Journal Of Pharmaceutical And Biomedical Analysis[JOURNAL]
Sun
200 papers
Identification of chemical components in Thalictrum glandulosissimum using UPLC-Q-TOF-MS/MS and pharmacokinetic analysis of multiple alkaloids in normal and ulcerative colitis rats.
Zhang H, Li W, Li Z … +5 more , Cao Z, Zhao X, Hou M, Zhu M, Song Y
J Pharm Biomed Anal · 2026 Jun · PMID 42330697 · Publisher ↗
Thalictrum glandulosissimum (TG) is traditionally used for treating ulcerative colitis (UC). Given the continuously increasing global incidence of UC and the limitations of current therapeutic options, there is an urgent...
Thalictrum glandulosissimum (TG) is traditionally used for treating ulcerative colitis (UC). Given the continuously increasing global incidence of UC and the limitations of current therapeutic options, there is an urgent need for safer treatments. However, most existing studies have focused on single component. Studies on the multi-component profile of TG's active alkaloids, particularly systematic pharmacokinetic investigations under pathological conditions, remain insufficient. Without a systematic understanding of which components are absorbed into the bloodstream and how their disposition is altered under UC pathology, the clinical translation of TG is significantly hindered. This research first established a UPLC-Q-TOF-MS/MS method to characterize TG's chemical composition, identifying 58 constituents including 16 prototypes. Integrating network pharmacology and in vitro assays, we predicted berberine, coptisine, cryptopine, and berlambine as core components, with STAT3, EGFR, and SRC as key targets. Molecular docking, qRT-PCR, and Western blot were used for validation. Furthermore, a rapid UPLC-MS/MS method was developed and validated to quantify five major bioactive alkaloids in rat plasma. Pharmacokinetic comparisons between normal and UC model rats revealed that UC significantly shortened T (0.5-1.0 h) and increased the C of berberine, coptisine, and columbamine by 1.19- to 1.67-fold (p < 0.05), suggesting enhanced intestinal absorption under inflammation. This study completes a "prediction-verification-application" workflow, laying a solid foundation for further pharmacokinetic-pharmacodynamic investigations into the therapeutic effects of TG in UC.
α-Glucosidase immobilization on cellulose filter paper coated with a blend of chitosan and polyvinyl alcohol for inhibitor screening from traditional Chinese medicines.
Shi XY, Zhang MT, Ma X … +1 more , Chen J
J Pharm Biomed Anal · 2026 Jun · PMID 42323927 · Publisher ↗
In this work, α-glucosidase was successfully immobilized on commercially available cellulose filter paper and applied to screen inhibitors from traditional Chinese medicines combined with capillary electrophoresis analys...
In this work, α-glucosidase was successfully immobilized on commercially available cellulose filter paper and applied to screen inhibitors from traditional Chinese medicines combined with capillary electrophoresis analysis. For the immobilization of α-glucosidase, cellulose filter paper was employed as the carrier. Which was first coated with a chitosan-polyvinyl alcohol blend solution and subsequently activated with polyethyleneimine to introduce a positively charged surface. Finally, α-glucosidase was immobilized onto the modified cellulose filter paper via electrostatic adsorption. The carrier was characterized, and several parameters affecting the catalytic activity of immobilized enzymes were optimized. The results showed that the tensile strength of chitosan-polyvinyl alcohol-modified cellulose filter paper was 1.8 times that of the original cellulose filter paper, indicating that the mechanical properties of the carrier were enhanced. Moreover, the immobilized α-glucosidase showed good storage stability (retained 51.7 ± 0.43% of its initial activity after storing at 4℃ for 30 days), excellent reusability (retained 79.5 ± 1.18% of its initial activity after reusing 10 times), improved environmental tolerance (70°C and pH 8.0). In addition, the reliability of the immobilized enzyme for enzyme inhibitor screening was verified using acarbose as a model inhibitor, and its half-maximal inhibitory concentration was 0.85 ± 0.02 μM. Eventually, the immobilized α-glucosidase was used to screen inhibitors from 12 traditional Chinese medicine extracts combined with capillary electrophoresis analysis, and Sanguisorbae Radix exhibited the strongest inhibitory effect. This established platform provides a rapid and reliable strategy for screening α-glucosidase inhibitors from traditional Chinese medicine.
Development of new liquid chromatography-tandem mass spectrometry methods for the quantification of seven metabolites in three related breast cancer cell lines.
Ghanbarian M, Michel D, Alyari M … +3 more , Khajavinia A, Dmitriev OY, El-Aneed A
J Pharm Biomed Anal · 2026 Jun · PMID 42320281 · Publisher ↗
Metabolites of the tricarboxylic acid (TCA) cycle play crucial roles in cancer biology, and their accurate quantification is essential for understanding energy metabolism, signaling dynamics, and identifying metabolic vu...
Metabolites of the tricarboxylic acid (TCA) cycle play crucial roles in cancer biology, and their accurate quantification is essential for understanding energy metabolism, signaling dynamics, and identifying metabolic vulnerabilities in cancer cells. However, traditional liquid chromatograph-tandem mass spectrometry (LC-MS/MS) methods for these polar metabolites often encounter challenges, such as limited retention on reversed-phase columns and ion suppression. This study developed and validated two LC-MS/MS methods for the accurate quantification of seven key TCA cycle metabolites in MDA-MB-231, M67-2 (MEMO1 knockdown), and M67-9 (MEMO1 knockout) breast cancer cell lines. For five metabolites, namely citrate (CA), L-malate (MA), fumarate (FA), α-ketoglutarate (AKG), and glutamate (GA), an isotope-coded derivatization approach utilizing C/C-labeled dimethylaminophenacyl (DmPA) bromide was employed to develop a targeted high-performance liquid chromatography (HPLC)-MS/MS method. Inefficient DmPA derivatization in aqueous matrices was addressed by optimizing sample preparation in non-aqueous conditions, and the presence of multiple peaks of AKG was resolved by selecting triethanolamine (TEOA) as the reaction base to improve specificity. Conversely, due to persistent interferences with DmPA derivatization, pyruvic acid (PA) and succinic acid (SA) were quantified using another novel hydrophilic interaction liquid chromatography (HILIC)-MS/MS method in their native underivatized forms. Both methods were validated according to regulatory bodies, ensuring linearity, accuracy, precision, selectivity, and stability. The methods ensured the utilization of two multiple reaction monitoring (MRM) transitions to enhance specificity. The validation approach was adjusted to fit tissue culture studies. The validated methods were successfully used to measure the TCA metabolites in tested cell lines, providing valuable tools for investigating metabolic dynamics in cancer research.
Multi-omics analysis reveals mitochondrial dysfunction-driven oxidative stress pathways in Caenorhabditis elegans exposed to 2,2-bis(chloromethyl) trimethylene bis[bis(2-chloroethyl) phosphate] (V6).
Ahn J, Tien NTN, Thu NQ … +5 more , Lee SK, Kim DH, Park SM, Long NP, Kim HM
J Pharm Biomed Anal · 2026 Jun · PMID 42314374 · Publisher ↗
The widespread application of organophosphate flame retardants (OPFRs) in everyday products has resulted in significant environmental contamination. Among these products, Antiblaze V6 has been extensively utilized in pla...
The widespread application of organophosphate flame retardants (OPFRs) in everyday products has resulted in significant environmental contamination. Among these products, Antiblaze V6 has been extensively utilized in plastic manufacturing because of its low toxicity. However, the molecular mechanisms of its toxic effects remain unclear. In this study, we conducted metabolomics and transcriptomics analyses to identify convergent and divergent key events associated with the potential toxicity of V6, with the aim of uncovering common patterns of these V6-related processes. We exposed Caenorhabditis elegans (C. elegans) to V6 and performed transcriptomics and metabolomics analyses. Preliminary experiments confirmed increased oxidative stress and mitochondrial dysfunction in C. elegans exposed to V6, indicating that mitochondrial impairment is a key feature of V6-induced toxicity. Overall, 62 metabolites were altered in C. elegans that were exposed to V6. The pathways associated with oxidative stress and mitochondrial dysfunction were conserved in C. elegans. Additionally, transcriptome analysis revealed that 2392 differentially expressed genes were primarily affected by V6 exposure; the major altered pathways were the TCA cycle, oxidative phosphorylation, and mitochondrial inner membrane pathways. Integrated transcriptomics and metabolomics enrichment analyses further confirmed the findings of the investigation of individual omics modalities. Collectively, our findings provide significant insights into the development of adverse outcome pathways in species that are exposed to V6 and the regulation of the potential toxicity of V6.
A rapid, sensitive, and straightforward bacterial capture tool -boronic acid-functionalized FeO nanoparticle- for antimicrobial susceptibility testing.
Gu XL, Chen R, Chen JW … +8 more , Huang YF, Liu QF, Huang XZ, Li SB, Man XP, Li YJ, Liu J, Li L
J Pharm Biomed Anal · 2026 Jun · PMID 42302553 · Publisher ↗
Pathogenic multi-resistant bacterial infections represent a significant and persistent threat to public health. The development of a rapid, accurate, and convenient method for antimicrobial susceptibility testing (AST) i...
Pathogenic multi-resistant bacterial infections represent a significant and persistent threat to public health. The development of a rapid, accurate, and convenient method for antimicrobial susceptibility testing (AST) is crucial for the timely diagnosis of pathogenic bacteria in clinical settings and is essential for the rational use of antibiotics. However, the low abundance of pathogenic multi-resistant bacteria in patient samples typically necessitates a waiting period of 24 h to 3 days to obtain positive samples for AST. To address this challenge, a novel, rapid, and straightforward bacterial capture tool- phenylboronic acid-functionalized FeO nanoparticles (B-FeONPs)-has been developed to enrich pathogenic bacteria without compromising their viability. Relying on the selective binding affinity to cis-diol groups on bacterial surfaces in alkaline aqueous solutions, B-FeONPs can effectively capture low concentrations of pathogenic bacteria from urine within 30 min, without affecting their activity. The magnetic properties of B-FeONPs facilitate the enrichment of captured bacteria into a small volume solution, thereby providing high-concentration positive samples for subsequent analysis. The enriched complex "bacteria-B-FeO" effectively facilitated the performance of AST, with results obtained within 12 h- an interval generally deemed adequate for providing clinicians with guidance on medication. In comparison to the conventional clinical AST method, the B-FeONPs demonstrated a 93.75% accuracy and 74.23% reduction in processing time, indicating their potential for rapid and effective bacterial enrichment and seamless integration into an automated AST instrument. These findings support that B-FeONPs possess significant potential as a powerful tool for the early diagnosis of pathogenic multi-resistant bacteria in clinical settings.
UPLC-ESI-QToF-MS/MS profiling and anxiolytic-like effects of Simira paraensis (Baill.) Steyerm bark.
Martins LRJ, Paracampo NENP, Ribeiro PRV … +8 more , Filho FO, Alves AMB, Dos Santos HS, de Menezes JESA, Marinho MM, da Rocha MN, Marinho ES, Canuto KM
J Pharm Biomed Anal · 2026 Jun · PMID 42302552 · Publisher ↗
Simira paraensis (Baill.) Steyerm (Rubiaceae), popularly known as araribá-rosa, is a small tree found mainly in the Amazon. Studies on the genus Simira report a chemical composition rich in indole alkaloids of the β-carb...
Simira paraensis (Baill.) Steyerm (Rubiaceae), popularly known as araribá-rosa, is a small tree found mainly in the Amazon. Studies on the genus Simira report a chemical composition rich in indole alkaloids of the β-carboline class, which are associated with effects on the central nervous system. The present study aimed to characterize the chemical profile and evaluate the anxiolytic activity of S. paraensis bark through in vivo and in silico assays. The powdered bark was extracted with a hydromethanolic solution, yielding a red-colored extract (SP-EMB), which was analyzed by Ultra High Performance Liquid Chromatography coupled to Electrospray Ionization Mass Spectrometry and Quadrupole-Time-of-Flight Analyzer (UPLC-ESI-QToF-MS/MS). The neuropharmacological activity was evaluated in zebrafish (Danio rerio) using locomotor activity, light/dark, novel tank, GABAergic neuromodulation, and PTZ-induced seizure assays. UPLC-ESI-QToF-MS/MS analysis revealed 15 β-carboline alkaloids, 4 phenolic acid derivatives, and 1 phenolic glycoside. Harmane, the major constituent, was isolated by preparative HPLC and identified by UPLC-ESI-QToF-MS/MS and NMR analyses. SP-EMB exhibited anxiolytic-like effects in both light/dark and novel tank tests, with low acute toxicity (LD₅₀ > 400 mg·kg⁻¹) and reduced sedative effects compared to diazepam (DZP, 4 mg·kg⁻¹). Molecular docking showed that harmane and chlorogenic acid have high affinity for the GABA receptor, indicating their influence on the anxiolytic effect. Both compounds showed low toxicity (LD₅₀ > 40 mg·kg⁻¹) and dose-dependent anxiolytic-like activity without locomotor impairment. Furthermore, chlorogenic acid exhibited anxiolytic effects mediated by GABA receptors. These findings may suggest that S. paraensis is a promising alternative source of anxiolytic agents with lower sedative effects.
Integrated miniaturized direct ionization mass spectrometry and machine learning for discrimination and artificial mixing detection of Lonicerae japonicae Flos and Lonicerae Flos.
Zheng X, Deng Y, Zhang S … +5 more , Huang Z, Xiong W, Tang Y, Li W, Weng L
J Pharm Biomed Anal · 2026 Jun · PMID 42302551 · Publisher ↗
LJF (Lonicerae japonicae flos) is a high-value plant that is both edible and medicinal. It has multiple functions such as clearing heat, detoxifying and reducing inflammation, and is widely used in the field of food and...
LJF (Lonicerae japonicae flos) is a high-value plant that is both edible and medicinal. It has multiple functions such as clearing heat, detoxifying and reducing inflammation, and is widely used in the field of food and traditional Chinese medicine. Due to the low yeiled and high value of LJF, LF (Lonicerae flos), which has a similar appearance and lower price, is often used as LJF. This not only affects the medicinal quality but also poses a risk to clinical medication. Therefore, establishing rapid and reliable detection methods is crucial for market supervision and ensuring the safe use of drugs. This paper collects the characteristic mass spectra of two medicinal materials based on miniaturized direct ionization mass spectrometry. Through the integration of chemometrics and systematic comparison of pretreatment methods and prediction models, the combination of original data and random forest was ultimately chosen, enabling accurate prediction of unknown samples. Meanwhile, based on variable importance analysis from the random forest model, swertimarin was identified as the characteristic discriminating component in LJF. Finally, the TLC-MS method verified that the feature component mined by machine learning was consistent with that recorded in the pharmacopoeia. Miniaturized direct ionization mass spectrometry is unrestricted by environment or location and offers a high degree of flexibility. The integration with machine learning methods offers a promising proof-of-concept for rapid and accurate quality assessment of traditional Chinese medicine.
An improved method for quantification of cannabidiol, Δ-tetrahydrocannabinol, and their metabolites in human plasma and urine.
Zagzoog A, Michel D, Ha N … +6 more , Bachi K, Kudrich C, van Oort J, Hurd YL, Alcorn J, Laprairie RB
J Pharm Biomed Anal · 2026 Jun · PMID 42296921 · Publisher ↗
Cannabidiol (CBD), the second most prevalent phytocannabinoid in Cannabis sativa, potentially offers numerous therapeutic benefits without psychoactive effects. Research into CBD's therapeutic applications must be suppor...
Cannabidiol (CBD), the second most prevalent phytocannabinoid in Cannabis sativa, potentially offers numerous therapeutic benefits without psychoactive effects. Research into CBD's therapeutic applications must be supported by an understanding of the time course of CBD concentrations in the body and how these concentrations relate to CBD's safety and efficacy. This study aimed to develop a simplified protocol for quantifying CBD, Δ-Tetrahydrocannabinol (THC) and its metabolites in human plasma and urine, eliminating complex and time-consuming sample preparation, especially for urine samples, while maintaining accuracy comparable to traditional methods. This protocol was used to assess the influence of an oral capsule of CBD (BSPG CBD BRAINS Bioceutical laboratories) on the pharmacokinetics of CBD and its metabolites in plasma and urine relative to an FDA approved CBD formulation (Epidiolex®). The method development focused on optimizing mass spectrometry (MS) conditions with an ultra-high performance liquid chromatography (UHPLC) C18 column. Plasma and urine were collected at fourteen and eight time points, respectively, across 24 h and analyzed using liquid chromatography-tandem mass spectrometry (LC-MS/MS) to quantify CBD and its metabolites. Additionally, (THC) and its metabolites were examined, with no detectable levels found in either plasma or urine. This newly developed analytical method successfully quantified CBD and its metabolites in both plasma and urine, contributing valuable data to the understanding of CBD pharmacokinetics in different oral products. This study's findings have important implications for optimizing CBD administration and assessing therapeutic outcomes.
An integrated multi-technique strategy for in vitro metabolite identification and profiling of gymnodimine A using LC-HRMS/MS.
Chen J, Liu S, Liang S … +10 more , Zhong M, Li J, Ling L, Peng Y, Qu L, Zhang Y, Huang W, Li S, Wu J, Zhao J
J Pharm Biomed Anal · 2026 Jun · PMID 42296920 · Publisher ↗
Gymnodimine A (GYM-A) is a lipophilic cyclic imine toxin produced by marine dinoflagellates that accumulates in shellfish and poses potential risks to human health. However, regulatory limits have not been established wo...
Gymnodimine A (GYM-A) is a lipophilic cyclic imine toxin produced by marine dinoflagellates that accumulates in shellfish and poses potential risks to human health. However, regulatory limits have not been established worldwide, largely due to insufficient understanding of its metabolic pathways and toxicokinetic behavior. This study characterized the in vitro metabolism of GYM-A using human liver microsomes (HLM) and human liver S9 fractions (HS9) combined with liquid chromatography-high-resolution tandem mass spectrometry (LC-HRMS/MS). An integrated identification strategy incorporating segmented data-dependent acquisition (DDA), targeted/untargeted screening, MS/MS fingerprint comparison, density functional theory (DFT) calculation, and μElution solid phase extraction (SPE) enabled confident structural elucidation of metabolites derived from low-concentration substrates in complex matrices. Four phase I hydroxylated metabolites were identified: three mono-hydroxylated derivatives (M1-M3) and one di-hydroxylated derivative (M4), with 21-hydroxy-GYM-A (M1) as the highest relative abundance. No phase II glucuronide conjugates were detected under the conditions tested. Metabolic stability studies revealed high intrinsic clearance following first-order kinetics, with elimination primarily mediated by CYP450-dependent phase I oxidation. Enzyme phenotyping identified CYP3A5 as the principal isoform responsible for GYM-A hydroxylation. Detection of metabolite M2 in urine from dosed rats supported the in vitro findings. This work provides the first systematic metabolic profile of GYM-A and advances knowledge of its kinetic behavior, while the analytical workflow may serve as a useful tool for risk assessment and metabolism studies of related marine toxins.
Identification and characterization of polysaccharide from Paeoniae Radix Rubra, and its mechanism in alleviating anti-tuberculosis drug-induced liver injury based on integrating gut microbiota and non-targeted metabolomics.
Ren G, Duan H, Zou X … +2 more , Qu J, Wang H
J Pharm Biomed Anal · 2026 Jun · PMID 42296919 · Publisher ↗
A novel polysaccharide, designated PRRP2, was extracted from the dried root of Paeoniae Radix Rubra. Structural analysis suggested that the PRRP2 backbone was predominantly composed of →4)-Glcp-(1→ and →6)-Glcp-(1→ glyco...
A novel polysaccharide, designated PRRP2, was extracted from the dried root of Paeoniae Radix Rubra. Structural analysis suggested that the PRRP2 backbone was predominantly composed of →4)-Glcp-(1→ and →6)-Glcp-(1→ glycosidic linkages, with a trace amount of →2)-Xylp-(1→ embedded within the backbone. Supplementary PRRP2 effectively ameliorated rifampicin (RFP) + isoniazid (INH)-induced hepatic functional injury. PRRP2 also alleviated intestinal inflammation and enhanced intestinal barrier integrity in RFP + INH-induced liver injury mice. 16S rRNA sequencing results revealed that PRRP2 administration restored gut microbiota homeostasis by promoting the growth of beneficial bacteria, including Lachnospiraceae_NK4A136_group, Bacteroides, norank_f_Prevotellaceae, and Ligilactobacillus. Furthermore, PRRP2 prominently regulated bile acid (BA)-related metabolites in RFP + INH-induced liver injury mice. Supplementary PRRP2 reshaped the BA biosynthesis and excretion process possibly via the modulation of the farnesoid X receptor (FXR)-mediated signaling pathway. Collectively, PRRP2 shows promising prospects as a functional supplement for alleviating anti-tuberculosis drug-induced liver injury.
Corrigendum to "Identification of anticancer and cardioprotective quality markers in Chuanxiong Rhizoma using a bioassay driven effect-constituent index approach" [J. Pharm. Biomed. Anal. 277 (2026) 117507].
Yang J, Liu X, Fan L … +3 more , Qi S, Li C, Li G
J Pharm Biomed Anal · 2026 Jun · PMID 42287950 · Publisher ↗
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Development and validation of a time domain NMR relaxometric method for rapid screening of soybean oil adulteration in copaiba oil-resin.
Marinho MO, Vitolano LES, Santos YF … +5 more , Oliveira AJG, Xavier LA, Costa LAMA, Colnago LA, Machado MB
J Pharm Biomed Anal · 2026 Jun · PMID 42284919 · Publisher ↗
Copaiba oil-resin (CO), extracted from trunks of various copaiba species, has several therapeutic and cosmetic properties and is a valuable non-timber forest product that contributes to preservation of the Amazon rainfor...
Copaiba oil-resin (CO), extracted from trunks of various copaiba species, has several therapeutic and cosmetic properties and is a valuable non-timber forest product that contributes to preservation of the Amazon rainforest. Unfortunately, adulteration of this oil-resin with cheaper vegetable oils such as soybean oil (SO) has been common. In this paper, a method for the fast screening of SO in CO using time-domain NMR (TD NMR) relaxometry was developed and validated. CPMG relaxation measurements were performed by two analysts using two TD NMR instruments from different manufacturers. Strict temperature control, a low number of echoes, and a long echo time were required for adequate repeatability. The first derivative of CPMG decays and the percentage of SO in CO were modeled with partial least squares regression (PLSR). The first derivative of CPMG signal was found to minimize contributions of longer T components and to emphasize those of shorter T components, associated with more viscous components of the CO/SO mixture. As a result, the first derivative increased sensitivity of the method to the SO content. Results obtained with 1 latent variable showed an R²CV > 0.98, RMSECV between 2.9% and 4.7% SO, and LOQ values ranging from 29.3% to 48.3% SO, with an average close to 36% SO, lower than the adulteration level normally above 50%, but unable to monitor low-level contamination. The precision was assessed by repeatability (RMSEP 2.6 ± 0.5% SO) and intermediate precision (RMSEP 4.2 ± 1.0% SO). The results agreed with those obtained using established infrared and NMR spectroscopic methods. Therefore, this method shows potential for rapid and non-destructive screening of gross adulteration of CO with SO, as observed in Brazilian markets.
UHPLC-Q-Exactive Orbitrap MS-based brain-gut metabolomics implicates multi-pathway modulation by Ginseng stem-leaf saponins in chronic fatigue syndrome mice.
Wu W, Aishan S, Zhang M … +2 more , Chen X, Li H
J Pharm Biomed Anal · 2026 Jun · PMID 42284918 · Publisher ↗
Ginseng stem-leaf saponins (GSLS) were evaluated as potential bioactive food ingredients by characterizing brain-gut metabolic disturbances in a chronic fatigue syndrome (CFS) mouse model and assessing the regulatory eff...
Ginseng stem-leaf saponins (GSLS) were evaluated as potential bioactive food ingredients by characterizing brain-gut metabolic disturbances in a chronic fatigue syndrome (CFS) mouse model and assessing the regulatory effects of GSLS using ultra-high-performance liquid chromatography-Q-Exactive Orbitrap mass spectrometry (UHPLC-Q-Exactive Orbitrap MS). Male C57BL/6 mice were assigned to control, model, positive control, and GSLS groups (n = 6). A long-term forced-swimming induction protocol was used to establish fatigue-like phenotypes, and fecal and brain tissue samples were collected for untargeted metabolomics with multivariate and pathway analyses. Seventeen differential metabolites were identified in brain tissue and 17 in fecal samples in association with model induction and GSLS supplementation. The altered pathways were mainly related to lipid-derived mediators and membrane-lipid remodeling, including arachidonic acid metabolism, steroid biosynthesis, glycerophospholipid metabolism, ether lipid metabolism, and primary bile acid biosynthesis, with additional involvement of energy- and redox-relevant cofactor/vitamin metabolism, such as pantothenate and CoA biosynthesis, folate-mediated one-carbon metabolism, and lipoic acid metabolism. GSLS partly normalized fatigue-like brain and fecal metabolic abnormalities, suggesting potential links to brain-gut axis regulation involving neurotransmitter-related metabolism, hypothalamic-pituitary-adrenal (HPA)-axis-associated steroid metabolism, inflammation, and oxidative stress. These findings support GSLS as a promising bioactive ingredient for maintaining vitality and metabolic resilience in functional food applications.
A sensitive detection of C-reactive protein based on the combination of CRISPR/Cas13a, MNPs and RNase H.
Zhao D, Peng W, Liu Z … +4 more , Zhou Q, Wu L, Zhou Y, Ran F
J Pharm Biomed Anal · 2026 Jun · PMID 42284917 · Publisher ↗
C-reactive protein (CRP) is a potential risk factor for disease. Here, developed a rapid and accurate fluorescence biosensor for detecting CRP, which contributes to early diagnosis and timely treatment of diseases. The C...
C-reactive protein (CRP) is a potential risk factor for disease. Here, developed a rapid and accurate fluorescence biosensor for detecting CRP, which contributes to early diagnosis and timely treatment of diseases. The CRP binds with the aptamer resulting in the probe 1 (P1) releasing from the complex of aptamer/P1/magnetic nanoparticles (MNPs). After magnetic separation, the free P1 hybridized with the RNA (P2) modified on the MNPs, leading to the P2 being multiple-turnover cut by ribonuclease H (RNase H). The formed free RNA can specifically bind with the crRNA and the tans-cleavage activity of CRISPR/Cas13a was triggered, leading to the RNA reporter containing a dye and quencher pair being cleaved and generating the fluorescence signal. This developed fluorescent biosensor takes full advantage of the synergy of aptamer, RNase H, MNPs and CRISPR/Cas13a. Here, the developed fluorescent biosensor exhibits excellent sensitivity and specificity towards the detection of CRP with a linear range from 10 pg/mL to 200 ng/mL. The detection limit is low down to 7.5 pg/mL. Additionally, this method successfully detected the CRP in human serum samples with satisfactory recoveries. Therefore, this developed biosensor will offer a valuable tool for the rapid diagnosis of CRP-related diseases.
A novel electrochemical sensing with MIP for highly selective and sensitive determination of anticancer drug erlotinib.
Erdogan-Kablan S, Cetinkaya A, Unal MA … +3 more , Bellur Atici E, Nemutlu E, Ozkan SA
J Pharm Biomed Anal · 2026 Jun · PMID 42284916 · Publisher ↗
The sensitive and selective determination of targeted anticancer drugs is crucial for pharmaceutical quality control and therapeutic monitoring. Erlotinib (ERL), a tyrosine kinase inhibitor approved by the U.S. Food and...
The sensitive and selective determination of targeted anticancer drugs is crucial for pharmaceutical quality control and therapeutic monitoring. Erlotinib (ERL), a tyrosine kinase inhibitor approved by the U.S. Food and Drug Administration (FDA) for the treatment of metastatic or locally advanced non-small cell lung cancer (NSCLC), requires reliable analytical methods due to its clinical importance and potential impurities. In this study, an ultrasensitive nanomaterial-supported molecularly imprinted polymer (MIP)-based electrochemical sensor was rationally designed for the selective detection of ERL. Zinc oxide nanoparticles (ZnONPs) were incorporated to enhance the effective surface area and increase the density of active recognition sites. The polymeric film was synthesized using 3-aminophenyl boronic acid (3-APBA) as the functional monomer, ethylene glycol dimethacrylate (EGDMA) as the cross-linker, 2-hydroxyethyl methacrylate (HEMA) as the base monomer, and 2-hydroxy-2-methylpropiophenone as the initiator. The fabricated 3-APBA/ERL/ZnONPs@MIP-modified glassy carbon electrode (GCE) was characterized by scanning electron microscopy (SEM), electrochemical impedance spectroscopy (EIS), and cyclic voltammetry (CV). The sensor exhibited a linear response in the range of 1.0 × 10-1.0 × 10 M (100-1000 fM) with a limit of detection (LOD) of 1.89 × 10 M (18.9 fM) and a limit of quantification (LOQ) of 6.30 × 10 M (63.0 fM) (r = 0.997). Selectivity and specificity studies demonstrated that ERL could be accurately quantified even in the presence of structurally related drugs and ERL-related impurities at 1000-fold excess, yielding recovery values between 98.40% and 103.76%. The sensor was successfully applied to ERL determination in tablet dosage forms, demonstrating its suitability for pharmaceutical quality control. Furthermore, density functional theory (DFT) and Monte Carlo simulations elucidated the molecular recognition mechanism, revealing a precise "lock-and-key" fit of ERL within the imprinted cavities and supporting a target-induced "site-blocking" sensing mechanism.
Comprehensive profiling of chemical composition, plasma-absorbed prototypes, metabolites, and pharmacokinetics of Jiannao Bushen Pill in rats using UHPLC-MS and microdialysis.
Yu X, Kong L, Wang B … +7 more , Liu J, Lv X, Sun Q, Liu R, Zhao B, Lv J, Gao Y
J Pharm Biomed Anal · 2026 Jun · PMID 42275740 · Publisher ↗
Jiannao Bushen Pill (JNBSP) is a traditional Chinese medicine (TCM) preparation used for nourishing the brain and kidney, tonifying qi and spleen, calming the mind, and improving memory. Clinically, it has been widely ap...
Jiannao Bushen Pill (JNBSP) is a traditional Chinese medicine (TCM) preparation used for nourishing the brain and kidney, tonifying qi and spleen, calming the mind, and improving memory. Clinically, it has been widely applied for the treatment of amnesia and cognitive decline; however, its pharmacodynamic material basis remains largely unclear. In the present study, an ultra-high-performance liquid chromatography coupled with Q-Exactive Orbitrap high-resolution mass spectrometry (UHPLC-Q-Exactive Orbitrap-HRMS) strategy was established to systematically characterize the chemical constituents of JNBSP. A total of 181 compounds were identified, and their herbal origins were further assigned through comparison with the chemical profiles of the 25 individual medicinal materials comprising the formula. In addition, 40 prototype compounds absorbed into the bloodstream and 41 metabolites were tentatively characterized in rat plasma after oral administration of JNBSP. To further evaluate the in vivo exposure behavior of representative absorbed constituents, microdialysis sampling combined with ultra-high-performance liquid chromatography-triple quadrupole tandem mass spectrometry was employed to monitor the temporal concentration profiles of six prototype compounds. The results revealed comparable T values but different systemic exposure levels and elimination characteristics among these constituents, suggesting potentially different temporal and quantitative contributions to the pharmacological effects of JNBSP. To the best of our knowledge, this is the first systematic study to integrate comprehensive chemical profiling, characterization of absorbed prototypes and metabolites, and dynamic in vivo monitoring of representative constituents for JNBSP. These findings provide an important foundation for subsequent pharmacokinetic-pharmacodynamic studies, target identification, and mechanistic investigations of JNBSP in the treatment of cognitive dysfunction.
Comprehensive metabolic profiling of Dictamni Cortex in normal and rheumatoid arthritis rats using UHPLC-Q/TOF-MS/MS coupled with polygonal mass defect filtering.
Li Y, Guan W, Wen T … +9 more , Xu S, Hao Z, Chen Q, Zhang L, Liu S, Kuang H, Ma X, Huang L, Liu Y
J Pharm Biomed Anal · 2026 Jun · PMID 42269330 · Publisher ↗
Due to the low efficiency and time-consuming nature of detecting multiple metabolites from complex backgrounds-especially those with unpredictable metabolic types-as well as significant methodological limitations and dat...
Due to the low efficiency and time-consuming nature of detecting multiple metabolites from complex backgrounds-especially those with unpredictable metabolic types-as well as significant methodological limitations and data processing complexities, the in vivo metabolite profile analysis of herbs remains a major challenge. Therefore, this study developed an integrated strategy combining VBA background subtraction, polygonal mass defect filter (p-MDF), and untargeted metabolomics for identifying metabolites of quinoline alkaloids and limonoids. Through applying VBA background subtraction and p-MDF, the filtration ranges achieved for the biological samples were 19.30-24.34% and 78.32-85.46%, respectively. Finally, 108 compounds were efficiently and accurately identified from the water extract of Dictamni Cortex (DDW), including 84 quinoline alkaloids and 24 limonoids, among which 24 previously undescribed and 11 first-identified compounds were revealed. And a total of 158 compounds were detected in the plasma, urine, and feces of rheumatoid arthritis (RA) and normal rat following oral administration with DDW, including 69 prototype compounds and 89 metabolites. Untargeted metabolomics was performed to analyse plasma, urine, and feces samples from RA and normal rat. A total of 51, 28, and 9 differential parent compounds and metabolites were identified in the three sample types, respectively. It was speculated that the impact on the hepatointestinal environment and bioavailability under the RA state caused metabolic abnormalities in rats. In conclusion, this study provides a conceptual framework and methodological reference for the comprehensive analysis of herbal metabolites in complex biological matrices.
Validation of qualitative and quantitative methods for 40 benzodiazepines and Z-drugs in hair by UPLC-MS/MS.
Zhang M, Zhao J, Yu S … +3 more , Xiang P, Yan F, Yan H
J Pharm Biomed Anal · 2026 Jun · PMID 42263410 · Publisher ↗
In recent years, the analysis and identification of benzodiazepines and Z-drugs have presented significant challenges in forensic medicine and pharmaceutical analysis due to their widespread use. Notably, some of these s...
In recent years, the analysis and identification of benzodiazepines and Z-drugs have presented significant challenges in forensic medicine and pharmaceutical analysis due to their widespread use. Notably, some of these substances are classified as new psychoactive substances (NPS) by the UNODC. Hair was chosen as a biological matrix for monitoring long-term drug intake in this study. We aimed to develop and validate a rapid and sensitive method for simultaneous determination of 40 benzodiazepines and Z-drugs in hair using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). All the analytes were detected within 11 min. The method was validated with linear calibration curves over the range of 5-500 pg mg (coefficient of determination, r > 0.99). The limits of detection (LOD) were 1-3 pg mg, and the limits of quantification (LOQ) were 5 pg mg. The method demonstrated acceptable selectivity, accuracy, and precision (< 20%). Matrix effects ranged from -29.8-23.5%, and recoveries ranged from 77.9% to 119.9%. The method was successfully applied to six authentic hair samples, detecting nine substances: Nitrazepam, Temazepam, Lorazepam, 7-Aminoflunitrazepam, Clobazam, Lormetazepam, α-Hydroxyalprazolam, 7-Aminoclonazepam, and Zolpidem. Benzodiazepines concentrations ranged from 5.6 to 436.1 pg mg, while zolpidem concentrations ranged from 11.1 to 113.8 pg mg. This method provided a reliable tool for detecting benzodiazepines and Z-drugs in hair and addresses the requirements of routine forensic practice.
In-depth glycosylation and aspartic acid isomerization characterization of therapeutic fusion protein using electron transfer/higher-energy collision dissociation on the new hybrid high-resolution mass spectrometer.
Wu G, Zhang X, Du J … +4 more , Xu G, Guo L, Huang Z, Yu C
J Pharm Biomed Anal · 2026 Jun · PMID 42250337 · Publisher ↗
Glycosylation is a critical post-translational modification (PTM) in biotherapeutics that influences protein structure, stability, pharmacokinetics, biological activity, and immunogenicity. Comprehensive characterization...
Glycosylation is a critical post-translational modification (PTM) in biotherapeutics that influences protein structure, stability, pharmacokinetics, biological activity, and immunogenicity. Comprehensive characterization of glycosylation and other PTMs is therefore important for biopharmaceutical development and quality assessment. Aflibercept is a recombinant fusion protein containing five N-glycosylation sites and multiple potential O-glycosylation sites. Although site-specific N-glycosylation of aflibercept has been previously investigated, integrated characterization of glycosylation heterogeneity and aspartic acid (Asp) isomerization using an electron-transfer/higher-energy collision dissociation (EThcD) based workflow remains limited. In this study, EThcD data-dependent MS (ddMS) peptide mapping was performed on a Thermo Scientific Orbitrap Excedion Pro mass spectrometer equipped with the EASY-ETD option for detailed characterization of aflibercept. Site-specific N-glycosylation profiles at all five glycosylation sites were identified and relatively quantified. In addition, an O-glycopeptide localized at S12 was detected, providing direct experimental evidence supporting site-specific O-glycosylation in aflibercept. The EThcD fragmentation approach also enabled differentiation and localization of isoAsp residues through characteristic diagnostic fragment ions, including low-abundance peptides containing multiple Asp residues. Several additional PTMs, including deamidation and oxidation, were simultaneously characterized within the same analytical workflow. The results also indicate that EThcD peptide mapping can support the integrated multi-attribute method (MAM) concept for complex glycoproteins by combining glycosylation analysis, Asp/isoAsp differentiation, and PTM profiling in a single experiment. This workflow may be useful for detailed structural characterization and analytical comparability assessment of therapeutic glycoproteins and biosimilars.
Glycovariant-based diagnosis of bladder cancer using urinary mucin 1 and carcinoembryonic antigen.
Syed P, Islam MK, Kekki H … +5 more , Terävä J, Lamminmäki U, Boström PJ, Leivo J, Gidwani K
J Pharm Biomed Anal · 2026 Jun · PMID 42250336 · Publisher ↗
Glycan alterations, or glycovariants (GV), are well-recognized features of malignant transformation and are commonly observed in several cancers, including bladder cancer (BlCa). However, their integration into practical...
Glycan alterations, or glycovariants (GV), are well-recognized features of malignant transformation and are commonly observed in several cancers, including bladder cancer (BlCa). However, their integration into practical diagnostic assays remains limited. Here, we investigated whether glycan modifications on the urinary glycoproteins mucin 1 (MUC1) and carcinoembryonic antigen (CEA) could serve as diagnostic indicators for BlCa diagnosis. MUC1 and CEA were captured directly from urine samples of patients with benign prostate disease (n = 20) and BlCa (n = 19) by immobilizing monoclonal antibodies against these glycoproteins on microtitration wells. Cancer-associated glycan structures were detected using wheat germ agglutinin (WGA) lectin and glycan-specific antibody C241 (a clone of anti-carbohydrate antigen 19-9), both conjugated to Eu-doped nanoparticles. This glycovariant-based detection approach enables selective recognition of disease-associated glycoforms. By combining assay results, several models were constructed to evaluate marker panels with improved sensitivity and selectivity. A combined diagnostic model incorporating MUC1-WGA and CEA-C241 immunoassays, designed to detect N-acetylglucosamine (GlcNAc) on MUC1 and sialyl-Lewis (sLe) structures on CEA, achieved approximately 95% sensitivity and 95% selectivity for identifying bladder cancer. The MUC1-WGA assay alone distinguished cases with 79% sensitivity and 95% selectivity, while other individual GV assays demonstrated comparatively lower sensitivities. In contrast, conventional protein-level measurements showed lower diagnostic performance. Concurrent detection of glycan alterations on MUC1 and CEA improved discrimination between bladder cancer and benign conditions. This GV-assay framework provides a modular platform that can be extended to incorporate additional urinary biomarkers. However, validation in larger patient cohorts is required to confirm clinical applicability.
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