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Synopsis: SARS‐CoV‐2 was detected in the vaginal and cervical fluid, amniotic fluid, cord blood, placental membranes, and breastmilk of pregnant women, therefore suggesting the possibility of vertical transmission. [ABSTRACT FROM AUTHOR]

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Objective To establish a method for determination of escitalopram in biological samples by ultrasound-assisted ionic liquid-dispersive liquid-liquid microextraction combined with gas chromatography-tandem mass spectrometry （GC-MS/MS） and provide evidences for forensic determination of cases related to escitalopram. Methods The 1-hexyl-3-methylimidazolium hexafluorophosphate （[C6MIM][PF6]） was selected as an extract solvent to process biological samples. Ultrasound-assisted extraction was used on the samples. Then the samples were detected by GC-MS/MS. Results The linear range of escitalopram in blood and liver were 5.56-1 111.10 ng/mL and 0.025-5.00 mg/g, respectively. The correlation coefficient （r） were greater than 0.999, limit of detection （LOD） were 4.00 ng/mL and 2.00 μg/g, limit of quantitation （LOQ） were 14.00 ng/mL and 6.00 μg/g, respectively. The extraction recovery rates were all greater than 50%, the interday and intraday precision were less than 20%. Escitalopram was detected in blood and liver samples from the actual poisoning case by this method with a content of 1.26 μg/mL and 0.44 mg/g, respectively. Conclusion The ultrasound-assisted ionic liquid-dispersive liquid-liquid microextraction combined with GC-MS/MS is environment friendly, rapid, has good enriching effect and consumes less organic solvent and can be used for forensic determination of escitalopram related cases.

This article summarizes the publishing activities including bioanalytical and pharmaceutical analyses researches carried out in Iran in 2018 in order to connect academic researchers to those in industry, medical care units and hospitals. A wide spectrum of analytical methods has been used to determine and/or evaluate drug levels in the biological samples, based on physical, chemical and biochemical principles. We have compiled a concise survey of the literature covering 125 reports and tabulated the relevant analytical parameters. Chromatographic and electrochemical methods were found to be the technique of choice for many workers and almost 83% studies were performed by using these methods. This is the first annual review of the literature searching in SCOPUS database for published bioanalytical and pharmaceutical analysis researches in Iran.

The analysis of the literature data for the last 10 years showed that microbiological, spectroscopic, chromatographic and electrochemical methods were most often used in quantitative determination of antibiotics in biological samples and drugs. Beta-lactams, aminoglycosides, tetracyclines, fluoroquinolones and other antibiotics were widely investigated. The characteristics of different methods of the antibiotic determination were discussed.

BACKGROUND Boron is an important trace element in high calcium biological samples, such as teeth and bones. Boron content and isotopic composition are important environmental tracers. However, the calcium content in biological samples is relatively high (>90%), and it is impossible to separate and enrich boron isotopes by using the conventional boron-special resin separation process. OBJECTIVES To establish an efficient method for treatment of boron isotopes in high calcium samples. METHODS An acetic acid-ammonium acetate buffer (pH=6.0) was used as a resin regeneration solution to replace ammonia. The adsorption pH of boron resin, boron-special resin (Amberlite IRA 743) was dropped from 8-9 to 6.0, thus the precipitation was avoided during digestion of the high calcium biological samples under alkaline conditions. Only one step of ion exchange is necessary to enrich boron in biological samples. The boron isotope of samples after separation was determined by multi-collector inductively coupled plasma-mass spectrometry (MC-ICP-MS) using a standard-sample-standard bracketing method. RESULTS A one-step ion exchange method was used for separation and enrichment. The analytical accuracy of MC-ICP-MS for the determination of boron isotopes in teeth was less than 0.42‰, reaching the same level as other separation and determination methods. CONCLUSIONS This method is not only suitable for boron isotope tracing of high calcium biological samples such as teeth and bones, but also provides a reference for the analysis of high calcium soil and marine sediment.

Objective A simple and sensitive method for the determination of 3-nitropropionic acid (3-NPA) in plasma and urine by ion chromatography-triple quadrupole mass spectrometry (IC-MS/MS) was established. Methods Plasma and urine samples were extracted with aqueous solution containing 3% perchloric acid, and then the extract was centrifuged to remove the protein and lipids. The target analyte in the extract was cleaned-up by solid supported liquid/liquid extraction under pH=1-2, and methyl tert-butyl ether (MTBE) was used as eluent. After the MTBE was removed by nitrogen, the 3-NPA in the residues was dissolved into water. The separation of 3-NPA was carried out on a Dionex Ionpac AS19 analytic column (250 mm×2 mm, 7.5 μm) with gradient elution using KOH solution electrolytically generated from on-line eluent generation cartridge. Before the eluent flow entered the ion source of mass spectrometer, the potassium ion in the eluent was removed by an in-line suppressor. The 3-NPA was detected by negative electrospray ionization triple quadrupole mass spectrometry in the multiple reaction monitoring (MRM) mode. Results The result showed that the correlation coefficients of linear calibration cuve of 3-NPA were above 0.999 at the corresponding concentration ranges of 0.1-250 μg/L. The average recoveries were 92.0%-114% for 3-NPA in plasma and urine with relative standard deviations of 2.0%-12% (n=6). The limits of detection of 3-NPA (S/N=3) were 0.1 μg/L. Conclusion The method is simple, sensitive and accurate, and can be used for the determination of 3-NPA in plasma and urine.

Task-specific ionic liquids (TSILs) represent a sub-family of ionic liquids characterized by their high specificity towards a target analyte or group of analytes. This characteristic has made them valuable tools for sample preparation, where selectivity represents a key aspect, especially when other species represent a significant source of interference or when non-specific detectors are used. This review presents an overview of TSILs applications for sample preparation from the last ten years, with a special emphasis on their use as liquid-liquid microextraction solvents or as functionalizing agents for sorbents applied to solid-phase microextractions. TSILs applications for the treatment of environmental, food and biological samples are reviewed, including reports devoted to speciation analysis, a relevant trend in recent years regarding elemental studies. Additionally, focus is made on the ‘task-specificity’ of the presented TSILs, including a description of the chemical characteristics that made them selective towards the studied analytes. Finally, future trends and gaps to be covered in the field are also discussed.

Cortisol is a steroid hormone that is involved in a broad range of physiological processes in human/animal organisms. Cortisol levels in biological samples are a valuable biomarker, e.g., of stress and stress-related diseases; thus, cortisol determination in biological fluids, such as serum, saliva and urine, is of great clinical value. Although cortisol analysis can be performed with chromatography-based analytical techniques, such as liquid chromatography–tandem mass spectrometry (LC-MS/MS), conventional immunoassays (radioimmunoassays (RIAs), enzyme-linked immunosorbent assays (ELISAs), etc.) are considered the “gold standard” analytical methodology for cortisol, due to their high sensitivity along with a series of practical advantages, such as low-cost instrumentation, an assay protocol that is fast and easy to perform, and high sample throughput. Especially in recent decades, research efforts have focused on the replacement of conventional immunoassays by cortisol immunosensors, which may offer further improvements in the field, such as real-time analysis at the point of care (e.g., continuous cortisol monitoring in sweat through wearable electrochemical sensors). In this review, most of the reported cortisol immunosensors, mainly electrochemical and also optical ones, are presented, focusing on their immunosensing/detection principles. Future prospects are also briefly discussed.

The wide-spread usage of ciprofloxacin (CIP) resulted in its presence in different parts of the ecosystem. Thus, a simple, reliable, on-spot detection method for CIP is required in environmental context. Herein, a colorimetric assay is developed for the detection of CIP based on the branched polyethyleneimine (PEI) conjugated silver nanoparticles (PEI-AgNPs). AgNPs are prepared using PEI as stabilizing agent following a simple one-pot two-phase procedure. The prepared PEI-AgNPs are subsequently used for an efficient and selective detection of CIP. The characteristic yellow colour of PEI-AgNPs changed to colourless when CIP was added which was further confirmed by quenching in the intensity of the SPR (surface plasmon resonance) band (hypochromic shift). The proposed method is efficient for the quantitation of CIP in a linear dynamic range (LDR) of 0.1–200 µM with a limit of detection (LOD) of 0.038 µM, and limit of quantification (LOQ) of 0.12 µM. The developed method is selective, efficient, and sensitive to CIP in the presence of numerous interfering species and in real biological, environmental, and commercial pharmaceutical samples. Excellent performance of the proposed method compared to UV-Vis spectroscopy and UPLC in environmental, biological, and commercial pharmaceutical samples is demonstrated.

Paraquat (PQ) and diquat (DQ) are quaternary ammonium herbicides which have been used worldwide for controlling the growth of weeds on land and in water. However, PQ and DQ are well known to be toxic. PQ is especially toxic to humans. Moreover, there is no specific antidote for PQ poisoning. The main treatment for PQ poisoning is hemoperfusion to reduce the PQ concentration in blood. Therefore, it is essential to be able to detect PQ and DQ concentrations in biological samples. This critical review summarizes the articles published from 2010 to 2022 and can help researchers to understand the development of the sample treatment and analytical methods for the determination of PQ and DQ in various types of biological samples. The sample preparation includes liquid–liquid extraction, solid-phase extraction based on different novel materials, microextration methods, and other methods. Analytical methods for quantifying PQ and DQ, such as different chromatography and spectroscopy methods, electrochemical methods, and immunological methods, are illustrated and compared. We focus on the latest advances in PQ and DQ treatment and the application of new technologies for these analyses. In our opinion, tandem mass spectrometry is a good choice for the determination of PQ and DQ, due to its high sensitivity, high selectivity, and high accuracy. As far as we are concerned, the best LOD of 4 pg/mL for PQ in serum can be obtained.

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., Competing Interests: No competing interests were disclosed., (Copyright: © 2024 López-Alonso J et al.)

Enrichment and quantification of sugar phosphates (SPx) in biological samples were of great significance in biological medicine. In this work, a series of zirconium-based metal-organic frameworks (MOFs) with different degrees of defects, namely, HP-UiO-66-NH 2 - X , were synthesized using acetic acid as a modulator and were utilized as high-capacity adsorbents for the adsorption of SPx in biological samples. The results indicated that the addition of acetic acid altered the morphology of HP-UiO-66-NH 2 - X , with corresponding changes in pore size (3.99-9.28 nm) and specific surface area (894.44-1142.50 m 2 ·g -1 ). HP-UiO-66-NH 2 -10 showed the outstanding performance by achieving complete adsorption of all four SPx using only 80 μg of the adsorbent. The excellent adsorption efficiency of HP-UiO-66-NH 2 -10 was also obtained with a wide pH range and short adsorption time (10 min). Adsorption experiments demonstrated that the adsorption process involved chemical adsorption and multilayer adsorption. By utilizing X-ray photoelectron spectroscopy and density functional theory to explain the adsorption mechanism, it was found that various interactions (including coordination, hydrogen bonding, and electrostatic interactions) collectively contributed to the exceptional adsorption capability of HP-UiO-66-NH 2 -10. Those results indicated that the defect strategy not only increased the specific surface area and pore size, providing additional adsorption sites, but also reduced the adsorption energy between HP-UiO-66-NH 2 -10 and SPx. Moreover, HP-UiO-66-NH 2 -10 showed a low limit of detection (0.001-0.01 ng·mL -1 ), high precision (<13.77%), and accuracy (80.10-111.83%) in serum, liver, and cells, good stability, high selectivity (SPx/glucose, 1:100 molar ratio), and high adsorption capacity (292 mg·g -1 for SPx). The practical detection of SPx from human serum was also verified, prefiguring the great potentials of defective zirconium-based MOFs for the enrichment and detection of SPx in the biological medicine.

Tenofovir disoproxil fumarate (TDF) is an antiretroviral medication with significant curative effects, so its quantitative detection is important for human health. At present, there are few studies on the detection of TDF by electrochemical sensors. This work can be a supplement to the electrochemical detection of TDF. Moreover, bare electrodes are susceptible to pollution, and have high overvoltage and low sensitivity, so it is crucial to find a suitable electrode material. In this work, zirconium oxide (ZrO2) that has a certain selectivity to phosphoric acid groups was synthesized by a hydrothermal method with zirconyl chloride octahydrate as the precursor. A composite modified glassy carbon electrode for zirconium oxide-chitosan-multiwalled carbon nanotubes (ZrO2-CS-MWCNTs/GCE) was used for the first time to detect the TDF, and achieved rapid, sensitive detection of TDF with a detection limit of sub-micron content. The ZrO2-CS-MWCNTs composite was created using sonication of a mixture of ZrO2 and CS-MWCNTs solution. The composite was characterized using scanning electron microscopy (SEM) and cyclic voltammetry (CV). Electrochemical analysis was performed using differential pulse voltammetry (DPV). Compared with single-material electrodes, the ZrO2-CS-MWCNTs/GCE significantly improves the electrochemical sensing of TDF due to the synergistic effect of the composite. Under optimal conditions, the proposed method has achieved good results in linear range (0.3~30 μM; 30~100 μM) and detection limit (0.0625 μM). Moreover, the sensor has the merits of simple preparation, good reproducibility and good repeatability. The ZrO2-CS-MWCNTs/GCE has been applied to the determination of TDF in serum and urine, and it may be helpful for potential applications of other substances with similar structures.

Molecularly imprinted polymers (MIP) consist of a molecular recognition technology with applicability in different areas, including forensic chemistry. Among the forensic applications, the use of MIP in biological fluid analysis has gained prominence. Biological fluids are complex samples that generally require a pre-treatment to eliminate interfering agents to improve the results of the analyses. In this review, we address the development of this molecular imprinting technology over the years, highlighting the forensic applications of molecularly imprinted polymers in biological sample preparation for analysis of stimulant drugs such as cocaine, amphetamines, and nicotine. [ABSTRACT FROM AUTHOR]

Methadone (MTD) is a synthetic analgesic drug used for treating opioid dependence and effectively used clinically for patients with severe pain. The abuse of MTD may lead to poisoning, disorder in the central nervous system and even death. The regular monitoring of MTD in biological matrices including serum, plasma and urine samples is an effective way to control abuse of MTD. In this manner, the selection of analytical monitoring of MTD in biological matrices is of paramount importance. This study was conducted to review high-performance liquid chromatography (HPLC) techniques carried out on MTD and its main metabolite 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP) in the biological samples during 2015–June 2021. [ABSTRACT FROM AUTHOR]

Fourier Transform Infrared (FTIR) Spectroscopy, in particular ATR-FTIR, is a widely used technique that allows, in a very short time, to screen biological samples and to identify its specific spectral signature, being an important tool for clinical diagnosis and biomarker discovery. FTIR spectroscopy is used to screen cells, tissues and biofluids and is already implemented in biomedicine, mainly in pre-clinical setting. Although the experimental procedure is easy to implement, sample preparation, definition of spectra acquisition parameters and spectral analysis are crucial steps to obtain reliable and reproducible results. However, the selection of experimental conditions for spectral analysis can be a difficult task for researchers because the information is dispersed and often the choice is made in an empirical and inaccurate way. This review gathers and summarizes studies using FTIR in pre-clinical and clinical setting and aims to systematize information and propose some guidelines for FTIR spectroscopy studies of biological samples. This will help new users to prepare samples for FTIR analysis and understand the critical steps to correctly perform spectra pretreatment, preprocessing and statistical analysis and to implement appropriate and evidence-based experimental designs. [ABSTRACT FROM AUTHOR]

This study evaluated the effect of an algoclay-based mycotoxin decontaminant on the levels of ZEN, DON, and their derivatives in the colostrum, milk, and serum of sows, as well as in the serum of weaned piglets after maternal mycotoxin exposure during the last week of gestation and during lactation of sows (26 days). For this, sows (n = 5) were fed diets artificially contaminated with 100 (LoZEN) or 300 (HiZEN) ppb ZEN, with or without an algoclay-based mycotoxin decontaminant in the highly contaminated diet. All diets contained 250 ppb deoxynivalenol (DON). Dietary treatments did not affect the performance of the sows and piglets. Only α-ZEL was significantly increased in the colostrum of sows fed the HiZEN diet, and this increase was even higher in the colostrum of the sows fed the HiZEN diet supplemented with the test decontaminant. However, no differences in milk mycotoxin levels were observed at weaning. The highest levels of ZEN, α-ZEL, and β-ZEL were observed in the serum of sows fed the HiZEN diet. When the HiZEN diet was supplemented with the tested algoclay-based mycotoxin decontaminant the levels of ZEN and its metabolites were significantly decreased in the serum of sows. Although all sows were fed the same levels of DON, the serum level of de-epoxy-DON was increased only in the serum of piglets from the sows fed a diet with the non-supplemented HiZEN diet. In conclusion, the tested algoclay-based mycotoxin decontaminant can decrease the levels of ZEN and its metabolites in the serum of sows and the level of de-DON in the serum of piglets.

Fatty acids are widespread naturally occurring compounds, and essential constituents for living organisms. Short chain fatty acids (SCFAs) appeared as physiologically relevant metabolites for their involvement with gut microbiota, immunology, obesity, and other pathophysiological functions. This has raised the demand for reliable analytical detection methods in a variety of biological matrices. Here, we describe an updated overview of sample pretreatment techniques and liquid chromatography-mass spectrometry (LC-MS)-based methods for quantitative analysis of SCFAs in blood, plasma, serum, urine, feces and bacterial cultures. The present review incorporates various procedures and their applications to help researchers in choosing crucial parameters, such as pretreatment for complex biological matrices, and variables for chromatographic separation and detection, to establish a simple, sensitive, and robust quantitative method to advance our understanding of the role of SCFAs in human health and disease as potential biomarkers.

Abstract Bats are important for the homeostasis of ecosystems and serve as hosts of various microorganisms including bacteria, viruses, and fungi with pathogenic potential. This study aimed to isolate fungi from biological samples obtained from bats captured in the city of Sinop (state of Mato Grosso, Brazil), where large areas of deforestation exist due to urbanization and agriculture. On the basis of the flow of people and domestic animals, 48 bats were captured in eleven urban forest fragments. The samples were processed and submitted to microbiological cultures, to isolate and to identify the fungal genera. Thirty-four (70.83%) of the captured bats were positive for fungi; 18 (37.5%) and 16 (33.33%) of these bats were female and male, respectively. Penicillium sp., Scopulariopsis sp., Fusarium sp., Aspergillus sp., Alternaria sp., Cryptococcus sp., Trichosporon sp., and Candida sp., which may cause opportunistic infections, were isolated. The bat species with the highest number of fungal isolates was Molossus molossus: 21 isolates (43.8%). According to our results, bats captured in urban forest fragments in Sinop harbor pathogenic fungi, increasing the risk of opportunistic fungal infections in humans and domestic animals.

Electrospun poly(vinyl alcohol)-(PVA)-poly(acrylic acid) (PAA)/carbon nanotubes(CNTs)-cellulose nanocrystal (CNC) (PVA-PAA/CNT-CNC) composite nanofibers were prepared and characterized using Fourier transform-infrared spectroscopy and field emission scanning electron microscopy. The resultant composite was used as an effective and novel sorbent for pipette-tip micro-solid phase extraction (PT-μSPE) of seven opioid analgesics (OAs) in biological samples followed by HPLC-UV analysis. Addition of CNT-CNC with the high specific surface area and plenty of OH-functional groups endows the nanofibers with considerable extraction efficiency. Under the optimum conditions, the linearity was obtained in the range 1.5 to 700.0 ng mL−1 for morphine, codeine, oxycodone, and tramadol, and 0.5 to 1000.0 ng mL−1 for nalbuphine, thebaine, and noscapine with coefficient of determination (r2) ≥ 0.9990. Detection limits (LODs) based on S/N = 3 were in the range of 0.15–0.50 ng mL−1. The relative standard deviations (RSDs) of 4.1–5.4% (intra-day, n = 5) and 5.2–6.4% (inter-day, n = 3) for three consecutive days were achieved. Finally, the efficiency of the PT-μSPE-HPLC-UV method was evaluated for the determination of OAs in human plasma and urine samples with good recoveries (87.3 to 97.8%). [ABSTRACT FROM AUTHOR]

Analysis of biological samples is affected by interfering substances with chemical properties similar to those of the target analytes, such as drugs. Biological samples such as whole blood, plasma, serum, urine and saliva must be properly processed for separation, purification, enrichment and chemical modification to meet the requirements of the analytical instruments. This causes the sample preparation stage to be of undeniable importance in the analysis of such samples through methods such as microextraction techniques. The scope of this review will cover a comprehensive summary of available literature data on microextraction techniques playing a key role for analytical purposes, methods of their implementation in common biological samples, and finally, the most recent examples of application of microextraction techniques in preconcentration of analytes from urine, blood and saliva samples. The objectives and merits of each microextration technique are carefully described in detail with respect to the nature of the biological samples. This review presents the most recent and innovative work published on microextraction application in common biological samples, mostly focused on original studies reported from 2017 to date. The main sections of this review comprise an introduction to the microextraction techniques supported by recent application studies involving quantitative and qualitative results and summaries of the most significant, recently published applications of microextracion methods in biological samples. This article considers recent applications of several microextraction techniques in the field of sample preparation for biological samples including urine, blood and saliva, with consideration for extraction techniques, sample preparation and instrumental detection systems. [ABSTRACT FROM AUTHOR]

Neurodegeneration disorders are complex and multifaceted, leading to many chronic diseases, like Parkinson's disease (PD). Electrolytes imbalance has a significant role in the pathophysiology of neurological disorders, which might serve as a bio-indicator of these problems. In the present study, the disturbances of the electrolytes, calcium (Ca), magnesium (Mg), sodium (Na), and potassium (K), concentrations, and their correlation with biochemical parameters of PD patients at three different age groups (15 to 75 years) and stages were studied. The all resulted data of PD patients was compared with non-diseased/referents (PD) of same age groups. The biological samples (scalp hair, serum and plasma) were collected from Parkinson's disease (PD) patients, diagnosed at three stages, early (15 to 30 years), mild (30 to 60 years) and severe (61 to 75 years). The electrolyte concentrations were measured after acid digested biological samples using flame atomic absorption spectrometry. The precision of the digestion method was verified by matrices matched certified reference materials. The resulted data indicated that the contents of Ca and Mg were found to be higher in scalp hair samples of PD patients at early to severe stages as compared with those results obtained from referents. The concentrations of Na and K were found to be lower for all PD patients groups as compared with referents; however, the difference was not significant (p < 0.05). Electrolytes levels in blood serum and plasma were found to be lower in all patients than healthy groups (p < 0.01). These results suggest a disturbance in the electrolytes homeostasis during the different clinical stages of PD, whereas the higher disturbance was observed in patients at severe stage (61 to 75 years). [ABSTRACT FROM AUTHOR]

A rapid, accurate, and sensitive analytical method, ultrasonication-assisted spraying based fine droplet formation–liquid phase microextraction–gas chromatography–mass spectrometry (UA-SFDF-LPME-GC-MS), was proposed for the determination of trace amounts of hydroxychloroquine sulfate in human serum, urine, and saliva samples. To determine the best extraction strategy, several liquid and solid phase extraction methods were investigated for their efficiencies in isolation and preconcentration of hydroxychloroquine sulfate from biological matrices. The UA-SFDF-LPME method was determined to be the best extraction method as it was operationally simple and provided accurate results. Variables such as the extraction solvent, spraying number, sodium hydroxide concentration and volume, sample volume, mixing method, and mixing period were optimized for the proposed method using the one-variable-at-a-time approach. In addition, Tukey's method based on a post hoc comparison test was employed to evaluate the significant difference between the parameters inspected. After the optimization studies, the limit of detection (LOD) and limit of quantification (LOQ) were determined to be 0.7 and 2.4 μg/kg, respectively. The sensitivity of the GC-MS system based on the LOD was enhanced approximately 440-fold when the UA-SFDF-LPME method was employed. Spiking experiments were also conducted for the human serum, urine, and saliva samples to determine the applicability and accuracy of the proposed method. Recoveries for the human serum, urine, and saliva samples were found to be in the ranges of 93.9%–101.7%, 95.2%–105.0%, and 93.1%–102.3%, respectively. These results were satisfactory and indicated that the hydroxychloroquine sulfate level in the above biological samples could be analyzed using the proposed method. [Display omitted] • Several microextraction methods were tested to detect trace levels of hydroxychloroquine sulfate. • Detection power of the GC-MS system was enhanced 440-fold with the selected UA-SFDF-LPME method. • LOD and LOQ values for the method were 0.7 and 2.4 ng/g, respectively. • Recoveries for human serum, urine and saliva were found between 93.1% and 105.0%. [ABSTRACT FROM AUTHOR]

• A fiber-in-tube SPME-CapLC-MS/MS method was developed. • The reduced flow rate increased the sensitivity due to better desolvation of the analytes. • The method developed here was compared with the fiber-in-tube SPME-LC-MS/MS (performed on a conventional scale). • The use of a chromatography column was significant not only to focus the analytes in the column. Mass spectrometry is characterized by its high sensitivity, ability to measure very low analyte concentrations, specificity to distinguish between closely related compounds, availability to generate high-throughput methods for screening, and high multiplexing capacity. This technique has been used as a platform to analyze fluid biomarkers for Alzheimer's disease. However, more effective sample preparation procedures, preferably antibody-independent, and more automated mass spectrometry platforms with improved sensitivity, chromatographic separation, and high throughput are needed for this purpose. This short communication discusses the development of a fiber-in-tube SPME-CapLC-MS/MS method to determine Aβ peptides in cerebrospinal fluid obtained from Alzheimer's disease patients. To obtain the fiber-in-tube SPME capillary, we longitudinally packed 22 nitinol fibers coated with a zwitterionic polymeric ionic liquid into the same length of the PEEK tube. In addition, this communication compares this fiber-in-tube SPME method with the conventional HPLC scale (HPLC-MS/MS) and when directly coupled to CapESI-MS/MS without chromatographic separation, and, as a case study, discusses the benefits and challenges inherent in miniaturizing the flow scale of the sample preparation technique (fiber-in-tube SPME) to the CapLC-MS/MS system. Fiber-in-tube SPME-CapLC-MS/MS provided LLOQ ranging from 0.09 to 0.10 ng mL−1, accuracy ranging from 91 to 117 % (recovery), and reproducibility of less than 18 % (RSD). Analysis of the cerebrospinal fluid samples obtained from Alzheimer's disease patients evidenced that the method is robust. At the capillary scale (10 µL min−1), this innovative method presented higher analytical sensitivity than the conventional HPLC-MS/MS scale. Although fiber-in-tube SPME directly coupled to CapESI-MS/MS offers advantages in terms of high throughput, the sample was dispersed and non-quantitatively desorbed from the capillary at low flow rate. These results highlighted that chromatographic separation is important to decrease the matrix effect and to achieve higher detectability, which is indispensable for bioanalysis. [ABSTRACT FROM AUTHOR]

• New magnetic sorbent based on MIL-101Cr (NH 2) MOF and NiFe 2 O 4 was prepared for the first time. • Dispersive solid phase extraction method was done for extraction of sunitinib from biological samples. • The sample preparation was effectively performed prior to HPLC-MS/MS analysis. • High efficiency, broad linear range, and sensitive determinations were the advantages of the method. Herein, a simple, sensitive, and reliable dispersive solid phase extraction was reported for the efficient extraction of sunitinib from biological samples. To facilitate the extraction of the desired analyte from urine and plasma samples, magnetic MIL-101Cr (NH 2) @SiO 2 @ NiFe 2 O 4 was synthesized by a hydrothermal method and applied as an effective sorbent during the extraction process. After adsorption of the drug using 10 mg of MIL-101Cr (NH 2) @ SiO 2 @ NiFe 2 O 4 nanoparticles through vortexing (1 min), the sorbent was separated from the sample solution using a magnet. To eluate the drug, the sorbent containing the sunitinib was contacted with 100 µL dimethylformamide. The eluent was analyzed by high performance liquid chromatography-tandem mass spectrometry. Reasonable validation data consisting of low limits of detection (0.14, 0.35, and 0.70 ng mL−1 in deionized water, plasma, and urine) and quantification (0.48, 1.2, and 2.4 ng mL−1 in deionized water, plasma, and urine, respectively), a wide linear range of the calibration curve (0.48–200, 1.2–200, and 2.4–100 ng mL−1 in deionized water, plasma, and urine, respectively) good extraction recovery (76 %), and low relative standard deviations for inter- and intra-day precisions (6.9 %) were obtained by the method. Eventually, the proposed procedure was effectively implemented on both plasma and urine samples, yielding successful outcomes. [ABSTRACT FROM AUTHOR]

[Display omitted] • A combining dispersive micro solid phase extraction with HPLC-DAD was developed to antiepileptic drugs. • The method is used for determining three antiepileptic drugs in biological and water samples. • A new sorbent was synthesized using hydrothermal and sol–gel methods. • The sorbent components ratio was optimized using the simplex lattice design. • The effective parameters in the method were optimized by experimental design and one factor at a time. Due to the widespread utilization of antiepileptic drugs for seizure control and patient well-being, it is crucial to determine their presence in biological and water samples. This is essential for optimizing therapy, comprehending drug behavior, identifying drug interactions, monitoring environmental contamination, and safeguarding public health and ecology. Hence, a novel method that combines dispersive micro solid phase extraction with HPLC-DAD was developed to simultaneously determine the presence of Lacosamide, Levetiracetam, and Phenytoin. To achieve this, a new sorbent was synthesized using the hydrothermal and sol–gel methods, which consisted of bimetallic MIL-100 (Fe, Ni) on MIL-100 (Mn), SiO 2 , and Fe 3 O 4 nanoparticles. We compared the extraction capabilities of several sorbents in order to select the most effective one. The optimal ratio of components for the chosen sorbent was determined through the simplex lattice design to enhance its efficiency. The optimized values for SiO 2 , Fe 3 O 4 , and MIL-100 (Fe, Ni) on MIL-100 (Mn) were found to be 0.1, 0.34, and 0.56, respectively. The parameters that affected the dispersive micro solid phase extraction method were optimized using both experimental design and one factor at a time. Under the optimal conditions, the linear range for the detection of Lacosamide, Levetiracetam, and Phenytoin was determined to be 0.1–363.0, 0.3–372.0, and 0.4–435.0 ng mL−1, respectively, with low LODs below 0.13 ng mL−1. Additionally, a preconcentration factor of 492.6, 487.1, and 469.5 was achieved for measuring Lacosamide, Levetiracetam, and Phenytoin, respectively. The intra-day and inter-day relative standard deviations (RSDs) ranged from 3.8 % to 4.6 % and 4.2 % to 5.2 %, respectively. The recoveries and RSDs for analyzing real water, human urine, and serum samples were found to be between 89.6–97.0 % and 4.53–6.44 %, respectively. [ABSTRACT FROM AUTHOR]

This study involved the assessment of 222Rn concentrations in liquid samples (namely serum and urine) obtained from individuals who were smokers and non-smokers across five distinct age groups in the Najaf Governorate of Iraq. The measurements were conducted using a portable digital Air Things device commonly employed for detecting radon gas in residential environments. This device was placed in a container that is placed in liquid samples, which makes it work to capture the existing radon. The mean value of radon concentrations in serum and urine samples for smokers was 5.64 ± 2.80 Bq/m3 and 3.56 ± 2.31 Bq/m3, respectively. While, the mean value of radon concentrations in serum and urine samples for non-smokers was 2.32 ± 0.67 Bq/m3 and 1.61 ± 1.00 Bq/m3, respectively. By comparing the radon concentrations for serum and urine samples with age and smoking groups, the value of P-Value (p < 0.01) was increased significantly statistically. Also, it is found that a positive and good correlation for radon concentrations between serum and urine. Although the levels of radon were found to be under the globally accepted thresholds, the results of 222Rn in all samples of serum and urine in smokers were higher than in non-smokers. Thus, it may be concluded that cigarette smoking is used as a biomarker of the presence of radon gas. • Evaluate using of Air Things radon detector. • Determine radon concentration in Liquid Samples (Serum and Urine) of smokers and non-smokers in Al-Najaf city, Iraq. • Compare determined activity level with results obtained from similar studies in other parts of the world. • To access the Environmental impact of prevalent radionuclides in the study area. • Evaluate safety levels of each radionuclide to human and animals in the Environment. [ABSTRACT FROM AUTHOR]

• Chemical attribution was first used to identify the exposure source of OPNAs exposed biological samples based on the data from GC × GC-TOFMS analysis. • This work used chemical attribution to explore organic impurity profiles in biological samples exposed to various OPNAs. • Conventional method was used to remove the irrelevant components for obtaining the impurity profile only applicable to a certain weapon' samples. • The outcomes can be a reference for tracing the source for OPNA-exposed samples, which was beneficial to the further development in source matching of forensic samples. Chemical attribution is a vital tool to attribute chemicals or related materials to their origins in chemical forensics via various chemometric methods. Current progress related to organophosphorus nerve agents (OPNAs) has mainly focused on the attribution of chemical sources and synthetic pathways. It has not yet been applied in matching exposed biological samples to their sources. This work used chemical attribution to explore organic impurity profiles in biological samples exposed to various OPNAs. Chemical attribution was first used to identify the exposure source of biological samples based on the full-scan data via comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometer (GC × GC-TOFMS). Taking peak area as the only variable, it can quickly match exposed samples to their sources by applying unsupervised or supervised models, screen difference compounds via one-way ANOVA or t -tests, and then identify valuable impurities that can distinguish different types of exposed samples. To further obtain the impurity profile only applicable to a certain weapon' samples, the irrelevant components were removed via conventional methods. The findings showed there were 53 impurities that can promote distinguishing six groups of OPNA exposed samples, as well as 42 components that can be used as valuable impurities to distinguish class G and class V samples. These were all unique impurities that appear in a certain weapon' samples. The outcomes can be a reference for tracing the source for OPNA-exposed samples, which was beneficial to the further development in source matching of forensic samples. Moreover, the chemical attribution for impurity profiles in biological samples after weapons exposure may inspire research into the characteristics of impurity profile in biological samples as well as practical applications of chemical attribution for OPNA-exposed samples, that may expand potential biomarkers and break the limits of existing markers in the future. [ABSTRACT FROM AUTHOR]

Biosensors have been explored for their application in analytical assays with an increasing reliance on nanomaterials and biomolecule recognition units. Recently, magnetic nanoparticle-aptamer (MNPA) hybrids found crucial for their strengths in target binding, low limit of detection (LOD), enhanced sensitivity, exceptional stability, and superior selectivity. They have been employed for the identification of a diverse range of analytes in biological, food, and environmental samples. However, their integration with conventional sensing technologies remains a challenge. Herein, the current state-of-the-art of MNPA sensors are reviewed. First, the significance of using MNP and aptamers in biosensors is discussed and then the technologies incorporating MNPAs to achieve higher sensitivity and selectivity in quantifying analytical samples are introduced. Finally, prospects and practical approaches to address the existing drawbacks of MNPA sensors are presented. [Display omitted] • Recent advances and limitations in magneto-aptasensing of biomolecules were discussed. • The analytical figures of merit of the developed methods are evaluated. • Current improvements on the monitoring of biomolecules using magneto-aptasensors were investigated. • All of research gaps on the magneto-aptasensors were surveyed. [ABSTRACT FROM AUTHOR]

The following paper presents statistical analysis of measurement results close to the detection limit of an analytical technique and being random-left censored data. For such observations the measured value is not known precisely but is restricted by the detection limit. In the paper, the idea of random-left censored observations and data analysis are presented generally and next it is shown how to include censored observations into the statistical analysis with the use of available statistical analysis software (survival analysis procedure). Statistical procedure is presented on the examples of the X-ray spectroscopic analysis of element concentrations in medical and biological samples. Censored observations are included in data analysis and quartiles are estimated. Additionally, two- and multigroup comparison is presented for the censored observations. The accuracy of the presented procedure is demonstrated and discussed on the basis of Monte-Carlo simulations. [Display omitted] • X-ray spectroscopic measurement results limited by detection limit (censored data). • Analysis of censored observations with the use of statistical analysis software. • Analysis based on examples of TXRF measurements in medical and biological samples. • Procedure accuracy demonstrated on the basis of Monte-Carlo simulations. [ABSTRACT FROM AUTHOR]

• Nanoplate-like calcium molybdate (CaMoO 4) with molybdenum oxide (MoO 3) was developed as effective electrocatalyst. • The fabricated electrode was studied for flutamide (FLT) detection. • With the linear range 0.044–1184.9 µM the detection limit was 1.6 nM. • The real sample FLT analysis had an excellent recovery rate. • The designed CaMoO 4 /MoO 3 will act as successful material for drug monitoring. The growing population is prone to be affected by various infections and diseases. On this basis, cancers are widespread, ranging from acute to chronic conditions. One such prostate cancer is herein concentrated due to its harmful effects on males. Flutamide (FT) acts as an antiandrogen drug by controlling testosterone hormonal growth and decreasing the C-19 steroid metabolism to prevent its spread. The impact of electrochemical sensors is herein highly motivated due to their robust, sensitive, selective approach, and easier operation and is employed to detect FT. The design of the working electrode in the electrochemical sensing of FT is based on nanoplate-like calcium molybdate/molybdenum oxide (CaMoO 4 /MoO 3). The CaMoO 4 /MoO 3 was characterized by recognizing its physical and morphological features. The X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) studies proved the crystalline nature and the elemental presence of CaMoO 4 /MoO 3. The field emission scanning electron microscope (FESEM) analysis determined a nanoplate-like structure with elemental presence observed with EDAX and elemental mapping analysis. The linear range for the FT detection ranged from 0.044 to 1184.9 µM with a sensitivity of about 53.34 μAμM−1cm2, and the limit of detection (LOD) 0.0016 μM. The real sample studies executed in biological samples established an excellent recovery result. The fabricated electrode material will be an essential tool in sensing with high significance. [Display omitted] [ABSTRACT FROM AUTHOR]

Abstract Based on the highly toxic effects of Cd(II) on the aquatic environment and the human health, identification and evaluation of such pollutants is required. Efficient and economic electrodes for sensitive and selective detection of this element are very important. In this study, carbon paste electrode (CPE) modified with lanthanum tungstate ion exchanger was assembled for potentiometric assay of Cd(II) ions. The prepared sensor exhibited a Nernstian response for Cd(II) within a wide working range of 8 × 10−8–1 × 10−1 mol L−1, with a slope of 29.4 ± 0.12 mV/decade. It has been specified by a low detection limit of 8 × 10−8 mol L−1 and a short response time of ~ 5 s and can be utilized efficiently up to 22 weeks without any significant errors in the potential determination. The standard electrode potentials, E°, and the isothermal temperature coefficient (dE°/dt) of the sensor were estimated at various temperatures. The obtained results indicated that the nominated electrode has efficient performance to estimate Cd(II) in its pure solutions and other various real samples (river water, plant foodstuff, industrial wastewater, nickel cadmium battery, and fish tissue samples).

We present here a perspective detailing the current state-of-the-art technologies for the characterisation of nanoparticles (NPs) in liquid suspension. We detail the technologies involved and assess their applications in the determination of NP size and concentration. We also investigate the parameters that can influence the results and put forward a cause and effect analysis of the principle factors influencing the measurement of NP size and concentration by NP tracking analysis and dynamic light scattering, to identify areas where uncertainties in the measurement can arise. Also included are technologies capable of characterising NPs in solution, whose measurements are not based on light scattering. It is hoped that the manuscript, with its detailed description of the methodologies involved, will assist scientists in selecting the appropriate technology for characterising their materials and enabling them to comply with regulatory agencies’ demands for accurate and reliable NP size and concentration data.

In this study, a lab‐made parallel single‐drop microextraction methodology using the magnetic ionic liquid trihexyltetradecylphosphonium tetrachloromanganate (II) as extraction solvent was developed to determine the pesticides tebuconazole, pendimethalin, dichlorodiphenyltrichloroethane, and dichlorodiphenyldichloroethylene in human urine samples. The experimental setup consisted of a 96‐well plate system containing a set of magnetic pins that allowed for the manipulation of up to 96 samples simultaneously, providing an enhanced drop stability compared to traditional single‐drop microextraction approaches. The optimal conditions employed 5.38 ± 0.55 mg of extraction solvent, 1.5 mL of diluted urine samples (1:10), extraction time of 130 min, and subsequent dilution in 20 μL of acetonitrile. The method exhibited satisfactory analytical performance, with limits of detection of 7.5 μg/L for all analytes and coefficients of determination higher than 0.9955. Intraday and interday precisions ranged from 3 to 17% (n = 3) and 15 to 18% (n = 9), respectively, with relative recovery of analytes ranging from 70 to 122%. The method proposed was successfully applied in two human urine samples and no sign of the analytes was detected. The results demonstrated that the proposed method allowed for cost‐effective and high‐throughput methodology to be explored as a valuable tool in bioanalytical applications. [ABSTRACT FROM AUTHOR]

Objective To avoid the lack of biological samples data caused by confounding biological samples in the Phase Ⅰ clinical trial project，we used Y-chromosomal short tandem repeat（Y-STR）locus detection method to identify confounded biological samples from two individuals of different genders and discuss its feasibility. Methods We renumbered two blood samples with missing labels as A and B， extracted DNA from their plasma and blood cell samples，respectively.Meanwhile，we extracted DNA from a known male blood cell sample（P）and a known female blood cell sample（N）as positive and negative controls，respectively. Subsequently，we amplified three Y-STR loci fragments（DYS460，DYS513，and DYS570）in vitro using PCR technology.Finally，the amplification products were identified by 2% agarose gel electrophoresis. Results The electrophoresis bands showed that DNA was successfully extracted from the blood cell samples of P，N，A and B. Compared with the controls，three Y-STR loci DNA fragments of the correct size could be amplified from the blood cell sample of A，but none of them could be amplified from the blood cell sample of B. The Y-STR locus detection method successfully identified a sample of male subject as A and a sample of female subject as B. Conclusion The Y-STR locus detection method can identify confounded biological samples from two individuals of different genders. [ABSTRACT FROM AUTHOR]

Introduction: Organic molecules that interact with the cannabinoid receptors are called cannabinoids, which can be endogenous, natural or synthetic compounds. They possess similar pharmacological properties as produced by the plant, Cannabis sativa L. Before cannabinoids can be analysed, they need to be extracted from the matrices. Objective: To review literature on the methods and protocols for the extraction of naturally occurring cannabinoids. Methodology: An extensive literature search was performed incorporating several databases, notably, Web of Knowledge, PubMed and Google Scholar, and other relevant published materials. The keywords used in the search, in various combinations, with cannabinoids and extraction being present in all combinations, were Cannabis, hemp, cannabinoids, Cannabis sativa, marijuana, and extraction. Results: In addition to classical maceration with organic solvents, e.g. ethanol, pressurised solvent extraction, solvent heat reflux, Soxhlet extraction, supercritical fluid extraction, ultrasound‐assisted extraction and microwave‐assisted extraction, are routinely used nowadays for the extraction of cannabinoids from plant materials and cannabis consumer products. For the extraction of cannabinoids from biological samples, e.g. human blood, and also from food and beverages, and wastewater, solid‐phase extraction and its variants, as well as liquid–liquid extraction are commonly used. Parameters for extraction can be optimised by response surface methodology or other mathematical modelling tools. There are at least six US patents on extraction of cannabinoids available to date. Conclusions: Irrespective of the extraction method, extraction temperature, extraction time and extraction pressure play a vital role in overall yield of extraction. Solvent polarity can also be an important factor in some extraction methods. Cannabinoids are organic molecules that interact with the cannabinoid receptors. Before applying any analytical tools to analyse cannabinoids, it is essential to extract cannabinoids from the matrix. This review appraises the literature on the methods and protocols used for the extraction of naturally occurring cannabinoids from various matrices. An extensive literature search was performed incorporating several databases, notably, Web of Knowledge, PubMed and Google Scholar, and other relevant published materials including published books. The keywords used in the search, in various combinations, with cannabinoids and extraction being present in all combinations, were Cannabis, hemp, cannabinoids, Cannabis sativa, marijuana, and extraction. Several extraction methods, e.g. maceration, refluxing, Soxhlet, ultrasound‐assisted, microwave‐assisted, supercritical fluid and pressurised liquid extraction as well as various solid‐phase extraction methods, for the extraction of different naturally occurring cannabinoids from various matrices are available in the literature, together with a few patents. [ABSTRACT FROM AUTHOR]

A workflow was developed and implemented in a software tool for the automated combination of spatially resolved laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) data and data on the morphology of the biological tissue. Making use of a recently published biological annotation software, FishImager automatically assigns the biological feature as regions of interest (ROIs) and overlays them with the quantitative LA-ICP-MS data. Furthermore, statistical tools including cluster algorithms can be applied to the elemental intensity data and directly compared with the ROIs. This is effectively visualized in heatmaps. This allows gaining statistical significance on distribution and co-localization patterns. Finally, the biological functions of the assigned ROIs can then be easily linked with elemental distributions. We demonstrate the versatility of FishImager with quantitative LA-ICP-MS data of the zebrafish embryo tissue. The distribution of natural elements and xenobiotics is analyzed and discussed. With the help of FishImager, it was possible to identify compartments affected by toxicity effects or biological mechanisms to eliminate the xenobiotic. The presented workflow can be used for clinical and ecotoxicological testing, for example. Ultimately, it is a tool to simplify and reproduce interpretations of imaging LA-ICP-MS data in many applications. [ABSTRACT FROM AUTHOR]

Gelatin microsphere-coated Fe3O4@graphene quantum dots (Fe3O4@GQD@GM) were designed and synthesized as a novel sorbent via ultrasonic-assisted dispersive magnetic solid-phase extraction (UA-DMSPE) method. The synthesized sorbent was identified and confirmed by FT-IR, XRD, VSM, and SEM techniques. UA-DMSPE was combined with corona discharge ion mobility spectrometry for trace determination of desipramine, sertraline, and citalopram. Effective parameters were considered and optimized. The proposed method, under optimal conditions, showed excellent linearity in different concentration ranges (2–700 ng mL–1, R2 > 0.995), repeatability (RSD < 5.1%), good sensitivity (LODs in the range 0.6–1.5 ng mL−1), high preconcentration factor (PF = 207–218), and acceptable relative recoveries (93.5–101.8%). Eventually, this method was used to determine tricyclic antidepressants in various biological samples. [ABSTRACT FROM AUTHOR]

Coherent imaging enables noninvasive, label‐free, and quantitative monitoring of the dynamic motions of transparent microobjects requested in life sciences, biochemistry, material sciences, and fluid mechanics. Quantitative phase imaging (QPI), a coherent imaging technique, provides full‐field optical phase information through light interference. The use of coherence, however, inevitably accompanies phase ambiguity and coherent artifacts, such as speckle, diffraction, and parasitic interference, which severely deteriorate the interferograms to hinder successful phase reconstruction. Herein, it is demonstrated that a frequency comb can newly provide a wide coherence tunability for higher visibility interferograms, phase‐coherent multiple wavelengths for extracting physical height information from refractive index, and higher phase stability (2.39 × 10−3 at 10 s averaging time) at a higher speed up to 16.9 kHz. These superior characteristics of frequency‐comb‐referenced QPI will enable in‐depth understanding of dynamic motions in cellular, biomolecular, and microphysical samples.

Biological samples usually require cumbersome preparation steps before SEM imaging. Here we propose a simple, fast and inexpensive method to prepare and visualize biological cell culture samples in a few easy steps. We have tested this method with success on several adherent breast cancer and non-adherent leukemia cell lines. This method gives results comparable to other well-established techniques, and it can be convenient in day-to-day biological sample preparation for SEM imaging. • An easy and rapid method to visualize biological specimens under SEM. • Cells are grown on carbon tapes and gold coated. • Air drying without compromising the image quality.

The advances of biomedicine include the new technologies, diagnosis and treatment techniques, as well as the practical use of new types of biological targets, in particular, nucleic acids. Genomic deoxyribonucleic acid (DNA), extracellular DNA (exDNA) and microbiome DNA obtained from different types of samples (tissues, blood and its derivatives, feces, etc.) are used as objects of genetic research. The use of new technologies for DNA analysis required the development of standardized methods for processing biological samples in order to obtain high-quality DNA samples. The research uses various methods for collecting, preparing samples and storing various DNA-containing biomaterials and isolated DNA, as well as methods for assessing the quality of samples and biobank standards. It is obvious that the use of uniform standards will allow large-scale genetic research on the basis of biobanks and research laboratories. Specialists from professional organizations such as International Society for Biological and Environmental Repositories (ISBER), Biobanking and BioMolecular Resources Research Infrastructure-European Research Infrastructure Consortium (BBMRI-ERIC), European, Middle Eastern & African Society for Biopreservationa and Biobanking (ESBB) and the Russian National Association of Biobanks and Biobanking Professionals.

Green extraction techniques (GreETs) emerged in the last decade as greener and sustainable alternatives to classical sample preparation procedures aiming to improve the selectivity and sensitivity of analytical methods, simultaneously reducing the deleterious side effects of classical extraction techniques (CETs) for both the operator and the environment. The implementation of improved processes that overcome the main constraints of classical methods in terms of efficiency and ability to minimize or eliminate the use and generation of harmful substances will promote more efficient use of energy and resources in close association with the principles supporting the concept of green chemistry. The current review aims to update the state of the art of some cutting-edge GreETs developed and implemented in recent years focusing on the improvement of the main analytical features, practical aspects, and relevant applications in the biological, food, and environmental fields. Approaches to improve and accelerate the extraction efficiency and to lower solvent consumption, including sorbent-based techniques, such as solid-phase microextraction (SPME) and fabric-phase sorbent extraction (FPSE), and solvent-based techniques (μQuEChERS; micro quick, easy, cheap, effective, rugged, and safe), ultrasound-assisted extraction (UAE), and microwave-assisted extraction (MAE), in addition to supercritical fluid extraction (SFE) and pressurized solvent extraction (PSE), are highlighted.

New psychoactive substances (NPS), often designed as (legal) substitutes to conventional illicit drugs, are constantly emerging in the drug market and being commercialized in different ways and forms. Their use continues to cause public health problems and is therefore of major concern in many countries. Monitoring NPS use, however, is arduous and different sources of information are required to get more insight of the prevalence and diffusion of NPS use. The determination of NPS in pooled urine and wastewater has shown great potential, adding a different and complementary light on this issue. However, it also presents analytical challenges and limitations that must be taken into account such as the complexity of the matrices, the high sensitivity and selectivity required in the analytical methods as a consequence of the low analyte concentrations as well as the rapid transience of NPS on the drug market creating a scenario with constantly moving analytical targets. Analytical investigation of NPS in pooled urine and wastewater is based on liquid chromatography hyphenated to mass spectrometry and can follow different strategies: target, suspect and non-target analysis. This work aims to discuss the advantages and disadvantages of the different data acquisition workflows and data exploration approaches in mass spectrometry, but also pays attention to new developments such as ion mobility and the use of in-silico prediction tools to improve the identification capabilities in high-complex samples. This tutorial gives an insight into this emerging topic of current concern, and describes the experience gathered within different collaborations and projects supported by key research articles and illustrative practical examples. Image 1 • Determination of NPS in urine and wastewater provide timely complementary information. • Sensitive targeted methodologies play an important role in monitoring NPS use. • HRMS-based analytical strategies permit widening the scope of NPS monitored. • Identification capabilities can be improved by the MS acquisition workflow applied. • Ion mobility separation is an innovative technique that smooths identification. [ABSTRACT FROM AUTHOR]

In this study, a rapid, sensitive and novel nanodrop spectrometric approach is used for the trace level determination of cationic surfactant methyltrioctylammonium chloride (MTOAC) based on the reaction of Mo(III)-SCN− complex with MTOAC in acidic condition. The molar absorptivity of red-colored Mo(III)-SCN− complex was enhanced in the presence of MTOAC that is attributed to a hyperchromic shift. The absorptivity value of the complex with respect to MTOAC is 9.8 × 104 L mol−1 cm−1 at λmax 415 nm. The quality parameters show the good analytical performance of the proposed method with detection limit (LOD) of 8.3 × 10−3 mg L−1 and limit of quantitation of 2.7 × 10−2 mg L−1. The calibration curve for MTOAC determination obeys Beer's law with the concentration limit of 0.05–0.40 mg L−1 and determination coefficient (R2) 0.9992 along with slope and intercept 9.5 and 0.002, respectively. The proposed NDS method has been applied successfully in different environmental and biological samples for the determination of MTOAC. [ABSTRACT FROM AUTHOR]

Tributyltin (TBT) and triphenyltin (TPT) concentrations in water samples from Tanabe Bay were found to range from 4–28 ng l−1 and 3–7 ng l−1, respectively. In fishing ports, the concentrations of TBT in surface water were similar to those in bottom water. However, in aquafarming areas with poor flushing, the concentrations of TBT in bottom water were higher than those in surface water. This suggested that the TBT in water samples is re-eluted from sediment. No difference in the concentration of TPT was observed between the surface and bottom waters. The concentrations of TBT and TPT in sediment samples ranged from 3–23 μg kg−1 dry weight and 2–37 μg kg−1 dry weight. TBT and TPT concentrations ranged from 3.1–100 μg kg−1 and 3.1–7.2 μg kg−1 in oysters and gastropods, and from 1.1–4.9 μg kg−1 and ＜0.2–3.9 μg kg−1 in fish, respectively. Organotin concentrations in biota were lower than the tolerable average residue levels (TARLs). Alternative biocides – i.e. diuron, chlorothalonil, dichlofluanid, irgarol 1051 and Sea-Nine 211 – were also detected in surface water, and chlorothalonil and irgarol 1051 were detected in sediment. The concentrations of these compounds in surface water and sediment were lower than those reported previously. Dichlofluanid, chlorotharonil and irgarol 1051 were also found at low levels in oysters and gastropods, and at ranges of 325–339 μg kg−1, 268–291 μg kg−1 and 43–49 μg kg−1, respectively, in fish; the concentrations in fish were close to the TARL levels. [ABSTRACT FROM AUTHOR]