Journal of pharmaceutical and biomedical analysis最新文献

{"title":"Preparation of amyloid N-terminal nonapeptide imprinted monolithic column and evaluation of adsorption properties","authors":"Zehui Wei ,&nbsp;Wenxin Liu ,&nbsp;Jun Zhang ,&nbsp;Xue Dong ,&nbsp;Shuangxian Yan ,&nbsp;Yu Cheng ,&nbsp;Pingyuan Wei ,&nbsp;Suhong Wang ,&nbsp;Mei Tian","doi":"10.1016/j.jpba.2024.116577","DOIUrl":"10.1016/j.jpba.2024.116577","url":null,"abstract":"<div><div>A novel β-amyloid protein capillary microextraction column was designed and prepared using epitope molecular imprinting technology for specific recognition of trace β-amyloid proteins in complex biological matrices. Using N-terminal nonapeptide of β-amyloid protein as template molecule, choline chloride-MAA and N-hydroxymethyl acrylamide as functional monomers, ethylene glycol dimethacrylate as crosslinker, the imprinted capillary monolithic column was prepared by thermal polymerization in the acetonitrile-water system. The optimal preparation parameters were obtained with the ratio of template: functional monomer: crosslinker at 1:6:16 (mmol/mmol/mmol). The physical property evaluation through Scanning electron microscopy, Fourier transform infrared spectroscopy analysis, zeta potential analysis, particle size analysis, and Brunauer-emmett-teller showed that a porous imprinted monolithic column with a high specific surface area was successfully prepared. The static adsorption experiment showed that the theoretical maximum adsorption capacity was 0.060 μg/column and the optimal imprinting factor was 2.27. Under the optimal extraction conditions, the imprinted column exhibited good template selectivity and excellent robustness. Finally, the extraction efficiency of the capillary imprinted column in actual plasma was evaluated using ELISA method. For Aβ 40 and Aβ 42, the detection limits were 1.00 pg/mL and 0.67 pg/mL, the quantification limits were 3.00 pg/mL and 2.00 pg/mL, the detection ranges were 7.5–120.0 pg/mL and 5.0–80.0 pg/mL, respectively. After extraction of plasma samples, the measured concentrations of Aβ 40 and Aβ 42 by imprinted column were 157.31 pg/mL and 48.22 pg/mL, respectively, which were significantly higher than the measured concentrations by non-imprinted column of 89.60 pg/mL and 41.02 pg/mL. In summary, the epitope imprinted capillary monolithic column prepared in this study can effectively enrich and separate trace amounts of amyloid proteins in complex samples, and is expected to provide a new sample pretreatment method for clinical detection of amyloid proteins.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"254 ","pages":"Article 116577"},"PeriodicalIF":3.1,"publicationDate":"2024-11-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142746116","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Biodegradability of dietary supplements: Advanced analytical methods to study the environmental fate of artificial sweeteners and dyes.","authors":"Luisa Mattoli, Giada Fodaroni, Giacomo Proietti, Enrico Flamini, Bernardino Paoli, Luca Massa, Grazia Carmela Ferrara, Emiliano Giovagnoni, Mattia Gianni","doi":"10.1016/j.jpba.2024.116575","DOIUrl":"https://doi.org/10.1016/j.jpba.2024.116575","url":null,"abstract":"<p><p>Artificial sweeteners (ASs) and dyes are widely used in foods, beverages and pharmaceutical and are recognized as emerging environmental contaminants due to their persistence and widespread occurrence. These substances often pass through the human body unchanged and resist wastewater treatment processes, leading to continuous introduction into aquatic environments and potential long-lasting term environmental effects. This study investigated, for the first time, the biodegradability of nine commercial dietary supplements, both natural and those containing ASs and synthetic dyes, using the Organisation for Economic Cooperation and Development (OECD) 301 F ready biodegradation test (RBT), which is a respirometry-manometric method. While the products showed good biodegradability, those containing ASs and dyes were further studied to determine their fate at the end of the RBT. The study involved developing and validating a chromatographic method to quantitatively determine the presence of Acesulfame K (1), Sucralose (2), Tartrazine (3) and Carmoisine (4) in the RBT mineral medium, using ultra-high performance liquid chromatography (UHPLC) coupled with two detectors: a high-resolution mass-spectrometer with quadrupole time-of-flight (qToF) and a UV-Vis diode array detector (DAD). Results indicated that these additives were not readily biodegraded, highlighting a potential significant environmental concern. This issue extends beyond dietary supplements to all Pharmaceutical and Personal Care Products (PPCP) including drugs and medical devices. The findings underscore the importance of raising cultural awareness about the environmental impact of persistent substances, encouraging the healthcare chain and patients to make informed choices. From a One Health perspective, reducing environmental contamination can lead to positive outcomes for human health.</p>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"255 ","pages":"116575"},"PeriodicalIF":3.1,"publicationDate":"2024-11-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142791961","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Nitrogen dioxide sterilization of a set of five ophthalmic active pharmaceutical ingredients: Impact on impurity profile and content","authors":"Elias Vanneste ,&nbsp;Quinten Speleers ,&nbsp;Anke Meyers ,&nbsp;Karyna Krupianskaya ,&nbsp;Annick Gillet ,&nbsp;Bart Croonenborghs ,&nbsp;Aaron DeMent ,&nbsp;Erik Haghedooren ,&nbsp;Ann Van Schepdael","doi":"10.1016/j.jpba.2024.116578","DOIUrl":"10.1016/j.jpba.2024.116578","url":null,"abstract":"<div><div>Literature about sterilization of pharmaceutical substances is limited. The aim of this study was to evaluate the effect of nitrogen dioxide (NO₂) sterilization, a new emerging technology, on five different ophthalmic active pharmaceutical ingredients, i.e., tetracycline hydrochloride, aciclovir, dexamethasone, methylprednisolone, and triamcinolone. The NO₂ process concentrations tested were 5, 10, and 20 mg/L. The applied temperature was 21 °C and the relative humidity 30 %. The process cycle consisted of two pulses with a dwell time of 10 min each. Non-processed samples were used as a blank. The effect of the sterilization method was assessed by high performance liquid chromatography coupled to an ultraviolet/visible detector, used for the quantitative analysis of the degradation products and the relative content of the evaluated ophthalmic medicines. For tetracycline hydrochloride and aciclovir, an increase of impurities was observed by increasing the NO₂ concentration. The maximum permissible NO₂ concentrations were estimated to be 10 mg/L and 2.5 mg/L, respectively, considering the requirement for the impurities to be within the limit stated in the European Pharmacopoeia (Ph. Eur.). For both compounds, samples subjected to 20 mg/L NO₂ demonstrated a significant difference in content compared to the non-processed sample. For methylprednisolone, dexamethasone, and triamcinolone, impurities complied with the limits of the Ph. Eur. for each NO₂ concentration and relative contents were not significantly affected. Sterilization of tetracycline hydrochloride and aciclovir with NO₂ is not recommended due to extensive degradation. NO₂ sterilization of methylprednisolone, dexamethasone, and triamcinolone could find its application within the aseptic processing procedure of related pharmaceuticals.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"254 ","pages":"Article 116578"},"PeriodicalIF":3.1,"publicationDate":"2024-11-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142701982","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Discovery of potential female-specific biomarkers for major depressive disorder by LC–MS-based metabolomics","authors":"Yi Wang ,&nbsp;Dongcao Xu ,&nbsp;Xinxin Liu ,&nbsp;Mengchun Cheng ,&nbsp;Jingsong Huang ,&nbsp;Dan Liu ,&nbsp;Xiaozhe Zhang ,&nbsp;Lihua Zhang","doi":"10.1016/j.jpba.2024.116572","DOIUrl":"10.1016/j.jpba.2024.116572","url":null,"abstract":"<div><div>The prevalence of major depressive disorder (MDD) is higher in females than males, emphasizing the need to identify gender-specific biomarkers to improve diagnosis accuracy. In this study, a cross-sectional investigation with 258 samples was conducted to evaluate the discriminative power of potential gender-specific biomarkers for MDD. Eighteen MDD-related differential metabolites have been identified, involving pathways of phospholipids, glycerolipids, fatty acids, sphingolipids, cholesterol, vitamin E, and heme. A potential biomarker combination consisting of palmitelaidic acid, gamma carboxyethyl hydroxychroman (gamma-CEHC), and lysoPE(16:0) was confirmed for predicting depression in women using binary logistic regression analysis. To evaluate the panel's specificity, nine generalized anxiety disorder (GAD) samples, which share highly similar clinical symptoms with MDD, were included in the validation set. The discovery and validation sets yielded an area under the receiver operating characteristic curve of 0.86 and 0.83, respectively. All nine female GAD samples were correctly predicted as non-MDD, demonstrating the panel's specificity in diagnosing female MDD. Remarkably, this composite panel achieved a 75 % prediction accuracy in female samples in both the discovery and validation sets, but it did not reach 60 % prediction accuracy in male samples in either set. Our findings highlight the importance of gender-specific molecular diagnostics in developing practical and accurate diagnostic methods for MDD.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"254 ","pages":"Article 116572"},"PeriodicalIF":3.1,"publicationDate":"2024-11-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142701984","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Comparative analysis of various senescence inducers in proximal renal tubular cells","authors":"Piyaporn Rattananinsruang,&nbsp;Chadanat Noonin,&nbsp;Visith Thongboonkerd","doi":"10.1016/j.jpba.2024.116571","DOIUrl":"10.1016/j.jpba.2024.116571","url":null,"abstract":"<div><div>Senescence in renal cells has attracted wide attention as the critical factor promoting renal fibrosis and chronic kidney disease. Establishing a reliable cellular model is essential to study mechanisms underlying renal cell senescence. Herein, we compared various inducers to define the most suitable senescence inducer for HK-2 proximal tubular cells. These inducers included hydrogen peroxide (H₂O₂), high-temperature (HT), glucose, mannitol and hydroxyurea (HU). To screen for optimal concentration/level, the highest concentration/level of each inducer that did not increase cell death (to avoid severe toxicity) was selected for senescence induction and comparative analysis using the two most appropriate markers for HK-2 cell senescence as recently established. The data revealed that 0.4 mM, 43 °C, 80 mM, 80 mM and 100 μM were the optimal concentrations/levels of H₂O₂, HT, glucose, mannitol and HU, respectively. Comparative analysis using optimal concentration/level of each marker revealed that 0.4 mM H₂O₂, HT at 43 °C, 80 mM glucose and 80 mM mannitol were the weak senescence inducers. The most effective inducer for HK-2 senescence was 100 μM HU, which provided the greatest fold-changes of cell area and granularity when compared with other stimuli in a time-dependent manner. Based on these data comparing H₂O₂, HT, glucose, mannitol and HU at their optimal concentrations/levels, 100 μM HU seems to be most effective for senescence induction in HK-2 cells for <em>in vitro</em> study of proximal renal tubular cells.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"254 ","pages":"Article 116571"},"PeriodicalIF":3.1,"publicationDate":"2024-11-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142695529","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Rapid and simple fluorescent detection of chlorogenic acid in Aidi injection using aggregation-induced emission (AIE) nanoclusters","authors":"Pengwei Zhao ,&nbsp;Zhixuan Song ,&nbsp;Yunhan Li ,&nbsp;Xiaorui Liu ,&nbsp;Zhengjin Jiang ,&nbsp;Qing Zhu ,&nbsp;Jia-Huan Qu","doi":"10.1016/j.jpba.2024.116570","DOIUrl":"10.1016/j.jpba.2024.116570","url":null,"abstract":"<div><div>Chlorogenic acid (CGA) is a key component in Aidi injection, known for its anti-cancer properties and ability to reduce toxicity. Therefore, accurate detection of CGA levels in Aidi injection is essential for monitoring therapeutic efficacy and minimizing adverse effects. This study presents a rapid and simple fluorescent method for detecting CGA in Aidi injection using aggregation-induced emission (AIE) nanoclusters, i.e. D(-)-penicillamine (DPA)-capped bimetallic gold/copper nanoclusters (DPA-Au/CuNCs). Upon the addition of CGA, the aggregation state of DPA-Au/CuNCs was disrupted through hydrogen bond formation and ligand exchange, leading to fluorescence quenching. The prepared DPA-Au/CuNCs exhibited a rapid response time of 0.5 min, and demonstrated good sensitivity for CGA, with a limit of detection of 3.75 μg/mL, and a linear detection range of 12.5–200 μg/mL. This method was successfully applied for the analysis of CGA in Aidi injection and plasma with good recovery rates and minimal matrix effect, highlighting its potential for the applications in pharmaceutical products and clinical samples.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"254 ","pages":"Article 116570"},"PeriodicalIF":3.1,"publicationDate":"2024-11-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142682021","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Development and validation of an analytical method for the simultaneous quantitation of posaconazole Form I and Form-S in oral suspensions","authors":"Michail Lykouras ,&nbsp;Christos Kontoyannis ,&nbsp;Malvina Orkoula","doi":"10.1016/j.jpba.2024.116569","DOIUrl":"10.1016/j.jpba.2024.116569","url":null,"abstract":"<div><div>Any polymorphic conversion of an active pharmaceutical ingredient (API), even if partial, is likely to lead to changes in its efficiency and safety. Posaconazole, an antifungal drug, is detected as Form-S in the commercially available oral suspensions. However, a mixture of Form-S and the initial Form I is likely to coexist depending either on the manufacturing process of the suspensions and/or to the storage conditions of the suspension. The simultaneous quantitation of these crystal forms in suspensions is challenging because of the dose inhomogeneity and the instability of Form-S at ambient conditions. Although X-ray Powder Diffraction (XRPD) was initially employed, preferred orientation issues in the suspension inhibited the successful quantitative determination of the polymorphs. In order to circumvent the problem Raman spectroscopy was selected for addressing this challenge, while the additional application of a home-made rotation system reduced the inhomogeneity problems. A separate calibration curve was generated for each polymorph using a conventional linear regression. The combination of these two relations led to the formation of a comprehensive equation relating the characteristic Raman peak intensities of posaconazole Form-S and Form I with the concentrations thereof. The method was validated and the results were confirmed through a partial least square regression (PLSR). The detection limits for Form-S and Form I were determined equal to 1.9 mg/mL and 2.2 mg/mL, respectively.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"254 ","pages":"Article 116569"},"PeriodicalIF":3.1,"publicationDate":"2024-11-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142682052","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Probe electrospray ionization coupled to a quadrupole time-Of-flight: A feasibility study for the detection of cocaine and its derivatives in oral fluid","authors":"Elisa Jousselin ,&nbsp;Elies Zarrouk ,&nbsp;Pauline Griffeuille ,&nbsp;Sylvain Dulaurent ,&nbsp;Souleiman El Balkhi ,&nbsp;Franck Saint-Marcoux","doi":"10.1016/j.jpba.2024.116568","DOIUrl":"10.1016/j.jpba.2024.116568","url":null,"abstract":"<div><div>Probe Electrospray Ionization (PESI) is an atmospheric pressure ionization method that can be directly coupled with a mass spectrometer to allow ultrafast analyses without chromatographic separation and with minimal sample preparation. Using the particular case of cocaine and its metabolites in human oral fluid, the main objective of the present study was to test the feasibility of a new hybrid system combining a PESI source and a quadrupole time-of-flight (QTOF). The best results were obtained for a sample preparation with a simple dilution of 100 µL of oral fluids in an ethanol / 10 mM ammonium formate buffer (50/50) and 10 µL deposited on a dedicated sample plate and introduced into the PESI source. For HRMS acquisition, an approach consisting in a full-mass scan (“untargeted approach” from 100 to 500 <em>m</em>/<em>z</em>; MS1) followed by a targeted scheduled MSMS acquisition (precursor ions of the 3 molecules of interest and their 3 internal standards; MS2) gave the best signals. The total time of analysis was 0.45 min and the method was validated according to ISO15189 standard for a 5–100 ng/mL range, including accuracy and precision (inter-day and intra-day precision and bias values were lower than 15 %), matrix effect, carryover and specificity (no interference with a mixture of 119 psychotropic drugs spiked at 1 mg/L). The LLOD values were 1 ng/mL for the 3 cocaine derivatives and 83 Driving Under the Influence of Drug (DUID) cases sent to our Lab for the determination of illicit drugs in oral fluid were analyzed using the PESI-QTOF method and compared to a LC-MS/MS method. A perfect agreement was observed between the 2 methods, whether the cases were positive or negative. Cocaine was detected in 51 out of these 83 real cases (61.6 %). BZE and EME were also simultaneously detected in 50 of them (98.5 %). This feasibility study reports the first analytical method based on a coupling of a PESI source to a QTOF mass spectrometer. Adding the major advantage of high specificity through HRMS is a step forward for PESI technology.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"254 ","pages":"Article 116568"},"PeriodicalIF":3.1,"publicationDate":"2024-11-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142682018","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Portable Raman spectroscopy and fourier transform near infrared spectroscopy for the quantification of different sinomenine hydrochloride crystal forms","authors":"Zehua Ying ,&nbsp;Zixuan Yan ,&nbsp;Xuting Guo ,&nbsp;Cunhao Li ,&nbsp;Guoxiang Li ,&nbsp;Xingli He ,&nbsp;Wenlong Li","doi":"10.1016/j.jpba.2024.116567","DOIUrl":"10.1016/j.jpba.2024.116567","url":null,"abstract":"<div><div>The objective of this paper is to rapidly and accurately quantify the content of the dominant crystal form of Sinomenine hydrochloride (SH) and to evaluate the respective characteristics of Raman spectroscopy and Fourier transform near infrared spectroscopy techniques for rapid quantification of crystalline substances. In this study, we performed an adulterated gradient quantification based on two new crystalline forms of SH prepared in the laboratory in combination with commercially available products. And established 86 samples containing 66 batches of ternary and 20 batches of binary mixtures. We quantified SH possessing polycrystalline forms based on two kinds of spectroscopy techniques combined with chemometric methods. In the process of establishing the partial least squares quantitative model, according to the experimental design thought, we used the ensemble preprocessing method to screen the optimal preprocessing method for the spectral data of crystal samples. Then we optimized four variable selection methods by single factor investigation. Finally, after completing the PLSR model, we found that the regression models established for both Raman spectra (RMSEP = 0.00672) and FT-NIR spectra (RMSEP = 0.00533) have a high ability to rapidly quantify the crystals.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"254 ","pages":"Article 116567"},"PeriodicalIF":3.1,"publicationDate":"2024-11-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142692437","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Brewer’s spent grain as a potential sorbent for toxicology methods: Application to antidepressant analysis in urine","authors":"Letícia Birk ,&nbsp;Bruno Pereira dos Santos ,&nbsp;Daniela Souza Ossanes ,&nbsp;Patrícia de Souza Schwarz ,&nbsp;Suyanne Angie Lunelli Bachmann ,&nbsp;Viviane Cristina Sebben ,&nbsp;Sarah Eller ,&nbsp;Tiago Franco de Oliveira","doi":"10.1016/j.jpba.2024.116564","DOIUrl":"10.1016/j.jpba.2024.116564","url":null,"abstract":"<div><div>The use of antidepressants is well-documented for several health conditions. The determination of these drugs in biological fluids is often important in intoxication cases. However, appropriate sample preparation needs to be employed, such as dispersive liquid phase microextraction (DSPME). Therefore, this study aimed to develop a method for the determination of antidepressants in urine using Brewer’s spent grain (BSG) as sorbent in a DSPME procedure, followed by GC-MS analysis. In this methodology, only 500 µL of urine was required, alongside 15 mg of BSG as the sorbent for the DSPME technique. Desorption step was performed with 500 µL of ethyl acetate:MTBE solution (1:1, <em>v/v</em>), followed by evaporation of the organic layer, reconstitution in acetonitrile and injection into the analytical system. BSG was further characterized by several analytical techniques. The DSPME procedure was optimized using multivariate strategies, and the method was fully validated according to proper guidelines. Lower limits of quantitation (LLOQ) were set between 50 and 200 ng/mL, while linearity was achieved over the specified range of LLOQ to 5000 ng/mL, with R² ≥ 0.99. Additionally, the method was applied to the analyses of 109 urine samples. Of these, 76 were positive for at least one antidepressant, with the most prevalent being nortriptyline, amitriptyline, and fluoxetine. This study is the first to report the use of BSG as a sorbent for DSPME, demonstrating good efficiency as indicated by the analytical figures of merit. Moreover, the method proved to be applicable in real poisoning case samples. The analytical performance, combined with advantages such as high throughput and a green profile, suggests this method as a valuable alternative for toxicological laboratories.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"254 ","pages":"Article 116564"},"PeriodicalIF":3.1,"publicationDate":"2024-11-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142682049","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}