Journal of pharmaceutical and biomedical analysis最新文献

{"title":"A novel data fusion strategy of LC-MS and NMR technologies using random forest model for emodin hepatotoxic metabolomics research","authors":"Yuxin Zhang ,&nbsp;Haitao Wang ,&nbsp;Rui Mao ,&nbsp;Biying Chen ,&nbsp;Miaomiao Jiang","doi":"10.1016/j.jpba.2025.116990","DOIUrl":"10.1016/j.jpba.2025.116990","url":null,"abstract":"<div><div>Data fusion is a process of integrating data matrices from different detection sources into a comprehensive model, which can more comprehensively mine the characteristics of samples and provide the possibility of obtaining more accurate classification. In our previous study, liquid chromatography-mass spectrometry (LC-MS) and nuclear magnetic resonance (NMR) techniques were used to investigate liver metabolomics before and after emodin administration. However, the classification effect between groups of emodin with different durations of administration was not ideal. In this study, principal component analysis, partial least squares discrimination analysis, support vector machine, <em>k</em>-nearest neighbor, neural network, decision tree, and random forest (RF) algorithms were applied for building low-level (LLDF) and mid-level data fusion (MLDF) models. The model classification effects of both the single data set and LLDF were poor, while the separation effect of the MLDF model was significantly improved, among which an RF model established after combining the features selected by the RF model (RF-RF) had the best classification effect. This was the first study to apply LC-MS and NMR data fusion techniques to emodin hepatotoxic metabolomics research, to explore the differential metabolites at a more comprehensive and deeper level, and to provide a research basis for subsequent mechanism studies.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"264 ","pages":"Article 116990"},"PeriodicalIF":3.1,"publicationDate":"2025-05-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144169364","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":"Discovering the metabolic pathway of liver disease by breath mass spectrometry combined with machine learning","authors":"Xuanzhu Li ,&nbsp;Wenbo Zhang ,&nbsp;Tongtong Yang ,&nbsp;Ying Zhang ,&nbsp;Rui Su","doi":"10.1016/j.jpba.2025.116988","DOIUrl":"10.1016/j.jpba.2025.116988","url":null,"abstract":"<div><div>On account of the low concentration and complex background, most methods for detecting VOCs in exhaled breath samples required preconcentration prior to instrumental analysis. In the current study, a simple and rapid method is developed for analyzing the volatile organic compounds (VOCs) in exhaled breath by extractive electrospray ionization mass spectrometry (EESI-MS). Partial least square discriminant analysis (PLS-DA) using full scan mass spectrum data was used to distinguish exhaled breath of healthy volunteers, chronic hepatitis B patients, and liver failure patients. More VOCs were detected in exhaled breath samples from the volunteers including healthy adults, chronic hepatitis B patients, and liver failure patients by the enclosed EESI-MS method without any sample pretreatment in comparison to the traditional methods. The 9 new breath markers, including 2-hydroxyethanal, 2-methylpropene, butan-2-one, 2,5-dimethylfuran, 2-ethylprop-2-enoic acid, 2,4-dimethylpyridine, 2-methylbutanoic acid, cyclopentanone and 5-hexanolactone, were identified using high resolution tandem mass spectrometry, and some highly correlated metabolic pathways including tryptophan metabolism, tyrosine metabolism, butanoate metabolism, and fatty acid biosynthesis were found. EESI-MS² method, a promising non-invasive diagnostic tool, is robust and suitable for analysis of VOCs, and may provide further insight into the pathophysiologic processes and pathways leading to chronic hepatitis B and its complications.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"265 ","pages":"Article 116988"},"PeriodicalIF":3.1,"publicationDate":"2025-05-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144168916","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":"Analytical quality by design and measurement uncertainty in the development of discriminative dissolution method for pediatric fixed-dose combination dispersible tablets of isoniazid and rifampicin","authors":"Monique Silva dos Santos ,&nbsp;Diogo Dibo do Nascimento ,&nbsp;Juliana Johansson Soares Medeiros ,&nbsp;Felipe Rebello Lourenço ,&nbsp;Camila Areias de Oliveira ,&nbsp;Livia Deris Prado","doi":"10.1016/j.jpba.2025.116994","DOIUrl":"10.1016/j.jpba.2025.116994","url":null,"abstract":"<div><div>Analytical Quality by Design (AQbD) is a proactive approach that ensures the consistent performance of analytical methods throughout the lifecycle. The application of AQbD in dissolution testing remains limited, particularly with the incorporation of measurement uncertainty to minimize risks for both consumers and producers. This study applied AQbD principles to develop a dissolution method for a fixed-dose combination of isoniazid (INH) and rifampicin (RIF) in dispersible tablets. The Analytical Target Profile was defined based on the dissolved percentage of INH and RIF. A risk-based approach was used to assess risks impacting the discriminative power and measurement uncertainty. design of experiments optimized medium pH, volume and rotation speed, considering two experimental batches. With Monte Carlo simulations, the Method Operable Design Region was constructed to allow batch A approval and batch B failure. Validation confirmed that the methods were selective, precise and accurate, with combined standard uncertainties of 1.7 % for INH and 3.8 % for RIF. The guard bands defined new acceptance limits in the three stages of dissolution, minimizing both consumer and producer risks. A hazard analysis and critical control point plan was established as a control strategy. If the dissolved percentage of RIF or INH leads to a batch failure, two options are possible: retesting or discarding the batch, considering guard bands to ensure a producer risk lower than 5 %. The study innovates by demonstrating the relevance of incorporating AQbD in dissolution testing, ensuring more reliable methods for controlling product quality.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"265 ","pages":"Article 116994"},"PeriodicalIF":3.1,"publicationDate":"2025-05-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144169422","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":"Simultaneous analysis of four endocannabinoids and endocannabinoid congeners together with delta-9 tetrahydrocannabinol and related metabolites in dried blood spots","authors":"Alexandr Gish ,&nbsp;Jean-François Wiart ,&nbsp;Camille Richeval ,&nbsp;Delphine Allorge ,&nbsp;Jean-michel Gaulier","doi":"10.1016/j.jpba.2025.116991","DOIUrl":"10.1016/j.jpba.2025.116991","url":null,"abstract":"<div><div>In the medical field, the endocannabinoid system is both a difficult and hot topic for scientific and media reasons (cannabis, cannabidiol, etc.). Due to their instability and low concentrations in blood and physicochemical properties, the complexity of endocannabinoid assay is previously reported in different matrices. This study aims to report a LC-MS/MS method for the simultaneous quantification of four endocannabinoids and endocannabinoid congeners: <em>N-</em>arachidonoylethanolamide (anandamide or AEA), 2-arachidonoylglycerol/1-arachidonoylglycerol (2-AG/1-AG), oleoylethanolamide (OEA) and palmitoylethanolamide (PEA), together with Δ9-tetrahydrocannabinol (THC) and its main metabolites [11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THC-COOH) and 11-hydroxy- Δ9-tetrahydrocannabinol (11-OH THC] in Dried Blood Spot (DBS). This validated method reported LLOQs of 0.1 µg/L for AEA, 0.5 µg/L for THC and 11-OH THC, and 1 µg/L for OEA, PEA, 2AG and THC-COOH. The method demonstrated intra- and interassay accuracy and precision of less than 20 % for the LLOQ, and less than 15 % for the other calibration points. In particular, the stability carried out in this study demonstrated the practical applicability of DBS for the measurement of endocannabinoids in the whole blood. Therefore, we propose this method as a tool for basic and clinical research to support the growing interest of the scientific community in the endocannabinoid system.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"265 ","pages":"Article 116991"},"PeriodicalIF":3.1,"publicationDate":"2025-05-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144168915","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":"Mechanistic insights into Licorice-Evodiae Fructus interaction: UPLC-MS/MS-based hepatotoxic metabolite detection and CYP3A4 regulation study","authors":"Xiaofei Chen ,&nbsp;Tianwang Wang ,&nbsp;Kai Wang ,&nbsp;Ting Peng ,&nbsp;Yanan Zhang ,&nbsp;Xiaoliang Ren","doi":"10.1016/j.jpba.2025.116985","DOIUrl":"10.1016/j.jpba.2025.116985","url":null,"abstract":"<div><div>Evodiae Fructus (EF) is a hepatotoxic herbal medicine whose toxicity is linked to CYP3A4-mediated metabolic activation of evodiamine (EVD), as identified in our previous study using high-resolution MS platform. In clinic, EF is often combined with Licorice to enhance efficacy and reduce toxicity, but the detoxification mechanism is unknown. In this study, we developed an integrated analytical strategy combining multi-mass spectrometry techniques and biological experiments to investigate the detoxification mechanism of Licorice-EF combination. The changes in EVD serum contents, biochemical indexes and pathological sections in rats were monitored after Licorice administration, and correlation analysis was performed to clarify the detoxification effect of Licorice. In addition, the effect of the major components in Licorice on P450 enzymes and the electrophilic metabolites derived from EVD were investigated by combined application of UPLC-QQQ-MS/MS and UPLC-Q/TOF-MS/MS. Our study showed that the combined use of Licorice and EF in the ratio of 1:1 could significantly ameliorate EF-induced liver injury. The Licorice extract mainly inhibited the activities of CYP3A4, with isoliquiritigenin (ILG) exhibiting the most inhibitory potency with enzyme kinetics parameters k_inact and K_I at 0.034 min⁻¹ and 0.63 μM, respectively. Furthermore, ILG not only significantly alleviated EVD-induced liver injury, but also obviously reduced the production of EVD-derived reactive metabolites. These results suggested that Licorice alleviated EF-induced liver injury by inhibition of metabolic activation of EF mediated by cytochrome P450s, providing stringent and scientific evidence for such combination from perspectives of metabolism-based interaction.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"264 ","pages":"Article 116985"},"PeriodicalIF":3.1,"publicationDate":"2025-05-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144134732","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":"An investigation of the plasma and urinary metabolite profiles of the hepatotoxin methapyrilene in the male Wistar rat","authors":"Robert S. Plumb ,&nbsp;Steven K. Lai ,&nbsp;Lee A. Gethings ,&nbsp;Robert Trengove ,&nbsp;Peter Hancock ,&nbsp;Ian D. Wilson","doi":"10.1016/j.jpba.2025.116976","DOIUrl":"10.1016/j.jpba.2025.116976","url":null,"abstract":"<div><div>The plasma and urinary metabolite profiles of the 2-thiophene-based H1-receptor antagonist methapyrilene (<em>N</em>,<em>N</em>-dimethyl-<em>N</em>'-pyridin-2-yl-<em>N</em>'-(thiophen-2-ylmethyl)ethane-1,2-diamine) were investigated in the rat following the oral administration of 0, 50 or 150 mg/kg/day of the drug for 5 days. The systemic exposure and metabolic fate of methapyrilene were investigated initially using a rapid “fit for purpose” reversed-phase (RP) UHPLC-MS/MS assay followed by a more in-depth characterization of its metabolites using RP-UHPLC coupled to a high resolution multi reflecting time of flight mass spectrometer. No detectable methapyrilene was present in plasma when measured on days 1, 3 and 5, at any dose, using samples obtained 24 h post administration. However, methapyrilene-derived metabolites were detected, in increasing amounts, in these plasma samples on days 3 and 5 of the study. Both methapyrilene and large numbers of metabolites were present in the urines collected 24 h after dosing on days 3 and 5. The profiles of these metabolites were both dose and time dependent. From the urine and plasma profiles obtained using both +ve and -ve ESI HRMS some 24 metabolites were characterized showing functionalization by aliphatic and aromatic hydroxylation, <em>N</em>-oxidation, <em>N</em>-demethylation and loss of the thiophene ring. Glucuronic acid, glycine and glutathione-derived conjugates were also detected.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"264 ","pages":"Article 116976"},"PeriodicalIF":3.1,"publicationDate":"2025-05-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144154422","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":"Immobilization of human myeloperoxidase on silica gel for inhibitors assessment","authors":"Yalda Cobra Parsajoo ,&nbsp;Cédric Delporte ,&nbsp;Karim Zouaoui Boudjeltia ,&nbsp;Jean-Michel Kauffmann ,&nbsp;Pierre Van Antwerpen","doi":"10.1016/j.jpba.2025.116974","DOIUrl":"10.1016/j.jpba.2025.116974","url":null,"abstract":"<div><div>Myeloperoxidase (MPO), a hemo-protein present in neutrophils and monocytes, significantly contributes to immune responses against microbial pathogens. Increased MPO activity, however, promotes the production of highly reactive oxidized species in extracellular fluids that can damage host tissues causing inflammatory events. To explore the potential of MPO as a target for inhibitor screening, this study aimed to develop and evaluate a mini-reactor system based on immobilized MPO. Several immobilization strategies including physical adsorption and covalent binding, were tested using silica gel as the support material. Among them, immobilization via cyanogen bromide (CNBr) activation was selected as the optimal method based on long-term stability (&gt; 90 % after 20 runs) and a relative activity of 60 % after immobilization. Kinetic parameters for H₂O₂ were determined to characterize the enzymatic behavior post-immobilization, including K_mapp and V_max (46 ± 4 µM and 463 ± 38 µM/min, respectively). The system was then employed to evaluate the inhibitory potency (IC₅₀) of three model compounds—salicylhydroxamic acid (SHA), paroxetine (PARO), and 4-aminobenzohydrazide (4-ABAH)—on HOCl production in the presence of 10 µM H₂O₂. 4-ABAH emerged as the most potent irreversible inhibitor (IC₅₀ = 0.30 µM), while SHA was the least effective (IC₅₀ = 27.10 µM). Those results demonstrated that immobilized-MPO preserved its activity and exhibited good stability. This mini-reactor provides a reliable platform for inhibitor studies, offering potential applications in screening therapeutic compounds to mitigate MPO-related inflammatory conditions.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"264 ","pages":"Article 116974"},"PeriodicalIF":3.1,"publicationDate":"2025-05-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144108024","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":"Multi-omics analysis reveals classic decoction alleviates ulcerative colitis by modulating tryptophan metabolism, gut microbiota homeostasis, and mitochondrial Bax/Bcl-2 pathways","authors":"Xujin Yang ,&nbsp;Shen Peng ,&nbsp;Ping Wang ,&nbsp;Yi Tao","doi":"10.1016/j.jpba.2025.116972","DOIUrl":"10.1016/j.jpba.2025.116972","url":null,"abstract":"<div><div>Gegen Qinlian Decoction (GQD), a classic decoction documented in the Treatise on Febrile Diseases, is clinically used to treat ulcerative colitis (UC). However, the active components and underlying pharmacological mechanisms of GQD in UC remain inadequately explored. Herein, we identify the active components and elucidate the underlying pharmacological mechanisms of GQD in the treatment of UC. A mouse model of UC was induced using dextran sulfate sodium (DSS) and treated with low, medium, and high doses of GQD. The therapeutic effects were assessed by monitoring body weight, disease activity index (DAI), colon length, spleen index, pathological changes, and cytokine levels. Plasma biomarkers were analyzed using Ultra-Performance Liquid Chromatography Quadrupole-Orbitrap mass spectrometer (UPLC-Q-Orbitrap MS)-based metabolomics. Changes in gut microbiota were also examined to identify key microbes involved in the intestinal pathological shifts. Additionally, network pharmacology analysis was conducted to predict the potential pathways of GQD in UC, which were subsequently validated by western blotting and ELISA assays. GQD significantly improved UC symptoms.A total of 98 chemical constituents in GQD were identified. Of these, 25 differential metabolites were found between normal and UC mice, with GQD modulating 22 of these metabolites. Metabolic pathways related to tryptophan, arginine, and proline were normalized. Network pharmacology predicted the apoptosis pathway as a potential target for GQD in UC intervention. Further experiments confirmed that GQD reduced pro-inflammatory cytokines (TNF-α, IL-6, IL-1β) and downregulated the Bax/Bcl-2 apoptosis pathway. Moreover, gut microbiota analysis showed that GQD enhanced the diversity and abundance of beneficial bacteria. GQD alleviates UC by modulating tryptophan, arginine, and proline metabolism, maintaining gut microbiota balance, and reducing apoptosis in intestinal cells.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"264 ","pages":"Article 116972"},"PeriodicalIF":3.1,"publicationDate":"2025-05-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144108266","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":"Investigation of the material basis and mechanism of Qingfei Paidu granules in treating LPS-induced acute pneumonia using UPLC-Q-TOF-MS/MS, network pharmacology, molecular docking and experimental verification","authors":"Yuqing Ma ,&nbsp;Hao Zhao ,&nbsp;Ruonan Ma ,&nbsp;Qiang Guo ,&nbsp;Huizhen Li ,&nbsp;Yuxin Zhang ,&nbsp;Xia Wu ,&nbsp;Xing Wang","doi":"10.1016/j.jpba.2025.116973","DOIUrl":"10.1016/j.jpba.2025.116973","url":null,"abstract":"<div><div>Qingfei Paidu granules (QFPDG), derived from four classic traditional Chinese medicine formulas with a centuries-long history of treating respiratory disorders, have shown remarkable clinical efficacy against pneumonia and lung injury, yet their pharmacodynamic components and mechanisms require further elucidation. In this work, UPLC-Q-TOF-MS/MS was used to identify the chemical constituents in QFPDG, drug-containing serum, and lung tissue. Network pharmacology was employed to predict key targets and pathways. The anti-pneumonia efficacy was evaluated via an LPS-induced acute pneumonia mouse model and by measuring cytokine levels in LPS-stimulated RAW264.7 cells. Finally, Molecular docking along with molecular dynamics simulation was conducted to explore the interactions between key compounds and targets. Results showed that 145 compounds were identified in QFPDG solution, 94 in serum, and 83 in lung tissue, with 97 components in serum and lung associated with 350 pneumonia-related targets and crucial pathways. QFPDG alleviated acute lung injury and inflammation in LPS-induced acute pneumonia mice, reducing monocyte, neutrophil, lymphocyte, and leukocyte counts in bronchoalveolar lavage fluid (BALF), as well as decreasing TNF-α and IL-1β levels. Molecular docking and molecular dynamics simulations showed that five key components in QFPDG had strong binding affinities for TNF-α, IL-1β, IL-6 and AKT1 with minimal fluctuations at equilibrium. Binding free energy calculations indicated that the ∆G_bind values ranging from −8.59 to −41.98 kcal/mol, primarily driven by hydrophobic and electrostatic interactions, involving key amino acid residues like Glu93, Tyr97, Tyr119, Gly121, and Tyr151. In summary, QFPDG presents a multi-component, multi-target approach to treating pneumonia, targeting key signaling pathways including PI3K-AKT, MAPK, and TNF. The compound-target interactions clarify its anti-inflammatory and tissue-protective mechanisms, suggesting potential for clinical application and pharmaceutical development.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"264 ","pages":"Article 116973"},"PeriodicalIF":3.1,"publicationDate":"2025-05-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144108267","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":"Addressing temperature variations of miniaturized NIR spectrometers: Advancing quantitative models for pharmaceutical analysis","authors":"Ahmed Ramadan,&nbsp;Nicolas Abatzoglou,&nbsp;Ryan Gosselin","doi":"10.1016/j.jpba.2025.116959","DOIUrl":"10.1016/j.jpba.2025.116959","url":null,"abstract":"<div><div>Miniaturized near-infrared (NIR) spectrometers have gained wide popularity in various pharmaceutical applications, particularly for inline processes. However, their quantification capabilities still lag behind those of mature benchtop spectrometers, with miniaturized NIR spectrometers often lacking the accuracy required for pharmaceutical analysis without calibration transfer to a robust benchtop device. Therefore, a comprehensive investigation of their inherent error sources is imperative to enhance their analytical performance. Factors such as compact size, lack of thermal management systems, and operational conditions render miniaturized devices more susceptible to temperature fluctuations. These fluctuations lead to measurement errors, especially when the duration of inline processes limits the frequency of updating background scans. While previous research investigated the impact of sample and ambient temperature variations, we investigated the impact of temperature variations of miniaturized NIR spectrometers itself during sample and background acquisitions. These variations led to emergence of distinct spectral subsets, posing a risk to accuracy when combined in one model and making prediction of one subset by another challenging. We explored calibration transfer (CT) methods to enhance model robustness and maintain prediction accuracy across temperature subsets, with Ridge and LASSO regressions showing superior results. By addressing this error source, it is possible to enhance the accuracy and robustness of miniaturized NIR spectrometers, particularly in prolonged inline measurements.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"264 ","pages":"Article 116959"},"PeriodicalIF":3.1,"publicationDate":"2025-05-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144108025","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}