Journal of pharmaceutical and biomedical analysis最新文献

{"title":"Glutathione peroxidase-like activity of natural and semisynthetic phenylpropanoids and cannabinoids: An analytical investigation by a GC-MS- and HPLC-DAD-based Iwaoka’s assay","authors":"Chiara Collevecchio,&nbsp;Serena Fiorito,&nbsp;Francesco Epifano,&nbsp;Salvatore Genovese","doi":"10.1016/j.jpba.2026.117381","DOIUrl":"10.1016/j.jpba.2026.117381","url":null,"abstract":"<div><div>The present study explores the glutathione peroxidase (GPx)-like mimicking activity of selected natural phenylpropanoids, their oxyprenylated derivatives, and natural and semisynthetic cannabinoids using a revised version of Iwaoka’s assay based on the application of GC-MS and HPLC-DAD. Thus, naturally occurring phenylpropanoids, including ferulic acid, <em>p</em>-coumaric acid, and umbelliferone, together with their oxyprenylated derivatives, were synthesized and tested for catalytic effects on 1,4-dithiotrhreitol (DTT^red) oxidation. While ferulic acid and <em>p</em>-coumaric acid displayed an appreciable GPx-like activity, their oxyprenylated counterparts exhibited a reduction in catalytic efficiency, suggesting that the carboxylic acid and free phenolic hydroxyl groups play a key role in the observed activity. Coumarin derivatives showed minimal activity, likely due to their rigid ring system. Among cannabinoids, cannabidiol (CBD) and cannabigerol (CBG) enhanced DTT oxidation, with CBG displaying a nearly comparable effect to the reference catalyst Ebselen®. Structure–activity relationship analysis of semisynthetic CBG ethers and esters revealed that substitution patterns strongly influence catalytic performance, with diethyl and di-<em>n</em>-propyl derivatives demonstrating the highest GPx-like behavior. Overall, this work identifies cinnamic acids, CBG, and some of their etherified analogues as promising GPx mimetics and provides mechanistic insight into the redox properties of phenylpropanoids and cannabinoids, which may support future antioxidant drug design.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"272 ","pages":"Article 117381"},"PeriodicalIF":3.1,"publicationDate":"2026-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146078996","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":"Enantioselective high-performance liquid chromatography-tandem mass spectrometry method for bioanalysis and chemical and stereochemical stability study of N-ethylpentedrone","authors":"Saba Jorbenadze ,&nbsp;Tamar Khatiashvili ,&nbsp;Giorgia Sprega ,&nbsp;Aluda Tchelidze ,&nbsp;Vazha Tkemaladze ,&nbsp;Gizo Dolidze ,&nbsp;Simona Pichini ,&nbsp;Magi Farré ,&nbsp;Esther Papaseit ,&nbsp;Melani Nuñez-Montero ,&nbsp;Giuseppe Basile ,&nbsp;Tivadar Farkas ,&nbsp;Francesco Paolo Busardo ,&nbsp;Bezhan Chankvetadze","doi":"10.1016/j.jpba.2026.117375","DOIUrl":"10.1016/j.jpba.2026.117375","url":null,"abstract":"<div><div>The first high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) method was developed for enantioselective analysis of psychoactive compound N-ethylpentedrone. The method also enabled a detection of phase-1 metabolites of N-ethylpentedrone. Enantiomers some of the phase-1 metabolites were also separated. Application of this method to urine and oral fluid samples from the controlled naturalistic clinical study indicated to no enantioselective metabolism and elimination of N-ethylpentedrone. With the developed method a certain chemical and stereochemical instability of N-ethylpentedrone was also shown. Therefore, the observation about non-enantioselective pharmacokinetics of N-ethylpentedrone can be apparent and caused by post-collection racemization of this compound in the studied biological matrices.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"272 ","pages":"Article 117375"},"PeriodicalIF":3.1,"publicationDate":"2026-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146024126","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":"Metabolic profiling of Gegen-Qinlian Decoction and its modified formula in gut microbiota from healthy individuals and ulcerative colitis patients with different syndromes using UHPLC-QTOF-MS/MS and an in vitro incubation model","authors":"Zhitian Peng ,&nbsp;Xinyi Shi ,&nbsp;Ying Peng ,&nbsp;Jiaqi Zhang ,&nbsp;Chongsheng Peng ,&nbsp;Xudong Tang ,&nbsp;Xiaobo Li","doi":"10.1016/j.jpba.2026.117338","DOIUrl":"10.1016/j.jpba.2026.117338","url":null,"abstract":"<div><div>The efficacy of Gegen-Qinlian Decoction (GQD) and its modified formula (MGQD) against ulcerative colitis (UC) with damp-heat syndrome (UC-DHS) is closely linked to gut microbiota-mediated biotransformation. Using UHPLC-QTOF-MS/MS, this study profiled GQD and MGQD in artificial gastrointestinal fluids (AGF) and after incubation with gut microbiota from healthy individuals (HI) and UC patients with spleen deficiency syndrome (UC-SDS) and UC patients with UC-DHS. A custom-built MS data analysis workflow was developed to characterize the metabolic profiles of GQD and MGQD. The profiles comprised metabolized prototype constituents, metabolites, pathways, and metabolic rates. The results showed that GQD/MGQD remained stable in AGF. The HI, UC-SDS, and UC-DHS gut microbiota metabolized 52/60, 39/43, and 35/35 GQD/MGQD prototype compounds, resulting in 25 (GQD) and 28 (MGQD) metabolites common to all groups. All three groups exhibited similar metabolic pathways, predominantly deglycosylation to produce aglycones. However, the HI group demonstrated the highest metabolic capability, followed by UC-SDS and then UC-DHS, with superior metabolic rates, lower residual compounds, and higher metabolite abundance. Notably, the addition of two herbs to MGQD did not alter the core metabolic pathways of GQD-sourced constituents but inhibited the biotransformation of certain constituents. Further analysis revealed that glycoside metabolic rates depended on structural features: flavonoid glycosides were metabolized fastest, followed by phenylethanoid glycosides and saponins; among sugar moieties, glucosides were fastest, followed by glucuronides, xylosides, arabinosides, and apiosides. This study reveals the metabolic profiles of GQD/MGQD across different gut microbiota groups (HI, UC-SDS, UC-DHS) and provides a practical analytical workflow for herb-microbiota interaction research.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"272 ","pages":"Article 117338"},"PeriodicalIF":3.1,"publicationDate":"2026-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146078998","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":"Exploring the therapeutic potential of Anoectochilus roxburghii in glucose and lipid metabolism disorder: From phenotypic effects to molecular mechanisms and network pharmacology","authors":"Wei Li ,&nbsp;Yaqian Cheng ,&nbsp;Tong Wu ,&nbsp;Chenning Zhao ,&nbsp;Qingsong Shao ,&nbsp;Lanying Pan ,&nbsp;Ying Zheng","doi":"10.1016/j.jpba.2026.117360","DOIUrl":"10.1016/j.jpba.2026.117360","url":null,"abstract":"<div><div>Dysregulation of glucose and lipid metabolism has emerged as a leading cause of cardiovascular diseases worldwide. The current treatment for these diseases is often a combination of drugs. Despite the preference efficacy of combination therapies, adverse reactions have been frequently reported, such as gastrointestinal bleeding. <em>Anoectochilus roxburghii</em> (Wall.) Lindl<em>.</em>, one of the traditional Chinese medicines, is recognized for its hypolipidemic and hypoglycemic effects. However, the exact therapeutic potential of <em>A. roxburghii</em> in glucose and lipid metabolism remains unsolved. By employing <em>in vitro</em> and <em>in vivo</em> experiments, this study evaluated the pharmacological activities of <em>A. roxburghii</em> and identified the primary active compounds involved in glucose and lipid metabolism. The results indicated that <em>A. roxburghii</em> can ameliorate dysregulation in glucose and lipid metabolism by promoting glycogen synthesis, and inhibiting gluconeogenesis and fatty acid oxidation. Using UHPLC-QE-MS, a total of 662 compounds were detected in the aqueous extract of <em>A. roxburghii</em>, and 769 were identified in the ethanol extract. Key ingredients such as morin and kaempferol participated in glucose metabolism, while kinsenoside and naringenin modulating lipid metabolism. Furthermore, <em>A. roxburghii</em> may potentially intervene in the insulin resistance signaling pathway by influencing TP53 protein expression, thereby modulating glucose metabolism process. This research provides evidence for the development and application of <em>A. roxburghii</em> as potential drugs in the treatment of glucose and lipid disordered diseases.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"272 ","pages":"Article 117360"},"PeriodicalIF":3.1,"publicationDate":"2026-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145980443","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":"Elucidating the effects of ginger processing on Magnolia bark: A multi-platform strategy linking chemical composition to taste and bioactivity","authors":"Zhiyan Xie ,&nbsp;Haochen Wu ,&nbsp;Huixian Qing ,&nbsp;Yu Yin ,&nbsp;Zicheng Ma ,&nbsp;Guoqin Zhang ,&nbsp;Meiqi Liu ,&nbsp;Shiwei Chai ,&nbsp;Xiaoliang Ren","doi":"10.1016/j.jpba.2026.117333","DOIUrl":"10.1016/j.jpba.2026.117333","url":null,"abstract":"<div><div><em>Magnolia officinalis</em> (Houpo, HP) is a prominent Traditional Chinese Medicine(TCM). Despite its traditional processing with ginger to reduce irritation, enhance efficacy, and improve taste, the underlying mechanisms connecting this chemical transformation to its sensory and gastrointestinal effects are not fully understood. Existing studies lack systematic analysis of shared targets across gastrointestinal diseases and the identification of quality markers (Q-markers), limiting scientific justification for its processing and clinical use. This study therefore applied an integrated UPLC-Q-TOF/MS, chemometrics, and network pharmacology approach to elucidate the effects of ginger processing. In this study a total of 46 batches of samples (22 raw, 24 ginger-processed) were analyzed by UPLC-Q-TOF/MS to identify and quantify chemical constituents. Chemometric models were used to discriminate sample types and identify potential Q-markers. The correlation between taste and chemical profiles was assessed using an electronic tongue combined with Pearson correlation analysis. Network pharmacology was employed to predict targets related to functional dyspepsia (FD), postoperative nausea and vomiting (PONV), and chronic gastritis (CG), followed by GO/KEGG enrichment analysis. Molecular docking was performed to validate binding affinities between key bioactive components and core targets. The experimental results showed that Fifty-four compounds were characterized, and chemometric models clearly distinguished raw from ginger-processed HP (Jianghoupo, JHP). Electronic tongue analysis revealed that Magnoloside A plays a key role in reducing bitterness after ginger processing. Network pharmacology identified 51 overlapping targets across FD, PONV, and CG, with AKT1, TNF, CTNNB1, IL1B, and STAT3 as core nodes in the network. Molecular docking confirmed stable binding between principal components and these targets. An integrative “component transformation–taste modulation–gastrointestinal regulation” model was established, illustrating how ginger processing improves both palatability and pharmacological efficacy. In summary, ginger processing transforms the chemical and sensory profiles of HP into a state of improved palatability and strengthened gastrointestinal regulatory function. These findings provide a mechanistic rationale and scientific foundation for the traditional processing practice of combining ginger with HP in clinical use.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"272 ","pages":"Article 117333"},"PeriodicalIF":3.1,"publicationDate":"2026-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145928867","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":"Integrated dual-molecular marker analysis with SSR and UPLC-Q-TOF/MS fingerprints technology reveal the interrelation of the molecule-metabolite in Morus alba L. leaves","authors":"Yuqing Tian ,&nbsp;Pei Ma ,&nbsp;Liang Wang ,&nbsp;Bei Song ,&nbsp;Jinghua Yang ,&nbsp;Dan Qian ,&nbsp;Wei Guo","doi":"10.1016/j.jpba.2026.117359","DOIUrl":"10.1016/j.jpba.2026.117359","url":null,"abstract":"<div><div><em>Morus alba</em> L. (<em>M. alba</em>) leaves, valued for their medicinal and edible properties, possess substantial economic and social importance. Notably, diverse germplasm resources of <em>M. alba</em> exhibit considerable variation in both metabolite composition and pharmacological activity. However, the interrelationships among genetic diversity, metabolites profiles, and pharmacological activity across different <em>M. alba</em> varieties remain insufficiently elucidated. This study aimed to construct simple sequence repeat (SSR) and ultra-high performance liquid chromatography quadrupole time of flight mass spectrometry (UPLC-Q-TOF/MS) fingerprints, together with antipyretic clustering diagrams, for 69 different varieties of <em>M. alba</em> leaves, and analyze the correlations among their genetic structures, metabolite profiles, and antipyretic activities. In this study, 69 <em>M. alba</em> leaf samples representing different varieties were collected, and their antipyretic effects were evaluated using a rat pharmacodynamic model. SSR fingerprints were generated with TP-M13 SSR molecular markers to screen core primer pairs for variety identification. Simultaneously, metabolite fingerprints were established using UPLC-Q-TOF/MS with common peaks calibrated and compounds qualitatively identified by mass spectrometry. Finally, multivariate chemometric approaches were applied to integrate SSR data and UPLC-Q-TOF/MS fingerprint profiles, and antipyretic activity results for clustering and correlation analysis. The dominant <em>M. alba</em> varieties, Yantai 792, Zhesang 3, 8036, Fengyuan 1, Laiwugusang, Xiajingusang, Gaoqing 792, Zhesang 1 and Heizhenzhu exhibited the strongest antipyretic activities. In contrast, Guiyou, Danbaisang, and Dashi showed weaker effects and were clustered into a single category in the molecule-metabolite-efficacy clustering diagram, thereby indicating the substantial influence of varieties differences on genetic diversity, metabolite composition, and pharmacological activity. Pearson correlation analysis further confirmed significant correlations among genetic components, metabolites, and pharmacological effects. In addition, a core marker set comprising 7 SSR loci was identified, together with 8 key chemical markers including cryptochlorogenic acid, neochlorogenic acid, isoquercitrin, rutin, nicotiflorin, astragalin, salicylic acid, and umbelliferone. These findings help identify the “molecule-metabolite” dual molecular markers with the bias of antipyretic effects for <em>M. alba</em> leaves varieties, and provide valuable insights for refining the medicinal value of <em>M. alba</em> leaves and promoting the utilization of high-value resources.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"272 ","pages":"Article 117359"},"PeriodicalIF":3.1,"publicationDate":"2026-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145981049","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":"Identification of metabolites from the Himalayan herbal medicine Meconopsis integrifolia total flavonoids fraction in rats using UPLC-Q-exactive orbitrap-MS analysis","authors":"Enhui Ji ,&nbsp;Yuan Liu ,&nbsp;Yifan Tian ,&nbsp;Limin Li ,&nbsp;Pei Qun ,&nbsp;Zhengming Yang ,&nbsp;Chaoqin Ren ,&nbsp;Yanfei Huang ,&nbsp;Yongcang Zhang","doi":"10.1016/j.jpba.2026.117357","DOIUrl":"10.1016/j.jpba.2026.117357","url":null,"abstract":"<div><div><em>Meconopsis integrifolia</em> total flavonoids (MITF) have been identified as the hepatoprotective fraction of <em>M. integrifolia</em>, with its main components being flavonoid glycosides, along with lower levels of phenolic acids and alkaloids. Since flavonoid glycosides are poorly absorbed <em>in vivo</em>, metabolism serves as a crucial pathway for their biotransformation. However, the metabolism and material basis of pharmacological effects of MITF <em>in vivo</em> remain unknown. In this study, ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry was used to investigate the metabolic profiles of MITF. A total of 61 absorbed prototype compounds were identified, including 54 in feces (43 flavonoids, 8 phenolic acids, and 3 alkaloids), 8 in urine (2 flavonoids, 3 phenolic acids, 3 alkaloids), and 6 in plasma (2 flavonoids, 4 phenolic acids). Furthermore, 113 metabolites were characterized, including 64 in feces (38 flavonoids, 11 phenolic acids, 15 alkaloids), 46 in urine (17 flavonoids, 16 phenolic acids, 13 alkaloids), and 14 in plasma (5 flavonoids, 9 phenolic acids). The major metabolic pathways were dehydroxylation, hydroxylation, reduction, dehydrogenation, hydration, dehydration, methylation, sulfation, and glucuronidation. The results indicated that the biotransformation and absorption of flavonoids <em>in vivo</em> were limited. In contrast, phenolic acids and alkaloids were extensively absorbed. This research provides crucial insights into the metabolic fate of MITF in rats, thereby clarifying the pharmacologically active substances derived from <em>M. integrifolia</em>.</div></div><div><h3>Data availability</h3><div>The data that support the findings of this study are available on request from the corresponding author. The data are not publicly available due to privacy or ethical restrictions.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"272 ","pages":"Article 117357"},"PeriodicalIF":3.1,"publicationDate":"2026-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145980445","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":"Chemical profiling and multi-dimensional pharmacokinetic analysis of shengmaiyin oral liquid for cardiac dysfunction","authors":"Lifeng Zhao ,&nbsp;Siyang Wu ,&nbsp;Xin Yu ,&nbsp;Zhishan Huang ,&nbsp;Luyang Liu ,&nbsp;Xuehao Cheng ,&nbsp;Zheng Yuan ,&nbsp;Yingfei Li","doi":"10.1016/j.jpba.2026.117378","DOIUrl":"10.1016/j.jpba.2026.117378","url":null,"abstract":"<div><div>Shengmaiyin oral liquid (SMY), formulated with schisandra chinensis, red ginseng, and Ophiopogon japonicus, is widely used for treating cardiac dysfunction (CD). However, its functional chemical basis and pharmacological profiles remain insufficiently explored. This study employed advanced analytical strategies to characterize the bioactive components of SMY and investigate their in silico pharmacodynamics and in vivo pharmacokinetics, providing mechanistic insights into their roles in CD treatment. Using UPLC-Q-TOF-MS/MS, 132 compounds were identified in SMY, with 31 detected in the plasma of SMY-treated mice. Among these, 21 chemicals (12 lignans and 9 saponins) were identified as key bioactives against CD. Network pharmacology and molecular docking revealed their multi-target interactions and varied binding affinities with CD-related proteins. Pharmacokinetic (PK) analysis showed that 5 compounds had high plasma exposure and rapid elimination in CD model mice. All 21 chemicals exhibited significant tissue distribution following prolonged SMY administration. The globally pharmacokinetic seeking (GPS) box analysis revealed two distinct fast and slow PK patterns among the chemicals. Notably, a highly tissue-specific and time-dependent alteration of lignan and saponin clusters was observed in the hearts of CD mice within 8 h post-administration. This study highlights the GPS box as an innovative platform for multi-dimensional PK analysis. These findings advance the integration of traditional herb medicine with modern analytical methodologies, offering new perspectives for developing precision medicine approaches in ethnopharmacology.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"272 ","pages":"Article 117378"},"PeriodicalIF":3.1,"publicationDate":"2026-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146078997","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":"Ease of analysis through unification: One gas chromatographic method for the chemical profiling of essential oils","authors":"Dominik Kresnik,&nbsp;Bryan Bajor,&nbsp;Christian Steuer","doi":"10.1016/j.jpba.2026.117350","DOIUrl":"10.1016/j.jpba.2026.117350","url":null,"abstract":"<div><div>The rising interest in essential oils (EOs) for their therapeutic, antibacterial, and antifungal properties has led to an increasing demand for high-quality products in both medicinal and industrial sectors. To meet these stringent quality requirements, robust, precise, and efficient analytical methods are essential. Gas chromatography (GC) remains the gold standard for EO analysis due to its sensitivity and resolution. Although numerous methods are available –primarily targeting similar analytes in varying combinations standardization remains a challenge, with protocols differing across ISO guidelines and international pharmacopoeias. In this study, Design of Experiments (DoE) was employed to optimize and harmonize existing GC methods, focusing on sample preparation and chromatographic parameters. A polar GC column (60 m length, 0.25 mm inner diameter, 0.25 µm film thickness) was selected for its ability to effectively separate 87 terpenes, sesquiterpenes, and related compounds commonly found in EOs. The optimized temperature gradient enabled complete separation within a 75-minute runtime, outperforming or matching existing methods in terms of resolution and reproducibility. Streamlined sample preparation protocols led to reduced solvent consumption and minimized sample requirements across all tested EOs. As a proof of concept, the final method was applied to 12 different essential oils, demonstrating comparable analytical performance and confirming its broad applicability and efficiency.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"272 ","pages":"Article 117350"},"PeriodicalIF":3.1,"publicationDate":"2026-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145981048","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":"Identification and characterization of trametinib degradation product employing Orbitrap LC-HRMS, and development of a robust, eco-friendly stability indicating method of analysis","authors":"Sohan G. Jawarkar ,&nbsp;Gayatri Amliyar ,&nbsp;Nasir Khan,&nbsp;Pooja Dhakne,&nbsp;Megha Pillai,&nbsp;Shankha Dey,&nbsp;Jinal Ajabiya,&nbsp;Pinaki Sengupta","doi":"10.1016/j.jpba.2026.117355","DOIUrl":"10.1016/j.jpba.2026.117355","url":null,"abstract":"<div><div>Trametinib is a selective MEK1/2 inhibitor approved for the treatment of various cancers. Stress testing of a drug is essential for understanding the stability profile and ensuring compliance with regulatory requirements during pharmaceutical development. To the best of our knowledge, only a few reports on stress testing of trametinib are available to date. Moreover, comprehensive reports on the stress testing of trametinib using LC-HRMS are not available in any literature. Therefore, the present study aimed to conduct stress studies on trametinib in accordance with ICH guidelines. The RP-HPLC stability-indicating analytical method was developed, and the stress degradation condition for trametinib was optimised. Chromatographic separation of trametinib and its degradation products was achieved on a Phenomenex Luna C18 column (250 × 4.6 mm, 5 µm) using a mobile phase consisting of 0.1 % formic acid in Milli-Q water and acetonitrile using gradient elution. The proposed method demonstrated excellent specificity, linearity, precision (RSD ≤ 0.09 %), and accuracy (99.78–101.38 %). Results indicate that trametinib exhibited high susceptibility to acidic and basic stress conditions, whereas it remained relatively stable under oxidative and thermal stress conditions. All degradation products were characterised using Orbitarp LC-HRMS in positive HESI mode (<em>m/z</em> 50–800 Da) for accurate mass determination and fragmentation pathway elucidation. <em>In-silico</em> toxicity prediction suggested that among the degradation products, neurotoxicity was the most consistently predicted endpoint with high confidence (≥70 %), followed by respiratory toxicity and immunotoxicity. Greenness evaluation using AGREE, Eco-Scale, and BAGI tools indicated a moderate environmental impact.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"272 ","pages":"Article 117355"},"PeriodicalIF":3.1,"publicationDate":"2026-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146018804","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}