Journal Of Pharmaceutical And Biomedical Analysis[JOURNAL]
Sun
200 papers
Spatio-temporal analysis deciphers the energy metabolism disorders in depression based on stable isotope-resolved metabolomics.
Linghu T, Gu X, Zhao Y … +3 more , Tian J, Qin X, Zhang R
J Pharm Biomed Anal · 2026 Jul · PMID 41747486 · Publisher ↗
The significant impact of depression on human life has attracted great attention. However, the unclear and highly complex pathogenesis of depression has resulted in the limited efficacy of currently available antidepress...
The significant impact of depression on human life has attracted great attention. However, the unclear and highly complex pathogenesis of depression has resulted in the limited efficacy of currently available antidepressants. Therefore, it is imperative to explore the pathogenesis of depression from novel perspectives and develop next-generation antidepressants that target innovative mechanisms. In this study, the stable isotope tracing technology and a pseudo-first-order kinetics mathematical model were employed to assess the metabolic rates and the isotope distribution across various tissues from a spatio-temporal perspective. Our findings revealed that chronic unpredictable mild stress (CUMS) rats exhibited impaired tricarboxylic acid (TCA) cycle activity and activated gluconeogenesis, whereas nephrotic syndrome (NS) rats demonstrated impaired TCA cycle activity and enhanced fatty acid β-oxidation. Furthermore, our results revealed an interesting phenomenon that caecum displayed the lowest abundances in all metabolic pathways, while serum, heart, brain, and kidney displayed the highest abundances in glycolysis/gluconeogenesis, TCA cycle, neurotransmitters metabolism, and fatty acids metabolism, respectively. The results comprehensively and accurately revealed the specific pathway of energy metabolism disorders in depression from a spatio-temporal perspective. Our study provided a novel insight for exploring the pathological mechanisms of depression, identifying new therapeutic targets, and developing ideal antidepressants.
Simultaneous quantification of fat- and water-soluble vitamins in serum by valve-mediated dual LC-MS/MS.
Li W, Luo K, Qian H … +4 more , Wu Y, Wu Y, Gao Y, Gu D
J Pharm Biomed Anal · 2026 Jul · PMID 41740324 · Publisher ↗
Liquid chromatography-tandem mass spectrometry (LC-MS/MS) is the benchmark platform for multiplex vitamin quantification, yet simultaneous determination of chemically disparate fat-soluble (FSVs) and water-soluble vitami...
Liquid chromatography-tandem mass spectrometry (LC-MS/MS) is the benchmark platform for multiplex vitamin quantification, yet simultaneous determination of chemically disparate fat-soluble (FSVs) and water-soluble vitamins (WSVs) remains analytically challenging. We introduce a pragmatic dual-stream workflow that converts the intrinsic waste segments of any LC gradient into productive analytical time, delivering complete FSV and WSV profiles. Two 5-min chromatographic separations, optimized for fat-soluble and water-soluble vitamins respectively, are staggered through a six-port divert valve: while one column eluted its analytes to the mass spectrometer, the other was shunted to waste. This seamless overlap effectively doubles the throughput within 5 min. And every WSV elution window remained fully enclosed within the waste segment of the FSV gradient, with CVs < 10 % for the internal-standard peak areas across both vitamin classes. Moreover, method comparison between dual LC-MS/MS and single LC-MS/MS across twenty patient sera yielded Spearman's rho values ranging from 0.950 to 0.997, Passing-Bablok slopes spanning 0.884-1.128, and Bland-Altman biases below 8.3 %, confirming clinical concordance. Owing to its simple equipment requirements and setup process, this method should be highly accessible for other laboratories.
Counterfeit thyroid medications: A comprehensive analysis of the composition of products seized by law enforcement using liquid chromatography coupled with mass spectrometry.
Kalicka A, Kierasińska A, Woźniak P … +2 more , Fijałek Z, Giebułtowicz J
J Pharm Biomed Anal · 2026 Jul · PMID 41740323 · Publisher ↗
Drug counterfeiting is a global public health challenge affecting both developed and developing countries. This study reports the first comprehensive quality assessment of falsified medicinal products containing thyroid...
Drug counterfeiting is a global public health challenge affecting both developed and developing countries. This study reports the first comprehensive quality assessment of falsified medicinal products containing thyroid hormones (liothyronine and levothyroxine) seized from two illegal manufacturing facilities in Poland, from which counterfeit products were distributed across Europe. Qualitative and quantitative analyses of the declared active ingredients, along with identification of pharmacologically active contaminants, were performed using high-performance liquid chromatography coupled with mass spectrometry. The results revealed poor product quality and a substantial potential health risk. Trace levels of undeclared substances-including anabolic agents, hormones and metabolic modulators, diuretics and masking agents, phosphodiesterase type 5 inhibitors, and drugs of abuse-provided forensic evidence linking counterfeit pharmaceutical production to organized drug trafficking, while not constituting a direct pharmacological threat. The primary risk arose from incorrect and highly non-uniform dosing of the declared active compounds, in some cases exceeding 600 % of the labeled dose, thereby critically compromising treatment safety and efficacy.
Digital multidimensional fingerprinting and monolinear method quantitation for quality consistency of traditional chinese medicine injection.
Zhou K, Ren Y, Zhang J … +1 more , Sun G
J Pharm Biomed Anal · 2026 Jul · PMID 41734438 · Publisher ↗
Traditional Chinese medicine (TCM) injections require stringent batch-to-batch quality control. This study established a digital, multidimensional fingerprinting workflow for Ixeris sonchifolia (Bunge) Hance injection (I...
Traditional Chinese medicine (TCM) injections require stringent batch-to-batch quality control. This study established a digital, multidimensional fingerprinting workflow for Ixeris sonchifolia (Bunge) Hance injection (ISHI), integrating: (i) five-wavelength HPLC fusion fingerprints, (ii) UV quantum fingerprints, (iii) equal-weight ratio quantitative fingerprinting with reliability theory, (iv) multi-component assay via a monolinear method, and (v) antioxidant activity profiling. Across 17 batches, the macro-qualitative similarity S from HPLC was ≥ 0.99, and the macro-quantitative similarity P fell within the accepted range of 89.6-106.0 %. UV quantum fingerprinting classified the batches into three quality tiers (P = 89.2-112.1 %). Data fusion (HPLC + UV) reduced result dispersion (RSD 4.07 %) compared to individual methods (HPLC 4.90 %, UV 5.99 %), demonstrating superior robustness. The monolinear multi-component method yielded contents closely matching those from the full calibration curve method and generally showed better agreement than the quantitative analysis of multi-components by a single marker method, enabling cost-efficient routine quantification. Reliability indices for single batches exceeded 0.98 for both macro-qualitative (SR) and macro-quantitative (PR) reliability, and the reference fingerprint exhibited near-ideal reliability. DPPH radical scavenging activity (IC50) correlated with specific fingerprint peaks, notably phenolic acids, linking chemical profiles to biological function. This integrated digital approach provides a practical and scalable strategy for enhancing quality consistency assessment of ISHI and related TCM injections.
Exploring potential mechanism of Chuanzhi Qingyu recipe for vulnerable atherosclerosis plaques based on UPLC-Q-TOF-MS, systems biology strategy, and experimental validation.
Weng J, Huan L, Zhang S … +3 more , Cao W, Xu F, Zhang Y
J Pharm Biomed Anal · 2026 Jul · PMID 41722459 · Publisher ↗
Chuanzhi Qingyu (CZQY) recipe is clinically used for the secondary prevention and treatment of cardiovascular diseases associated with atherosclerosis (AS) However, the potential active components and underlying molecula...
Chuanzhi Qingyu (CZQY) recipe is clinically used for the secondary prevention and treatment of cardiovascular diseases associated with atherosclerosis (AS) However, the potential active components and underlying molecular mechanisms require further elucidation. This study established a mouse model of vulnerable AS plaques through a high-fat diet. The efficacy of CZQY in stabilizing these vulnerable plaques was assessed using histological staining techniques. Additionally, biochemical analyses, ELISA assays, small animal ultrasound technology, and immunohistochemistry were employed. Subsequently, the active pharmaceutical ingredients of CZQY were identified through UPLC-Q-TOF-MSE. Finally, a network pharmacology approach, in conjunction with RNA-seq was utilized to predict the targets and mechanisms of CZQY in stabilizing vulnerable AS plaques, which were subsequently validated using Western blot and PCR methods. The research results show that CZQY can significantly improve lipid levels and liver function, reduce serum inflammation and oxidative stress levels, improve vascular function, and stabilize vulnerable AS plaques. The main components of CZQY that stabilize vulnerable AS plaques include flavonoids, terpenoids, and organic acids. The findings from RNA-seq and network pharmacology suggest that CZQY stabilizes vulnerable AS plaques potentially through mechanisms related to lipid metabolism, inflammatory responses, and cell migration, etc. Subsequent RT-qPCR and Western blot analyses confirmed that CZQY significantly modulated the expression of key targets at both mRNA and protein levels. In conclusions, CZQY effectively reduces risk factors associated with vulnerable AS plaques, improves vascular function, and stabilizes these plaques. This may be related to its ability to modulate mechanisms involving lipid metabolism, inflammation, extracellular matrix dynamics, and smooth muscle cell phenotype. These findings provide significant data support for further pharmacological research and clinical applications.
Analytical approaches for the determination of nitrate and nitrite in infant and baby foods: Advances and occurrence.
Kalaycıoğlu Z, Gölcü A
J Pharm Biomed Anal · 2026 Jul · PMID 41719788 · Publisher ↗
Infant and baby foods may contain nitrate and nitrite due to the accumulation of these ions in plant-based ingredients, and although nitrate itself is not acutely toxic, its potential conversion to nitrite and subsequent...
Infant and baby foods may contain nitrate and nitrite due to the accumulation of these ions in plant-based ingredients, and although nitrate itself is not acutely toxic, its potential conversion to nitrite and subsequent health risks necessitate accurate and reliable analytical determination. Therefore, determining nitrate and nitrite levels in commercially produced infant formulas is crucial for both infant health and regulatory compliance. Continuous monitoring and compliance with the relationship between these two factors are essential to prevent health risks to infants and maintain the overall quality of commercial infant products. This study compiles literature reports on analytical methods, method evaluations, sample preparation, and nitrate and nitrite concentrations of various commercial baby and toddler foods produced worldwide between 1975 and 2025, highlighting analytical approaches and sample preparation strategies for determining nitrate and nitrite in baby foods. The presence of nitrate and nitrite in baby and toddler foods, as well as relevant legal regulations, is also reviewed.
Integrating non-targeted metabolomics and machine learning for comprehensive phytochemical profiling and intelligent discrimination of Acorus tatarinowii and its adulterants.
Wang JW, Liu XK, Huang F … +6 more , Xu YB, Huang JH, Gan WJ, Li ZW, Zhang DD, Guo DA
J Pharm Biomed Anal · 2026 Jul · PMID 41719787 · Publisher ↗
The dried rhizome of Acorus tatarinowii Schott (SCP) is a valued medicinal material in traditional Chinese medicine (TCM). However, its quality and efficacy are often compromised by adulteration with morphologically and...
The dried rhizome of Acorus tatarinowii Schott (SCP) is a valued medicinal material in traditional Chinese medicine (TCM). However, its quality and efficacy are often compromised by adulteration with morphologically and chemically similar species, including Acorus calamus L. (ZCP), Acorus calamus f. submersa Glück (WCP), and Anemone altaica Fisch. (JJCP). To address this issue, we developed a robust authentication strategy by integrating ultra performance liquid chromatography quadrupole time of flight-tandem mass spectrometry (UPLC-Q-TOF-MS/MS)-based non-targeted metabolomics with machine learning (ML). Through comparison with authentic standards and high-confidence database matching, a comprehensive phytochemical profiling identified a total of 181 compounds across all studied species, with 141 characteristic compounds detected in SCP. Orthogonal partial least squares discriminant analysis (OPLS-DA) identified 40 key differential metabolites as potential biomarkers for species discrimination. Subsequently, six ML classification models were systematically constructed and evaluated. The support vector machine (SVM) model demonstrated optimal performance, achieving 100 % accuracy on both training and test sets in the internal validation, along with significantly improved computational efficiency compared to traditional chromatographic methods. Collectively, the integrated "UPLC-Q-TOF-MS/MS metabolomics-ML" workflow was successfully validated for authenticating SCP and its adulterants. This strategy proves to be both efficient and reliable, providing not only novel data support for SCP quality control but also offering a promising and transferable technical pathway for the accurate discrimination of closely related medicinal materials.
Insights into the mechanism of treatment of ulcerative colitis with pre- and post-processed dried ginger through perspective of metabolomics and intestinal microbiomics research.
Han S, Yang X, Du J … +6 more , Hou Z, Wei W, Huo J, Cui X, Yao T, Xu H
J Pharm Biomed Anal · 2026 Jul · PMID 41719786 · Publisher ↗
Numerous experiments and clinical practices have demonstrated the distinct therapeutic effect of dried ginger (DG) and processed ginger (PG) in the treatment of ulcerative colitis (UC), while, the differences in efficacy...
Numerous experiments and clinical practices have demonstrated the distinct therapeutic effect of dried ginger (DG) and processed ginger (PG) in the treatment of ulcerative colitis (UC), while, the differences in efficacy and mechanisms are not yet fully understood. By integrating metabolomics and gut microbiome analyses, combined with liquid chromatography-mass spectrometry technology for serum metabolism detection, 16S rRNA gene microbiota sequencing and Spearman correlation analysis, the pharmacological effects and mechanisms of action of the two were explored. Pharmacodynamic results demonstrated that both DG and PG have significant therapeutic effects on UC mice, and PG has a better effect in shortening the coagulation time and promoting hemostasis. Metabolomics analysis revealed that DG has 94 differential metabolites, mainly affecting the metabolism of arachidonic acid, whereas PG has 88 differential metabolites, focusing on pathways such as steroid biosynthesis. Intestinal microbiomics analysis indicates that DG and PG can regulate the richness and diversity of the microbiota. DG significantly regulated 3 bacterial families and 8 bacterial genera, while PG regulated 4 families and 11 genera. Spearman correlation analysis further confirmed that PG reshapes the "gut microbiota-host metabolism" interaction network. This study combined multi-omics techniques to analyze the microbiota-metabolism regulatory characteristics of DG and PG in the treatment of UC, and clarified how the component changes caused by ginger processing led to the differentiation of the two in terms of therapeutic focus and the microbiota-metabolism regulatory network. These findings provide scientific evidence supporting the precise application of ginger-derived medicinal materials in the treatment of UC.
Simultaneous quantification of chondroitin sulfate and dermatan sulfate in crude heparins using H NMR and independent component analysis.
Burger R, Do XT, Diehl BWK … +2 more , Schulze M, Monakhova YB
J Pharm Biomed Anal · 2026 Jul · PMID 41719785 · Publisher ↗
Heparin, an essential anticoagulant in clinical practice, is susceptible to contamination with chondroitin sulfate (CS) and dermatan sulfate (DS). Ensuring the reliable quantification of these polysaccharides in crude he...
Heparin, an essential anticoagulant in clinical practice, is susceptible to contamination with chondroitin sulfate (CS) and dermatan sulfate (DS). Ensuring the reliable quantification of these polysaccharides in crude heparins is critical for product safety and for monitoring the purification process, yet remains challenging due to their structural similarity and heterogeneous composition. ¹H NMR and Independent Component Analysis (ICA) were used to resolve the overlapping acetyl signals of CS and DS. Samples of crude heparin and synthetic mixtures were measured on a 500 MHz high-field NMR and an 80 MHz benchtop instrument. The ICA yielded models with root mean square errors (RMSEs) ≤ 1.7 % w/w (500 MHz) and ≤ 2.1 % w/w (80 MHz) for the synthetic mixtures (concentration range of 3-19 % w/w for CS and 3-40 % w/w for DS). The accuracy of the ICA method was confirmed by the conventional enzymatic digestion method for crude heparin samples. While the 500 MHz model completely conformed with the results of the enzymatic method, the 80 MHz benchtop system is best suited for screening applications where impurity levels are from moderate to high. The ICA-NMR workflow surpasses the traditional enzymatic assay in speed and simplicity, and opens the way towards the development of an automated and validated on‑site heparin quality control method.
Development and validation of a robust UPLC-MS/MS method for the analysis of polyamines in cells, biofluids and tissues.
Iannone M, Vereyken L, Grajchen E … +7 more , Deneubourg C, Gorremans S, Donck LV, Bretteville A, Moechars D, Jahouh F, Vreeken RJ
J Pharm Biomed Anal · 2026 Jul · PMID 41713120 · Publisher ↗
Loss of function (LoF) of the ATP13A2 protein, a polyamines transporter, has been linked to lysosomal and mitochondrial dysfunctions that play an important role in the early onset of Parkinson's disease (PD) and related...
Loss of function (LoF) of the ATP13A2 protein, a polyamines transporter, has been linked to lysosomal and mitochondrial dysfunctions that play an important role in the early onset of Parkinson's disease (PD) and related neurodegenerative disorders. To investigate the downstream consequences of these LoFs in relevant in-vitro and in-vivo models, we describe the development, optimization, validation and application of an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the quantification of a range of endogenous polyamines (putrescine, cadaverine, ornithine, spermidine, spermine, N1 acetylputrescine, N1 acetylcadaverine, N1 acetylspermidine, N1N8 diacetylspermidine and N1 acetylspermine) in cells, biofluids and brain tissues. Sample pre-treatment consists of protein precipitation, derivatization with benzoyl chloride (BZ) and liquid-liquid extraction clean-up with ethyl acetate. The chromatographic separation is achieved on an ACQUITY BEH C18 column within 5.5 min using an acetonitrile/water + 0.1 % formic acid gradient, while the mass spectrometric analysis is performed using a triple quadrupole operating in selected reaction monitoring (SRM) mode. The analytical method is validated in terms of linear dynamic range, lower and upper limit of quantification (LLOQ and ULOQ), accuracy, precision, matrix effect, carry-over and stability. LLOQ values are between 0.05 and 0.5 ng/mL while the ULOQ values are between 1*10 and 5*10 ng/mL, depending on the analyte and on the matrix. For certain compounds, the linear dynamic range extension, up to four orders of magnitude, is achieved using isotopologue transitions. Accuracy is between 97.5 % and 108.2 % while intra-day and inter-day precision, expressed as cv% of the control samples at three different concentration levels, are below 15 %. No carry-over and matrix effect are observed. The analysis of cell lysates, different biofluids (mouse plasma and mouse cerebrospinal fluid) and mouse brain tissue homogenates confirm the applicability of the developed method for the quantification of the polyamines included in the method.
An integrative strategy combining network pharmacology, metabolomics, and gut microbiota analyses to elucidate the bioactive ingredients and underlying mechanisms of Xin-Shu-Ning tablets against myocardial ischemia.
Gu Y, Huang H, Liu Y … +7 more , Liu X, Su W, Chen Y, Qian C, Zhu Q, Li J, Rong W
J Pharm Biomed Anal · 2026 Jul · PMID 41713119 · Publisher ↗
Xin-Shu-Ning tablets (XSNT) are clinically used for the treatment of angina pectoris and coronary insufficiency; however, their bioactive constituents and cardioprotective mechanisms remain insufficiently clarified. In t...
Xin-Shu-Ning tablets (XSNT) are clinically used for the treatment of angina pectoris and coronary insufficiency; however, their bioactive constituents and cardioprotective mechanisms remain insufficiently clarified. In this study, an integrated strategy combining network pharmacology, metabolomics, and 16S rDNA amplicon sequencing was employed to systematically elucidate the mechanisms of XSNT and identify its potential active components. The blood-absorbed constituents of XSNT were first characterized using an HPLC-MS/MS method. Network pharmacology analysis was then conducted to predict potential therapeutic targets and pathways, which were further validated by serum metabolomics and Western blot analysis. In parallel, fecal metabolomics was applied to evaluate metabolic alterations following XSNT administration. Differential metabolites were analyzed using the MetOrigin platform to predict associated gut microbiota and metabolic pathways, and these predictions were further validated by 16S rDNA sequencing. A total of 76 compounds were identified in XSNT, including 40 blood-absorbed constituents. Integrated network pharmacology and serum metabolomics analyses indicated that XSNT exerts cardioprotective effects mainly through modulation of the tyrosine metabolism pathway, with tyrosine hydroxylase and catechol-O-methyltransferase identified as potential key cardiac targets. Additionally, XSNT significantly regulated gut microbiota composition and amino acid metabolism, including arginine, phenylalanine, and lysine pathways. Notably, phenylalanine, as a precursor of tyrosine, may function as a metabolic bridge linking gut microbial regulation to cardiac tyrosine metabolism. Overall, XSNT exerts cardioprotective effects through coordinated direct cardiac actions and systemic regulation mediated by the heart-gut axis, providing a systems-level understanding of its multi-component and multi-target therapeutic mechanisms.
Bridging the gap: A systematic approach to integrating serum and plasma proteomic datasets for biomarker studies.
Lahav C, Dahan N, Harel M … +12 more , Elon Y, Sela I, Geyer PE, Schneider MA, Muley T, Bacchiocchi A, Marte J, Floudas CS, Halaban R, Sznol M, Christopoulos P, Gulley JL
J Pharm Biomed Anal · 2026 Jul · PMID 41713118 · Full text
Serum and plasma are widely used in proteomic biomarker discovery, but differences between their proteomes have hindered the integration of data from the two specimen types. Here, we describe a computational approach for...
Serum and plasma are widely used in proteomic biomarker discovery, but differences between their proteomes have hindered the integration of data from the two specimen types. Here, we describe a computational approach for bridging between serum and plasma proteomic measurements derived from the aptamer-based SomaScan assay. We aimed to enable cross-specimen data utilization in the context of the PROphet model designed to predict immunotherapy outcomes based on 388 plasma proteomic biomarkers. Proteomic profiling of 7289 proteins was performed on 177 matched serum-plasma sample pairs from cancer patients across three distinct cohorts. Remarkably, 91.6% of the proteins showed correlation (p-value < 0.05) between serum and plasma protein levels, highlighting the feasibility of serum-plasma bridging. Linear scaling factors derived from matched serum-plasma sample pairs were consistent across the three cohorts, suggesting that the scaling factors are generalizable. Notably, the PROphet model maintained its predictive power when applied to scaled serum proteomic measurements. Specifically, clinical benefit predictions and survival stratification based on scaled serum proteomic measurements were similar to those based on plasma proteomic measurements. Our study demonstrates the feasibility of generalizing plasma-based predictors to serum samples through appropriate bridging strategies, paving the way for integrating serum and plasma datasets.
Physicochemical and biological characterization of GNR-087, a Tocilizumab biosimilar.
Gusarova VD, Lyagoskin IV, Degterev MB … +3 more , Rodionov AV, Evdokimova OL, Shukurov RR
J Pharm Biomed Anal · 2026 Jun · PMID 41707327 · Publisher ↗
GNR-087 developed by IBC Generium, Russia is a biosimilar candidate to Tocilizumab reference product. A comprehensive analytical assessment of the structural and functional similarity of GNR-087 and Tocilizumab reference...
GNR-087 developed by IBC Generium, Russia is a biosimilar candidate to Tocilizumab reference product. A comprehensive analytical assessment of the structural and functional similarity of GNR-087 and Tocilizumab reference product is one of the steps of the stepwise approach and was performed using a sensitive state-of-the-art analytical techniques. Appropriate product quality attributes were taken into account, including those known to affect the mechanisms of action, efficacy and safety. GNR-087 was demonstrated to have the same amino acid sequence and high-order structure, similar N-glycosylation pattern and post-translational modification profile, and biological activities as Tocilizumab reference product. The minor differences in attributes (in particular, the content of individual types of glycans) were considered clinically insignificant, which was confirmed by biological and functional tests. The results of the comparative similarity assessment demonstrate high analytical comparability of GNR-087 and Tocilizumab reference product. GNR-087 (Complarate® drug product) was licensed in the Russian Federation in 2024 for the treatment of rheumatoid arthritis.
In vitro metabolic profiling of weight-loss-inducing amylin receptor agonists in the context of preventive doping research.
Alhalabi H, Borschel L, Le Foll C … +3 more , Thomas A, Bally L, Thevis M
J Pharm Biomed Anal · 2026 Jun · PMID 41702251 · Publisher ↗
Peptide hormone-based weight-loss therapeutics have gained increasing attention, driven amongst other reasons, by the clinical and commercial success of semaglutide. Their increasing accessibility raises concerns about t...
Peptide hormone-based weight-loss therapeutics have gained increasing attention, driven amongst other reasons, by the clinical and commercial success of semaglutide. Their increasing accessibility raises concerns about their potential misuse in sports, especially in disciplines where weight management is decisive for athletic performance. Semaglutide has been included in the World Anti-Doping Agency's monitoring program since 2024. Given that amylin signalling is a key therapeutic target for next-generation weight-loss drugs, amylin receptor agonists such as pramlintide, cagrilintide and KBP-066 also warrant consideration as to metabolism and detection strategies in sports drug testing programs. This study aimed to characterize the metabolic profiles of pramlintide, cagrilintide and KBP-066, identify analytically suitable metabolites and develop and validate a LC-MS/MS-based detection approach. Comprehensive in vitro models, including human skin S9 fraction, kidney S9 fraction and biological fluids, were used to investigate metabolic pathways. HRMS/MS was employed to characterize metabolites and evaluate their suitability as analytical targets. For comparison, authentic post-administration rat samples were analysed for cagrilintide and respective biotransformation products. All three peptides underwent N-terminal and C-terminal degradation, yielding multiple stable metabolic products suitable as detection targets. Cagrilintide metabolites predicted from in vitro experiments were observed in authentic post administration rat plasma samples, confirming in vivo relevance. Finally, suitable preparation and detection methods were established and validated. This study provides the first systematic metabolic characterization of pramlintide, cagrilintide and KBP-066. The identified metabolites and LC-MS/MS detection approach offer a foundation for future monitoring of emerging weight-loss peptide hormone analogues in anti-doping contexts.
Integrating plasma metabolomics using UPLC-Q Exactive Orbitrap HRMS and targeted amino acid and neurotransmitter analysis in plasma and cerebrospinal fluid by LC-MS/MS to explore biomarkers in pregnancy women with insomnia.
Han Y, Chen J, Chen G … +4 more , Shan L, Qiu Y, Wang F, Wang W
J Pharm Biomed Anal · 2026 Jun · PMID 41702250 · Publisher ↗
Insomnia is a common sleep issue among pregnant women. This study aimed to explore the metabolic characteristics of pregnant women with insomnia and identify potential biomarkers through plasma and cerebrospinal fluid (C...
Insomnia is a common sleep issue among pregnant women. This study aimed to explore the metabolic characteristics of pregnant women with insomnia and identify potential biomarkers through plasma and cerebrospinal fluid (CSF) metabolomics analysis. A total of 423 pregnant women participated in the plasma sample collection, and 89 provided CSF samples during delivery. Plasma metabolomics analysis was conducted using UPLC-Q Exactive Orbitrap high-resolution mass spectrometry. Furtherly, targeted amino acid and neurotransmitter analysis in plasma and CSF using validated LC-MS/MS methods. Multivariate statistical methods were employed for data analysis. The results indicated that the incidences of insomnia were 6.74 %, 14.0 %, and 50.0 % in the first, second, and third trimesters, respectively. Plasma metabolomics analysis revealed significant alterations in amino acid metabolism pathways in pregnant women with insomnia. In the following targeted amino acid analysis, alanine demonstrated the highest diagnostic value (AUC: 0.914) in the first trimester, remaining significant in the third trimester. CSF analysis showed elevated glutamine, histidine, methionine, 5-hydroxyindole acetic acid, and dopamine in pregnant women with insomnia. In conclusion, pregnant women with late-pregnancy insomnia exhibited specific amino acid metabolism disorders during the first trimester, indicating potential value of early intervention in preventing pregnancy insomnia. Disrupted amino acid and neurotransmitter metabolism may be key features of pregnancy-related insomnia.
3-mercaptopropionic acid agent-based biosensor system using gold-screen printed electrode for aflatoxin B1 detection.
Demi̇rbakan B, Çeti̇nkaya A, Altuntaş EG … +3 more , Ünal MA, Sezgi̇ntürk MK, Özkan SA
J Pharm Biomed Anal · 2026 Jun · PMID 41687227 · Publisher ↗
A novel electrochemical biosensor was constructed for the ultrasensitive detection of aflatoxin B1 (AFB1) in food samples. The biosensor design was based on a 3-mercaptopropionic acid (3-MPA)-modified self-assembled mono...
A novel electrochemical biosensor was constructed for the ultrasensitive detection of aflatoxin B1 (AFB1) in food samples. The biosensor design was based on a 3-mercaptopropionic acid (3-MPA)-modified self-assembled monolayer (SAM) constructed on disposable gold screen-printed electrodes (SPE-Au). Covalent attachment of anti-AFB1 antibodies was achieved on the functionalized electrode surface, and the modification process at each stage was analyzed using CV and EIS techniques. 3-MPA concentration was optimized to enhance analytical performance. The biosensor exhibited a wide linear detection range of 0.1-250 pg/mL with a calculated limit of detection (LOD) of 0.94 pg/mL and limit of quantification (LOQ) of 3.14 pg/mL. It also demonstrated high reproducibility and excellent selectivity toward AFB1. Finally, the biosensor was successfully applied to real food samples, including milk, rice, peanuts, and chili pepper, confirming its reliability and potential for practical food safety monitoring.
Corrigendum to "Integrative analysis of transcriptome and metabolome provide new insights into mechanisms of capilliposide A against cisplatin-induced nephrotoxicity" [J. Pharm. Biomed. Anal. 238 (2024), 115814].
Fang J, Wang L, Zhang D … +6 more , Liang Y, Li S, Tian J, He Q, Jin J, Zhu W
J Pharm Biomed Anal · 2026 Jun · PMID 41687226 · Publisher ↗
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Metabolomics technology combined with O2PLS analysis reveals the active components of Paeoniae Radix Alba in preventing renal damage in rheumatoid arthritis.
Lv S, Lin J, Sun Y … +4 more , Kang M, Li X, Song L, Li Y
J Pharm Biomed Anal · 2026 Jun · PMID 41687225 · Publisher ↗
Rheumatoid arthritis (RA) is a chronic autoimmune disorder characterized by symmetrical, erosive polyarthritis and multi-organ involvement, with renal complications posing a life-threatening risk. Paeoniae Radix Alba, kn...
Rheumatoid arthritis (RA) is a chronic autoimmune disorder characterized by symmetrical, erosive polyarthritis and multi-organ involvement, with renal complications posing a life-threatening risk. Paeoniae Radix Alba, known as BaiShao (BS) in Chinese, is a widely used herbal medicine for clinical RA treatment, yet its potential in preventing RA-associated renal damage and its underlying active ingredients remain elusive. To address this knowledge gap, we employed a type II collagen-induced arthritis (CIA) rat model. Biochemical assays and histopathological analyses confirmed that BS exerted robust renoprotective effects in CIA rats. Serum and urine metabolomics identified 48 renal damage-related biomarkers, 18 of which showed distinct regulatory trends following BS intervention. Meanwhile, ultra-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF/MS) was used to characterize 34 chemical components in BS. Through an integrative approach that combines two-way orthogonal partial least squares (O2PLS) and Pearson correlation analysis, 18 active ingredients were identified as key mediators of BS-mediated renoprotection. Collectively, this study establishes a novel metabolomics-O2PLS strategy for discovering active ingredients in BS, laying a foundation for understanding the mechanism underlying the prevention of RA-associated renal damage mediated by BS and providing insights for the development of novel preventive therapeutics.
A novel thin layer chromatography based method for the quantification of quillaic acid saponins.
Bülow FE, Matkowski A, Weng A
J Pharm Biomed Anal · 2026 Jun · PMID 41687224 · Publisher ↗
Saponins display medicinal properties such as enhancing the drug delivery of biologicals, and boosting immune responses within vaccinations. As plant derived molecules, their phytochemical analysis is key to ensure pharm...
Saponins display medicinal properties such as enhancing the drug delivery of biologicals, and boosting immune responses within vaccinations. As plant derived molecules, their phytochemical analysis is key to ensure pharmaceutical quality. The quantification of saponins is typically carried out by high-performance liquid chromatography (HPLC). The aim of this study was the development of a simple thin-layer chromatography (TLC) based method for the quantification of the sapogenin quillaic acid (QA), the triterpenoid backbone of saponins such as QS21 that are used as immunological adjuvants. Following acidic hydrolysis of the saponins, the corresponding sapogenins were derivatized with 4-hydrazino-7-nitro-2,1,3-benzoxadiazole hydrazine (NBD-H) to form fluorescent hydrazones, increasing both the sensitivity and selectivity of the method. The detection of sapogenins with NBD-H is reported here for the first time. The QA-containing TLC bands were identified by mass spectrometry and their quantification was subsequently performed by densitometry. After validation, the method was applied to two plant species from Caryophyllaceae. To verify the plant's QA contents determined by TLC, a complementary HPLC method was developed. This study presents a new cost-effective method to quantify QA, enabling laboratories with limited resources to monitor plant cultivation and perform phytopharmaceutical quality control.
Serum metabolomics reveal metabolic changes in coal workers' pneumoconiosis progression.
Xu J, Wang M, Hou Z … +6 more , Kong J, Zhang M, Tian Y, Liu J, Yang J, Dai H
J Pharm Biomed Anal · 2026 Jun · PMID 41687223 · Publisher ↗
Chronic inhalation of coal dust causes coal workers' pneumoconiosis (CWP), which is one of the leading occupational diseases. Coal workers' pneumoconiosis is currently incurable, posing a serious public health threat. Id...
Chronic inhalation of coal dust causes coal workers' pneumoconiosis (CWP), which is one of the leading occupational diseases. Coal workers' pneumoconiosis is currently incurable, posing a serious public health threat. Identifying the underlying molecular mechanisms of CWP is critical to overcome this challenge. Nowadays, metabolomics has bridged underlying molecular alterations with disease progression, providing a useful tool for researching the pathogenesis and finding biomarkers. In this study, a comprehensive view of metabolic characterization of serum from CWP patients at all stages was provided using untargeted metabolomic analysis. As a result, when compared to healthy controls, the specific alteration patterns of each stage were observed. The results showed arginine and cortisol could be core metabolites in CWP progression. Moreover, five metabolites that significantly changed when going from "solely chronic coal-dust exposure" to an early stage were screened out as potential biomarkers. The receiver operating characteristic results were 0.691-0.862 (individual) and 0.884-0.907 (combined). These findings will benefit the application of metabolomics to understand the pathological mechanism and identify diagnostic biomarkers for CWP.
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