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Carbamazepine (CBZ) is a widely used pharmaceutical for various purposes, including as an anticonvulsant, antibiotic, and antiepileptic agent, and it undergoes diverse metabolic pathways in both the environment and the human body. Therefore, this study aimed to explore the distribution of CBZ, the presence of its transformation products (TPs), and the transformation pathways in the Mangyeong and Dongjin Rivers in the Saemangeum watershed of Korea using non-targeted screening. The concentration distribution results for CBZ and its TPs showed that the average concentrations in the Mangyeong and Dongjin Rivers were 128.8 ng/L and 89.0 ng/L, respectively. The Mangyeong River exhibited a higher CBZ concentration than the Dongjin River, which was similar to those of the reported CBZ concentrations in other major domestic and international rivers. The types and detection frequencies of the identified TPs exhibited similar trends. The detection frequencies of the TPs decreased in the following order: CBZ-EP > DiOH-CBZ > 10OH-CBZ > 2OH-CBZ > 9-carboxyacridine > 9-acridinecarboxaldehyde. The detection frequency of the main TPs was high, and some were believed to be generated during the water treatment process. The presence of additional TPs (CBZ-O-quinone, acridine, and iminostilbene) was confirmed by the generated molecular networks. This study presents the transformation pathway of the CBZ and provides foundational data for understanding the environmental behavior of TPs, improving wastewater treatment plants, managing water quality, and establishing water environmental policies. [ABSTRACT FROM AUTHOR]

To avoid fraudulent practices, LC-Orbitrap and FT-NIRS combined with multivariate analysis was used to distinguish between 53 Korean and foreign Boston butt samples; forty were used to establish the calibration model and 13 were used as an external validation set. Twenty metabolites were determined to be good indicators of geographic origin. Both LC-Orbitrap with CDA model based on 20 metabolites and FT-NIRS with PLS achieved 100% efficiency in identifying Korean and foreign samples; overall predictive rates for LC-Orbitrap (94.9%) and FT-NIRS (100%). Thus, combined use of LC-Orbitrap and FT-NIRS could be proposed to determine reliably discriminate geographic origins of pork samples.

Triptorelin, a synthetic gonadotrophin-releasing hormone (GnRH), is mainly used in the clinical treatment of prostate cancer. The mechanism initially stimulates luteinizing hormone (LH) and testosterone secretion followed by suppression, resulting in a reduction in cancer progression. However, GnRHs are prohibited in doping control because of the indirect surge of LH and testosterone. Therefore, GnRH analog detection and confirmation are enforced by World Anti-Doping Agency (WADA) requirements. The effects of triptorelin on LH and endogenous steroid levels in urine and serum of five prostate cancer patients taking triptorelin for the first time were investigated and compared with leuprorelin. The samples were collected at 0.0 h, 3.0 h, 6.0 h, 1 month, and 3 months later after drug administration. The effect of triptorelin on LH levels was measured using a sandwich enzyme-linked immunoassay (ELISA). Testosterone and endogenous steroid levels were monitored using gas chromatography coupled with mass spectrometry (GC/MS). Triptorelin showed an advantage over leuprorelin on LH and testosterone suppression, which is preferable to use for prostate cancer treatment. In this study, triptorelin (5-10), a unique in vivo metabolite, was found in urine and serum and verified with synthetic triptorelin (5-10). The metabolite was analyzed using liquid chromatography combined with Orbitrap (LC-Orbitrap) and liquid chromatography coupled with ion trap/time-of-flight mass spectrometry (LC/MS-IT-TOF). When triptorelin levels are undetectable, the presence of triptorelin (5-10) in human urine can be used as evidence that triptorelin is being misused in doping control., (© 2025 The Author(s). Drug Testing and Analysis published by John Wiley & Sons Ltd.)

To avoid fraudulent practices, LC-Orbitrap and FT-NIRS combined with multivariate analysis was used to distinguish between 53 Korean and foreign Boston butt samples; forty were used to establish the calibration model and 13 were used as an external validation set. Twenty metabolites were determined to be good indicators of geographic origin. Both LC-Orbitrap with CDA model based on 20 metabolites and FT-NIRS with PLS achieved 100% efficiency in identifying Korean and foreign samples; overall predictive rates for LC-Orbitrap (94.9%) and FT-NIRS (100%). Thus, combined use of LC-Orbitrap and FT-NIRS could be proposed to determine reliably discriminate geographic origins of pork samples. [ABSTRACT FROM AUTHOR]

Dissolved organic matter (DOM) in aquatic systems is a highly heterogeneous mixture of water-soluble organic compounds, acting as a major carbon reservoir driving biogeochemical cycles. Understanding DOM molecular composition is thus of vital interest for the health assessment of aquatic ecosystems, yet its characterization poses challenges due to its complex and dynamic chemical profile. Here, we performed a comprehensive chemical analysis of DOM from highly urbanized river and seawater sources and compared it to drinking water. Extensive analyses by nontargeted direct infusion (DI) and liquid chromatography (LC) high-resolution mass spectrometry (HRMS) through Orbitrap were integrated with novel computational workflows to allow molecular- and structural-level characterization of DOM. Across all water samples, over 7000 molecular formulas were calculated using both methods (∼4200 in DI and ∼3600 in LC). While the DI approach was limited to molecular formula calculation, the downstream data processing of MS2 spectral information combining library matching and in silico predictions enabled a comprehensive structural-level characterization of 16% of the molecular space detected by LC-HRMS across all water samples. Both analytical methods proved complementary, covering a broad chemical space that includes more highly polar compounds with DI and more less polar ones with LC. The innovative integration of diverse analytical techniques and computational workflow introduces a robust and largely available framework in the field, providing a widely applicable approach that significantly contributes to understanding the complex molecular composition of DOM.

Mycotoxins' exposure by inhalation and/or dermal contact can occur in different branches of industry especially where heavily dusty settings are present and the handling of dusty commodities is performed. This study aims to explore the possible contribution of the occupational exposure to aflatoxins by analysing urine samples for the presence of aflatoxins B1 and M1 and aflatoxin B1-N7-guanine adduct. The study was conducted in 2017 on two groups of volunteers, the workers group, composed by personnel employed in an Italian feed plant (n = 32), and a control group (n = 29), composed by the administrative employees of the same feed plant; a total of 120 urine samples were collected and analysed. A screening method and a quantitative method with high-resolution mass spectrometry determination were developed and fully validated. Limits of detections were 0.8 and 1.5 pg/mLurine for aflatoxin B1 and M1, respectively. No quantitative determination was possible for the adduct aflatoxin B1-N7-guanine. Aflatoxin B1 and its adduct were not detected in the analysed samples, and aflatoxin M1, instead, was found in 14 samples (12%) within the range 1.9–10.5 pg/mLurine. Only one sample showed a value above the limit of quantification (10.5 pg/mLurine). The absence of a statistical difference between the mean values for workers and the control group which were compared suggests that in this specific setting, no professional exposure occurs. Furthermore, considering the very low level of aflatoxin M1 in the collected urine samples, the contribution from the diet to the overall exposure is to be considered negligible. [ABSTRACT FROM AUTHOR]

Demand for honey is increasing, especially if it is organic and if its nutritional properties are linked to untreated environments in order to guarantee quality for health. Sources of contamination of honey can be divided into environmental and apicultural. Therefore, the distribution of persistent organic pollutants, pesticides and antibiotic residues from geographical areas with different contamination sources (high anthropic impact, intensive farming, husbandry and low anthropic impact) was investigated in order to confirm the potential transfer of xenobiotics into the supply chain and to give beekeepers tools for the selection of areas dedicated to organic production. The presence of polychlorinated biphenyls, polybrominated diphenyl ether and polycyclic aromatic hydrocarbons was confirmed, not only in proximity to highly urbanised centres, where the concentrations were higher, but in all environment contexts, confirming their ubiquity. No antibiotics or neonicotinoids were detected in 95 organic honeys, demonstrating the absence of apicultural treatments and consequently the good quality of honey of different areas. These results are important due to the undefined regulatory European situation on honey antibiotic limits. [ABSTRACT FROM AUTHOR]

Abstract: A new method has been developed for the simultaneous determination of 13 tropane alkaloids in tea and herbal teas using high‐performance liquid chromatography coupled to an Exactive‐Orbitrap analyzer. A mixture of methanol, water, and formic acid was used for the extraction of the target compounds followed by a solid‐phase extraction step. The validated method provided recoveries from 75 to 128% with intra‐ and interday precision lower than or equal to 24% (except for apoatropine). Limits of quantification ranged from 5 to 20 μg/kg. Eleven tea and herbal tea samples and two contaminated samples with Datura stramonium seeds were analyzed. Tropane alkaloids were detected in six samples with concentrations from 5 (apoatropine) to 4340 μg/kg (sum of physoperuvine, pseudotropine, and tropine), whereas concentrations from 5 (apoatropine) to 1725 μg/kg (sum of physoperuvine, pseudotropine, and tropine) were found in the contaminated samples. [ABSTRACT FROM AUTHOR]

There are at least 554 identified compounds in C. sativa L., among them 113 phytocannabinoids and 120 terpenes. Phytocomplex composition differences between the pharmaceutical properties of different medical cannabis chemotype have been attributed to strict interactions, defined as ‘entourage effect’, between cannabinoids and terpenes as a result of synergic action. The chemical complexity of its bioactive constituents highlight the need for standardised and well-defined analytical approaches able to characterise the plant chemotype, the herbal drug quality as well as to monitor the quality of pharmaceutical cannabis extracts and preparations. Hence, in the first part of this study an analytical procedures involving the combination of headspace-solid-phase microextraction (HS-SPME) coupled to GC–MS and High Resolution Mass-Spectrometry LC-HRMS (Orbitrap ® ) were set up, validated and applied for the in-depth profiling and fingerprinting of cannabinoids and terpenes in two authorised medical grade varieties of Cannabis sativa L. inflorescences (Bedrocan ® and Bediol ® ) and in obtained macerated oils. To better understand the trend of all volatile compounds and cannabinoids during oil storage a new procedure for cannabis macerated oil preparation without any thermal step was tested and compared with the existing conventional methods to assess the potentially detrimental effect of heating on overall product quality. [ABSTRACT FROM AUTHOR]

Tropane alkaloids are a wide group of substances that comprises more than 200 compounds occurring especially in the Solanaceae family. The main aim of this study is the development of a method for the analysis of the principal tropane alkaloids as atropine, scopolamine, anisodamine, tropane, tropine, littorine, homatropine, apoatropine, aposcopolamine, scopoline, tropinone, physoperuvine, pseudotropine and cuscohygrine in cereals and related matrices. For that, a simple solid-liquid extraction was optimized and a liquid chromatographic method coupled to a single stage Exactive-Orbitrap was developed. The method was validated obtaining recoveries in the range of 60–109% (except for some compounds in soy), precision values (expressed as relative standard deviation) lower than 20% and detection and quantification limits equal to or lower than 2 and 3 μg/kg respectively. Finally, the method was applied to the analysis of different types of samples as buckwheat, linseed, soy and millet, obtaining positives for anisodamine, scopolamine, atropine, littorine and tropinone in a millet flour sample above the quantification limits, whereas atropine and scopolamine were detected in a buckwheat sample, below the quantification limit. Contaminated samples with Solanaceaes seeds ( Datura Stramonium and Brugmansia Arborea ) were also analysed, detecting concentrations up to 693 μg/kg (scopolamine) for contaminated samples with Brugmansia seeds and 1847 μg/kg (atropine) when samples were contaminated with Stramonium seeds. [ABSTRACT FROM AUTHOR]

Neurotransmission plays an essential role during the central nervous system (CNS) development. During the last years, several studies based on the changes produced in neurotransmitters of aquatic organisms caused by pharmaceuticals have been reported. Daphnia magna, the aquatic ecotoxicological model organism, shares several of the neurotransmitters targeted by antidepressant and other neuro-active drugs with vertebrates. Therefore, a method based on liquid chromatography coupled to high-resolution mass spectrometry (LC-HRMS) has been applied for the first time to study the levels of 41 neurotransmitters in Daphnia magna under the effect of four different neuro-active pharmaceuticals (sertraline, venlafaxine, duloxetine and fluoxetine). In addition, the performance of LC-HRMS was studied in terms of linearity, sensitivity, intra- and inter-day precision, and overall robustness. The developed analytical method using LC-HRMS is a new tool for neurotoxicology research using the Daphnia magna model. As a result, general differences on the concentrations of those neurotransmitters exposed to the mentioned pharmaceuticals were observed. Image 1 • Neurotransmitters of Daphnia magna were fully characterized by LC-HRMS. • Good recoveries and excellent sensitivity was achieved for the 44 neurotransmitters. • Pharmaceuticals affected neurotransmitter system of exposed D. magna. • The analytical method developed is a new powerful tool for neurobiology and neurotoxicology. This represents the first study that evaluates the changes produced by pharmaceuticals in the neurotransmitter profiles by using liquid chromatography coupled to high resolution mass spectrometry (LC-HRMS). [ABSTRACT FROM AUTHOR]