological matrices at room temperature for 24 h. The method was then effectively applied for the quantification of celecoxib to understand in vivo biodistribution following its intraperitoneal administration in mice. [ABSTRACT FROM AUTHOR]

Mitoxantrone (MXN) is a synthetic anthracenedione oncogenic therapy. It is often prescribed as an anticancer agent to manage a variety of cancers. A green, fast, and easy fluorimetric technique for the assay of MXN as a topoisomerase type II enzyme suppressor. An investigation of MXN's fluorescence behavior in various media and solvents constituted the basis for this new technique. Methanol was shown to enhance the intrinsic fluorescence considerably. After excitation at 610 nm, the highest fluorescence intensity was found at 675 nm. Various experimental parameters, such as media, solvents, and pH levels, were tested and adjusted. ICH (International Conference on Harmonization) guidelines were followed when validating procedures. It was possible to achieve linearity in the 0.02–1.50 μg ml−1 with the method. The sensitivity (in terms of limit of detection and limit of quantification) was 0.003 and 0.008 μg ml−1, indicating low toxicity. As a result, the current technology has a remarkable recovery for detecting residues in diverse bodily fluids. Also, the quantum yield was estimated for the designed system. Finally, the method was rated by eco‐scale scoring. [ABSTRACT FROM AUTHOR]

Background: Sevoflurane is a polyfluorinated compound extensively used as an inhalation anesthetic in patients undergoing surgery. If administered outside the operating room, sevoflurane is dangerous and potentially lethal, and toxicologists may be asked to investigate its presence in biological matrices for forensic purposes. The aim of the present study is to develop and validate a method for the detection and the quantification of sevoflurane in biological fluids and organs through gas chromatography coupled to flame ionization detection (GC–FID). Methods: The method was optimized based on the maximization of the signal-to-noise ratio. The GC–FID instrument was equipped with a Zebron capillary column ZB-624 (30 m, 0.32 mm ID, 1.80 µm film thickness). Results: The method was validated over a concentration range of 1.0–304.0 µg/mL (blood and urine) and µg/g (brain, lungs). The lower limit of quantitation was 1.0 µg/mL or µg/g. Both the intra- and interassay imprecision and inaccuracy were ≤15% at all quality control concentrations in all the matrices. The method was successfully applied to measure the sevoflurane concentrations for 20 negative controls and for a real forensic case. Conclusions: The present method is suitable for the identification and quantification of sevoflurane in fluids and organs and can be a reliable tool in forensic casework. [ABSTRACT FROM AUTHOR]

Benzisothiazolinone (BIT), a biocide widely used as a preservative in household cleaning and personal care products, is cytotoxic to lung cells and a known skin allergen in humans, which highlights the importance of assessing its toxicity and pharmacokinetics. In this study, a simple, sensitive, and accurate LC–MS/MS method for the quantification of BIT in rat plasma, urine, or tissue homogenates (50 μL) using phenacetin as an internal standard was developed and validated. Samples were extracted with ethyl acetate and separated using a Kinetex phenyl–hexyl column (100 × 2.1 mm, 2.6 μm) with isocratic 0.1% formic acid in methanol and distilled water over a run time of 6 min. Positive electrospray ionization with multiple reaction monitoring transitions of m/z 152.2 > 134.1 for BIT and 180.2 > 110.1 for phenacetin was used for quantification. This assay achieved good linearity in the calibration ranges of 2–2000 ng/mL (plasma and urine) and 10–1000 ng/mL (tissue homogenates), with r ≥ 0.9929. All validation parameters met the acceptance criteria. BIT pharmacokinetics was evaluated via an intravenous and dermal application. This is the first study that evaluated BIT pharmacokinetics in rats, providing insights into the relationship between BIT exposure and toxicity and a basis for future risk assessment studies in humans. [ABSTRACT FROM AUTHOR]

Aflatoxins (AFs) frequently contaminate food and animal feeds, especially in (sub) tropical countries. If animals consume contaminated feeds, AFs (mainly aflatoxin B1 (AFB1), B2 (AFB2), G1 (AFG1), G2 (AFG2) and their major metabolites aflatoxin M1 (AFM1) and M2 (AFM2)) can be transferred to edible tissues and products, such as eggs, liver and muscle tissue and milk, which ultimately can reach the human food chain. Currently, the European Union has established a maximum level for AFM1 in milk (0.05 µg kg−1). Dietary adsorbents, such as bentonite clay, have been used to reduce AFs exposure in animal husbandry and carry over to edible tissues and products. To investigate the efficacy of adding bentonite clay to animal diets in reducing the concentration of AFB1, AFB2, AFG1, AFG2, and the metabolites AFM1 and AFM2 in animal-derived foods (chicken muscle and liver, eggs, and cattle milk), chicken and cattle plasma and cattle ruminal fluid, a sensitive and selective ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method has been developed. High-throughput sample preparation procedures were optimized, allowing the analysis of 96 samples per analytical batch and consisted of a liquid extraction using 1% formic acid in acetonitrile, followed by a further clean-up using QuEChERS (muscle tissue), QuEChERS in combination with Oasis® Ostro (liver tissue), Oasis® Ostro (egg, plasma), and Oasis® PRiME HLB (milk, ruminal fluid). The different procedures were validated in accordance with European guidelines. As a proof-of-concept, the final methods were used to successfully determine AFs concentrations in chicken and cattle samples collected during feeding trials for efficacy and safety evaluation of mycotoxin detoxifiers to protect against AFs as well as their carry-over to animal products. [ABSTRACT FROM AUTHOR]

Midregional proadrenomedullin (MR-proADM) has been shown to play a key role in endothelial dysfunction, with increased levels helping to prevent early stages of organ dysfunction. Recent clinical evidence has demonstrated MR-proADM to be a helpful biomarker to identify disease severity in patients with sepsis as well as pneumonia. This biomarker is helpful at triage in emergency departments to assess risk level of patients. The aim of this study is to evaluate the stability of MR-proADM in different biological matrices. The results, obtained by Bland-Altman and scatter plot analyses, demonstrate that deviation of MR-proADM concentration in serum compared to EDTA plasma unequivocally shows that serum should not be used as a sample matrix. Instead, the excellent correlation of heparin plasma vs EDTA plasma samples shows that heparin plasma can be used without reservation in clinical routine and emergency samples. [ABSTRACT FROM AUTHOR]

Purpose: The present review aims to provide an overview of methods for the quantification of 2,5-dimethoxy-amphetamines and -phenethylamines in different biological matrices, both traditional and alternative ones. Methods: A complete literature search was carried out with PubMed, Scopus and the World Wide Web using relevant keywords, e.g., designer drugs, amphetamines, phenethylamines, and biological matrices. Results: Synthetic phenethylamines represent one of the largest classes of "designer drugs", obtained through chemical structure modifications of psychoactive substances to increase their pharmacological activities. This practice is also favored by the fact that every new synthetic compound is not considered illegal by existing legislation. Generally, in a toxicological laboratory, the first monitoring of drugs of abuse is made by rapid screening tests that sometimes can occur in false positive or false negative results. To reduce evaluation errors, it is mandatory to submit the positive samples to confirmatory methods, such as gas chromatography or liquid chromatography combined to mass spectrometry, for a more specific qualitative and quantitative analysis. Conclusions: This review highlights the great need for updated comprehensive analytical methods, particularly when analyzing biological matrices, both traditional and alternative ones, for the search of newly emerging designer drugs. [ABSTRACT FROM AUTHOR]

This review highlights recent advances in the bioanalysis of cephalosporins using liquid chromatographic methods, focusing on green sample preparation (GSP) techniques. Cephalosporins, a class of β-lactam antibiotics, are critical in combating bacterial infections but present challenges related to drug resistance and toxicity. This article evaluates various sample preparation methods, including solid-phase extraction, solid-phase microextraction, and protein precipitation, which have been employed in the extraction and quantification of cephalosporins from biological matrices. Special attention is given to the optimization of critical parameters, such as pH, extraction solvents, and purification techniques to maximize analytes' recovery and sensitivity. Emerging trends in GSP, such as the use of molecularly imprinted polymers and miniaturized processing devices, are also discussed. The review underscores the growing importance of integrating environmentally friendly approaches in cephalosporin bioanalysis, paving the way for future innovations in bioanalytical research., (© 2025 The Author(s). Journal of Separation Science published by Wiley‐VCH GmbH.)

Significance: Autologous adipose tissue grafting (AAG) can provide soft tissue reconstruction in congenital defects, traumatic injuries, cancer care, or cosmetic procedures; over 94,000 AAG procedures are performed in the United States every year. Despite its effectiveness, the efficiency of AAG is limited by unpredictable adipocyte survival, impacting graft volume retention (26-83%). Recent Advances: Acellular adipose matrices (AAMs) have emerged as a potential alternative to AAG. AAMs include adipose tissue-derived extracellular matrix (ECM) and growth factors (GFs), but not cells. When grafted, AAMs serve as scaffolds with biochemical and biophysical cues for local cell (especially adipocytes) proliferation, regenerating soft tissue, and restoring volume. Being acellular, the AAM is not limited by adipocyte necrosis/apoptosis. Critical Issues: Research on AAM has mostly been conducted on small animal models and with small grafts. Clinically relevant AAM research (large animal models and/or clinical trials) is sparse and limited. To address this gap, we conducted a systematic review of clinically relevant AAM literature to assess AAM's clinical efficacy and safety. Across 11 human and 1 porcine study involving reconstructive or cosmetic procedures, we found that AAMs resulted in significant volume retention, adipogenesis, and angiogenesis, without notable adverse effects. Future Directions: Available quantitative and qualitative data suggest that AAM is an effective and safe alternative to AAG. Yet, the current literature is still limited; more robustly designed studies with standardized methods to assess outcomes will help validate these positive preliminary findings, and possibly pave the way for a broader clinical adoption of AAM.

Propofol (PFL) owing to its excellent inhibitory property of neurotransmitters in CNS by positive modulation of ligand gated ion channels to an integrated chloride channeled GABAA thereby acts as a general anesthetic. It differs from other general anesthetics chemically and pharmacologically as it has lesser side effects compared to other general anesthetics and is most commonly used. The present review focuses on two aspects (a) various analytical methods used in quantification of Propofol in pharmaceutical formulations and (b) various analytical methods used to determine Propofol in biological matrices and some biological markers like hair and end tidal nasal air for forensic purpose to estimate drug concentration in suspected cases. Here the various analytical methods are developed using different parameters and validation of employed methods are discussed. Estimated parameters like the linearity, LOQ (Limit of quantification), % recovery, slope, intercept, validation are discussed for the individual method. The critical quality attributes like the wavelength of detection, columns, flow rate, gas flow, and the sample preparation methods for the determination of PFL by bioanalytical methods are also discussed. Type of electrode, mechanism involved and the potential voltage applied for a particular electrochemical method are also discussed. [ABSTRACT FROM AUTHOR]

Lamotrigine owing to its excellent inhibitory property of neurotransmitter release especially glutamate is used in the treatment of epilepsy as a second-line antiepileptic drug. It differs from other antiepileptic drugs chemically and pharmacologically and is used as both monotherapy and adjunct therapy in the treatment of epilepsy. The present review focuses on two aspects (a) various analytical methods used in quantification of Lamotrigine in pharmaceutical formulations and (b) various analytical methods used to determine Lamotrigine in biological matrices. Here the various analytical methods are developed using different parameters and validation of employed methods is discussed. Estimated parameters like the linearity, LOD (Limit of detection) and LOQ (Limit of quantification) of validation are discussed for the individual method. The critical quality attributes like the wavelength of detection, mobile phase, columns, flow rate, retention time, and the sample preparation methods for the estimation of Lamotrigine by bioanalytical methods are also discussed. [ABSTRACT FROM AUTHOR]

A sensitive and simple sample pretreatment method based on a two‐phase solvent bar microextraction (SBME) technique coupled with HPLC–diode array detector (DAD) was developed for simultaneous extraction and determination of trace amounts of furosemide and carbamazepine in human urine and plasma samples. The significance of operational factors on carbamazepine and furosemide extraction efficiency % (EE%) was screened using full factorial design (FFD) while central composite design (CCD) was used to model the entire process. A quadratic model was found convenient to correlate the extraction EE% of selected drugs with dominant experimental factors. A Pareto chart was also used to examine the importance of factors on drugs' EE%. The analytical performance of the method in urine and plasma samples demonstrated good linearity (R2 ˃ 0.992) with detection limits ranging from 4.2 to 10.9 μg L−1, and extraction recovery over 89.45% for both drugs in urine and plasma samples. A comparison against published methods was also performed and the results revealed that the developed method exhibits a confident sensitivity, feasible operation, and simple analysis for both drugs. Finally, the practicability of the validated SBME–HPLC–DAD method was demonstrated by successfully applying it to the analysis of furosemide and carbamazepine in real patient urine samples. [ABSTRACT FROM AUTHOR]

• Synthesis of novel Triazole Thiazole 4-Nitrobenzohydrazide Schiff base (4NHTS). • Preparation of 4NHTS-stabilizd AgNPs. • Selectivity of 4NHTS-AgNPs based sensor for Neomycine. • Low LoD and LoQ of 0.0061 μM and 0.020 μM. • Effectiveness of sensor for real samples. The widespread usage of antibiotics is leading to an increased negative impact on living organisms due to the consumption of polluted water containing drug residues. The emergence of drug-resistant bacteria has additionally manifested a growing need to identify commonly available medications in water sources. A rapid colorimetric nanosensor is developed in this study to selectively detect Neomycin, an antibiotic of class aminoglycosides. A straightforward reduction method was employed for the formation of Schiff base (4-nitrobenzohydrazide triazole thiazole) capped silver nanoparticles (4NHTS-AgNPs). Upon treatment with Neomycin, the colloidal solution of 4NHTS-AgNPs exhibited an immediate color change from yellow to red while no visible change was observed by addition of other competitive drugs. With an increase in drug concentration, the plasmonic characteristic peak of 4NHTS-AgNPs at 405 nm exhibited a progressive reduction. Furthermore, incubation with NeO resulted in a bathochromic shift and broadening to longer wavelength, specifically to 565 nm. The combined quenching and shift of the plasmonic peak were attributed to the aggregation of 4NHTS-AgNPs induced by the NeO through hydrogen bonding. The 4NHTS-AgNPs based sensor demonstrated a linear dynamic range of 0.02–100 μM, with a limit of detection and limit of quantification of 0.0061 μM and 0.020 μM, respectively. Even in the presence of interfering drugs and for real sample analysis, the selectivity of 4NHTS-AgNPs based sensor towards neomycin remained consistent. [Display omitted] [ABSTRACT FROM AUTHOR]

The abuse of buprenorphine and methadone has grown into a rising worldwide issue. After their consumption, buprenorphine, methadone and their metabolites can be found in the human organism. Due to the difficulty in the assessment of these compounds by routine drug screening, the importance of developing highly sensitive analytical approaches is undeniable. Liquid chromatography tandem mass spectrometry is the preferable technique for the determination of buprenorphine, methadone and their metabolites in biological matrices including urine, plasma, nails or oral fluids. This research aims to review a critical discussion of the latest trends for the monitoring of buprenorphine, methadone and their metabolites in various biological specimens. [ABSTRACT FROM AUTHOR]

Sample preparation is considered as the bottleneck step in bioanalysis because each biological matrix has its own unique challenges and complexity. Competent sample preparation to extract the desired analytes and remove redundant components is a crucial step in each bioanalytical approach. The matrix effect is a key hurdle in bioanalytical sample preparation, which has gained extensive consideration. Novel sample preparation techniques have advantages over classical techniques in terms of accuracy, automation, ease of sample preparation, storage, and shipment and have become increasingly popular over the past decade. Our objective is to provide a broad outline of current developments in various bioanalytical sample preparation techniques in chromatographic and spectroscopic examinations. In addition, how these techniques have gained considerable attention over the past decade in bioanalytical research is mentioned with preferred examples. Modern trends in bioanalytical sample preparation techniques, including sorbent-based microextraction techniques, are primarily emphasized. [Display omitted] • Bioanalytical sampling techniques are described with suitable applications in pharmaceuticals. • The pros and cons of each bioanalytical sampling techniques are described. • Relevant biological matrices are outlined. [ABSTRACT FROM AUTHOR]

Nowadays it is increasingly important from a pharmacological, toxicological, and clinical point of view to have rapid and reliable screening tests available for the analysis of numerous compounds in very short time. Often these procedures involve innovative and eco–friendly extraction and purification techniques, but it is necessary to apply preliminary steps such as the protein precipitation (plasma or whole blood) or enzymatic hydrolysis, to obtain a quantitative dosage also of the metabolites (urine). In this work a rapid screening procedure in liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS) for the qualitative evaluation of 739 compounds in biological samples (blood, post–mortem blood, and urine) has been reported. The method also considers the deuterated internal standards (d9–methadone and d3–monohydroxycarbazepine) to monitor the performances of the screening (check of the fragmentation process and retention times). The procedure involves two separate analyses in positive and negative ionization and a chromatographic run of 18 min, without modifying the instrumental parameters (except the ionization polarity of the turbospray source). The chromatographic separation was carried out using a Restek Allure PFP Propyl (5 µm, 60Å, 50 × 2.1 mm) column in gradient elution mode. The instrument works in Multiple Reaction Monitoring (MRM) mode on 697 specific transitions for the compounds subject to screening. Furthermore, real samples (human blood and urine) were analyzed to confirm the correct performance of the screening.

Abstract Background Recent advances in the diversified anti-diabetic drugs have appeared in the startling increase in the count of poisoning cases. The epidemics of diabetes mellitus are increasing; hence, the no. of anti-diabetic drug users raised by 42.9%. The use of glimepiride raised to 24%. As the toxicity and drug cases are also escalating with increasing epidemics of diabetes mellitus, a novel gas chromatography-mass spectrometry (GC-MS) method for detecting glimepiride in biological matrices is developed. Results Liquid-liquid extraction method was employed by using 1-butanol: hexane (50:50, v/v) under an alkaline medium, and then back extraction was done via acetic acid. Distinct derivatization techniques were employed for the sample preparation for GC-MS analysis, i.e., silylation and acylation. Derivatization approaches were optimized under different parameters, i.e., reaction temperature and reaction time. N-Methyl-N-(trimethylsilyl) trifluoroacetamide [MSTFA] was found to be the best sound derivatization reagent for the GC-MS analysis of glimepiride. Total ion current (TIC) mode was selected for the monitoring of ions of trimethylsilyl (TMS) derivative of glimepiride with an m/z ratio of 256. Distinct parameters like specificity, carryover, stability, precision, and accuracy were evaluated for validating the identification method. The GC-MS method is found to be linear and illustrated within the range 500 to 2500 ng/ml with the value of R 2 (coefficient of determination) at 0.9924. The stability of the extracted and derivatized glimepiride was accessed with regard to processed/extracted sample conditions and autosampler conditions, respectively. Accuracy at each concentration level was within the + 15% of the nominal concentration. Precision (%) for the interday and intraday analysis was found to be in the respectable spectrum. Conclusion Henceforth, the proposed GC-MS method can be employed for the determination of glimepiride in biological matrices.

The ubiquitous presence of contaminants like pesticides in the various environmental matrices has become a concern for environmental sustainability and global stability. Pesticides are a distinctive class of environmental contaminants that are specifically introduced into the environment to kill or inhibit pests attacking the different crops. Although pesticide application is beneficial to crop production by serving several significant purposes, like protection against vector-borne diseases and crop loss, there are substantial concerns as they have a persistent nature and can possess serious consequences because of harmful effects to non-targeted beings comprising humans also. Pesticide consumption has reached 4.1 million tonnes/year in 2017 almost 81% from 1990. Recent data suggest pesticides account for 14–20% of global suicides from 2006 to 2015 resulting in 111,000–168,000 deaths annually from 2010 to 2014. About 14 million people have died from suicide by consuming pesticides since the beginning of the Green revolution. About 1 million accidental pesticide poisoning occur each year causing 20,000 fatalities approximately. For this reason, the occurrence of pesticides in different mediums like crop, air, water resources, fruits and vegetables, soil, plants, birds, animal products, and human beings was reviewed. This paper presents an overview of pesticides occurrence, distribution, extraction method, analytical techniques for their detection. This review will assist policymakers to enforce guidelines to restrict the redundant use of pesticides. [ABSTRACT FROM AUTHOR]

The quantification and interpretation of drug concentrations in biological matrices to optimize pharmacotherapy and to perform the therapeutic drug monitoring (TDM) is particularly important for compounds with narrow therapeutic ranges, known to cause adverse effects. In these cases, the biomonitoring is essential to avoid the toxicity and side effects. In this study, an innovative Fabric Phase Sorptive Extraction (FPSE) followed by high performance liquid chromatography-photodiode array detection (FPSE–HPLC–PDA) method was optimized and validated for the extraction and quantitative evaluation of seven antidepressant drugs (ADs, venlafaxine, citalopram, paroxetine, fluoxetine, sertraline, amitriptyline, and clomipramine) in human whole blood, urine, and saliva samples.The best chromatographic separation was obtained using a reverse phase column and ammonium acetate (50 mM, pH 5.5) and acetonitrile (AcN) as mobile phases, with 0.3% of triethylamine (TEA) for the best peak shape. The used sample preparation technique, FPSE, developed in 2014, has offered numerous advantages such as low consumption of organic solvents, no sample pretreatment, and reduced overall sample preparation time. Among all tested membranes, sol-gel carbowax (CW 20 M) sorbent, coated on cellulose FPSE media, was the most efficient. The developed method provides satisfactory limit of detection of 0.06 μg/mL for all analytes except for venlafaxine that was 0.04 μg/mL. Both RSD% and BIAS% gave values below ±15%, according to current guidelines. Finally, real samples analyzes were carried out, comparing the obtained data with the anamnestic data of the subjects, confirmed the validity of the method.

In general, the analysis of biological matrices is challenging and a sample preparation step employing extraction/cleanup techniques is required. Liquid-phase microextraction using deep eutectic solvents has been exploited in numerous applications because these solvents exhibit fascinating physico-chemical properties in addition to simple and straightforward preparation. Varied configurations and strategies have been examined for the determination of different classes of analytes, and these methodologies offer environmentally friendly workflows with low solvent and sample consumption, rapid and simple experimental procedures, and satisfactory analytical performance. In this review, developments related to the use of deep eutectic solvents in microextraction approaches for the analysis of biological matrices are briefly discussed with a focus on studies reported from 2017 to 2021.