Journal Of Pharmaceutical And Biomedical Analysis[JOURNAL]
Sun
200 papers
Metabolic disparities of potentially toxic components derived from Psoraleae Fructus and Euodiae Fructus within the Sishen wan influenced by varying compatibilities and physiological conditions in an in vitro gut microbiota model.
Hong L, Ma L, Dong J … +5 more , Li X, Zou Y, Tian Q, Dong Y, Yang W
J Pharm Biomed Anal · 2026 Aug · PMID 41844463 · Publisher ↗
Sishen wan (SSW) is utilized in the treatment of irritable bowel syndrome (IBS). This study aimed to compare gut microbiota-mediated metabolic profiles of potential toxicants derived from Psoraleae Fructus (PF) and Euodi...
Sishen wan (SSW) is utilized in the treatment of irritable bowel syndrome (IBS). This study aimed to compare gut microbiota-mediated metabolic profiles of potential toxicants derived from Psoraleae Fructus (PF) and Euodiae Fructus (EF) in mice. Data analysis was performed using ultra-high-performance liquid chromatography/ion mobility-quadrupole time-of-flight mass spectrometry (UHPLC/IM-QTOF-MS) coupled with an in-house in vivo MS spectral database. An increase was observed in the peak area of coumarin compounds, indicating their metabolic transformation was inhibited by intestinal flora following compatibility. Regarding flavonoids, Myristicae Semen (MyS) and EF suppressed gut microbiota-mediated transformation under normal conditions, whereas Schisandrae Chinensis Fructus (SCF) exerted ed the opposite effect. Under IBS conditions, MyS and Quefang (QF) inhibited gut microbiota-mediated transformation, while EF exhibited the opposite effect. The peak areas of alkaloids increased, whereas those of triterpenoids decreased, suggesting that compatibility prevented alkaloid transformation while promoting triterpenoid metabolism by gut microbiota. MyS and SCF enhanced the overall metabolism of PF, while EF exhibited an inhibitory effect. After compatibility, EF metabolites increased in normal mice but decreased in IBS mice. Compared to the normal state, IBS mice showed higher peak areas for all potentially toxic components, with lower metabolite quantities (expect for EF, which demonstrated the opposite effect). PF and its compatibility group predominantly underwent oxidation, hydration, and reduction metabolism, whereas EF and its compatibility group favored oxidation, methylation/demethylation, reduction, and hydration reactions. These results provide further insight into the chemical mechanisms underlying the "compatibility attenuation" effect of SSW.
Isolation and identification of the designer benzodiazepine cyclopropylflualprazolam in pressed candies marketed for sleep improvement.
Liu X, Zhao L, Dong P … +2 more , Ge X, Xiang X
J Pharm Biomed Anal · 2026 Aug · PMID 41830715 · Publisher ↗
A novel alprazolam analog was detected as an illegal additive in pressed candies marketed for sleep improvement using high-performance liquid chromatography (HPLC)-diode array detection (DAD). The compound was further is...
A novel alprazolam analog was detected as an illegal additive in pressed candies marketed for sleep improvement using high-performance liquid chromatography (HPLC)-diode array detection (DAD). The compound was further isolated and purified via semi-preparative liquid chromatography, and its chemical structure was elucidated through high-resolution mass spectrometry (HRMS) and nuclear magnetic resonance (NMR) spectroscopy. The compound was identified as cyclopropylflualprazolam. Since alprazolam is a psychotropic controlled substance, this finding has garnered significant attention from regulatory authorities. It is recommended that cyclopropylflualprazolam be included in the screening list of prohibited substances in functional foods.
E-nose, HS-SPME-GC-MS and untargeted metabolomics reveal effects on Co gamma irradiation of Neng-An-Jun-Ning Pills: Changes in odor and chemical compositions.
Wang Z, An J, Daji R … +7 more , Peng G, Wei X, Su R, Liu S, Qiang R, Gu R, Zhong S
J Pharm Biomed Anal · 2026 Aug · PMID 41830714 · Publisher ↗
Tibetan medicinal preparations are mainly composed of crude medicinal powder, which are susceptible to microbial contamination. Due to its high efficiency and low-treatment characteristics, ⁶⁰Co gamma irradiation is curr...
Tibetan medicinal preparations are mainly composed of crude medicinal powder, which are susceptible to microbial contamination. Due to its high efficiency and low-treatment characteristics, ⁶⁰Co gamma irradiation is currently the most commonly used sterilization method for Chinese medicinal materials and their preparations. This study investigates the impact of ⁶⁰Co gamma irradiation on the Neng-An-Jun-Ning Pill (NJP), a Tibetan medicinal preparation rich in aromatic herbs. The research aims to evaluate the impact of ⁶⁰Co gamma irradiation on the odor, volatile chemical compounds, and main active ingredients of NJP due to irradiation changes. The aim is to evaluate the effects of various irradiation doses on the odor, volatile compounds, and key active ingredients of NJP, while establishing an appropriate dose through microbial limit testing Untargeted metabolomics was used to evaluate the changes in compound composition of this formula preparation under this dose. NJP samples were irradiated with ⁶⁰Co gamma at doses of 3, 6, 10, 15, and 20 kGy. The results of the E-nose (Electronic nose) analysis showed that sensors S1 and S8 demonstrated high sensitivity to the odor of NJP. Meanwhile, HS-SPME-GC-MS (Headspace solid-phase microextraction-gas chromatography- mass spectrometry) identified 50 volatile compounds, predominantly alkenes, esters, and phenolic compounds. In irradiated samples, alkene and phenolic content increased while ester content decreased. GC-MS results showed that Calamenene and Methyl Tetradecanoate only exist in irradiated groups, which may serve as indicator compounds to determine whether the product has undergone irradiation. Analysis of data from all experimental groups led to the identification of 18 differential volatile compounds. HPLC analysis showed that at 15 and 20 kGy, hydroxysafflor yellow A and ellagic acid decreased significantly, while eugenol content increased. Therefore, the overall results showed the optimal ⁶⁰Co gamma irradiation dose for NJP was 6 kGy, considering sterility compliance (dose ≥6 kGy), minimal odor, and major active ingredients' impact at medium doses, and adherence to irradiation guidelines. Under 6 kGy irradiation, UPLC-Q Exactive MS (Ultra-high-performance liquid chromatography coupled with quadrupole - Exactive mass spectrometry) detected 2084 compounds, mainly terpenoids and flavonoids. Through chemometrics analysis, 616 differential compounds were identified. This study provides a theoretical basis for the irradiation processing and quality control of Tibetan medicinal preparations such as NJP, and also serves as a valuable reference for the development of irradiation technology in Tibetan medicine and traditional Chinese medicine.
Polysaccharide-driven quality control of Gastrodia elata Blume: A multidimensional strategy integrating LC-MS/MS-based quantitative analysis, machine learning, and anti-neuroinflammatory bioactivity.
Kong X, Chen S, Shen L … +11 more , Wu W, Yang X, Li N, Huo J, Zhou Y, Long H, He H, Tian M, Zhang Z, Hou J, Wu W
J Pharm Biomed Anal · 2026 Aug · PMID 41830713 · Publisher ↗
Gastrodia elata Blume (GE), a highly regarded traditional Chinese medicinal herb, is widely recognized for its diverse pharmacological activities. Current quality control primarily relies on small molecule biomarkers, ye...
Gastrodia elata Blume (GE), a highly regarded traditional Chinese medicinal herb, is widely recognized for its diverse pharmacological activities. Current quality control primarily relies on small molecule biomarkers, yet critical research gaps persist in understanding the complex interactions of the key ingredient, Gastrodia elata polysaccharides (GEP), with bioactivity-related quality due to analytical challenges. To overcome the limitations of traditional non-specific degradation methods, this study established a novel multidimensional quality control strategy using optimized α-amylase-assisted Fenton's initiation toward defined oligosaccharide groups (FITDOG) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the simultaneous qualitative and quantitative characterization of specific GEP domains. Analysis of 205 batches across varying grades and origins identified α-1,4/1,6-glucans (0.3-40%) as robust, grade-dependent markers. Integration of these macromolecular profiles with small-molecule markers into an Extreme Gradient Boosting (XGBoost) model, superior cultivar discrimination was achieved (Area Under the Curve, AUC > 0.89), while SHapley Additive exPlanations (SHAP) analysis highlighting the predictive significance of the glucan content. Analytical findings were biologically validated in lipopolysaccharide (LPS)-stimulated human microglial clone 3 cells (HMC3), demonstrating that elevated levels of these α-1,4/1,6-glucans significantly correlated with enhanced cell viability (p < 0.05) and anti-neuroinflammatory regulation, characterized by suppression of IL6 and upregulation of TGFB1. This study proposes α-1,4/1,6-glucans as novel quality markers for GE and establishes a robust analytical framework that integrates chemical profiling and biological validation. This advancement enhances the precision of quality control in traditional Chinese medicine and underscores the potential of polysaccharide-driven strategies for the standardization of medicinal herbs.
Detection and quantification of ezetimibe and its major glucuronide in patients with hepatic impairment via liquid chromatography-tandem mass spectrometry.
Farrera DO, Maloney MM, LaMadrid CS … +3 more , Lenzen-Hammerel P, Radtke LR, Cherrington NJ
J Pharm Biomed Anal · 2026 Aug · PMID 41818831 · Full text
Following administration of ezetimibe (EZE), levels of the glucuronidated metabolite ezetimibe-glucuronide (EZEG) are altered in patients with hepatic impairment. A rapid and sensitive liquid chromatography-tandem mass s...
Following administration of ezetimibe (EZE), levels of the glucuronidated metabolite ezetimibe-glucuronide (EZEG) are altered in patients with hepatic impairment. A rapid and sensitive liquid chromatography-tandem mass spectrometry method (LC-MS/MS) method was developed and validated to quantify EZE and EZEG in human plasma and urine. Samples were prepared using a protein precipitation procedure with methanol containing stable isotope-labeled internal standards (EZE-d and EZEG-d). Separation of the analytes was achieved using acetonitrile-water (0.1% formic acid) as the mobile phase at a flow rate of 0.5 mL/min on a C18 column. The analytes were detected using negative ionization in multiple reaction monitoring (MRM) mode. The mass transition pairs of m/z 408.4→271.0 and m/z 584.5→271.0 were used to quantify EZE and EZEG, respectively. The method was linear over a concentration range of 1.5 ng/mL - 1 µg/mL for EZE and EZEG in the plasma. In the urine, EZE was detectable a linear range of 5 ng/mL - 1 µg/mL and EZEG ranged from 3 ng/mL - 1 µg/mL. The method was validated in accordance with U.S. Food and Drug Administration and European Medicines Agency regulatory standards, including specificity, sensitivity, stability, repeatability and reproducibility. This ensures accuracy and reliability of test results which thereby enhances patient safety and helps support clinical decisions.
Metabolic profile of 25E-NBOH in human liver microsomes, rat urine, and fungus Cunninghamella elegans.
Vágnerová M, Palivec P, Mrňavá M … +9 more , Mizerová E, Jurásek B, Rimpelová S, Sácký J, Šíchová K, Vejmola Č, Páleníček T, Sýkora D, Kuchař M
J Pharm Biomed Anal · 2026 Aug · PMID 41812548 · Publisher ↗
N-benzylphenethylamines are a class of new psychoactive substances (NPS) that are increasingly being used as recreational drugs with a wide range of adverse effects, possibly even death. Currently, the appearance of new...
N-benzylphenethylamines are a class of new psychoactive substances (NPS) that are increasingly being used as recreational drugs with a wide range of adverse effects, possibly even death. Currently, the appearance of new N-benzylphenethylamines far outweighs the studies of their metabolism. One of such compounds, 25E-NBOH, has been on the market for the last seven years but its pharmacological and toxicological effects have not yet been thoroughly reported. To provide a basis for such studies, we investigated 25E-NBOH metabolism in three different systems: human liver microsomes, Wistar rat urine, and Cunninghamella elegans fungus, which contains enzymes similar to those found in mammals and serves as an environmentally sustainable and ethically favourable alternative to animal-based metabolic models. Untargeted LC-HRMS/MS was used to detect phase I and phase II 25E-NBOH metabolites in all three systems. A total of 56 metabolites were annotated, many of which occurred in multiple isomeric forms. Despite metabolic differences between the systems, several abundant metabolites were found in all of them. The primary metabolic pathways detected were hydroxylation at various positions, O-demethylation, and N-debenzylation, followed by conjugation with glucuronic acid, sulphate, or glucose. To confirm the presence of metabolites, we synthesised and measured ten substances under the same LC-HRMS/MS conditions as the real samples. Seven of these were successfully matched to detected metabolites based on retention time and MS/MS spectra, enabling structural assignment and isomer distinction. Additionally, the identity of 2C-E, a known psychoactive substance, was confirmed as one of the metabolites using a commercial reference standard. Lastly, we report the structures of three main biomarkers, suggested by both this study and prior literature. This study provides the first comprehensive in vitro and in vivo metabolic profile of 25E-NBOH, identifying the structures of specific metabolites using in-house synthesised reference standards and proposing structures for the main biomarkers. These findings establish a solid foundation for future pharmacological and toxicological studies, supporting clinicians in the accurate diagnosis of intoxication cases.
Corrigendum to "Systematic characterization of chemical constituents and in vivo metabolites of Jiuwei Qianghuo Granules by UPLC-Q-TOF-MS/MS" [J. Pharm. Biomed. Anal. 274 (2026) 117443].
Xu Z, Zhou C, Wu M … +7 more , Sun S, Wu H, Xia J, Zhou M, Zhu Y, Xiang B, Yao Y
J Pharm Biomed Anal · 2026 Aug · PMID 41797083 · Publisher ↗
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Untargeted LC-MS-based metabolic fingerprinting of Escherichia coli-associated urinary tract infections and urosepsis: Insights into the urine, serum, and bacterial interactomes.
Wityk P, Raczak-Gutknecht J, Biesemans M … +3 more , Krawczyk B, Brzezińska W, Markuszewski MJ
J Pharm Biomed Anal · 2026 Aug · PMID 41793926 · Publisher ↗
Urinary tract infections (UTIs) and urosepsis necessitate a deeper understanding of host-pathogen interactions at the metabolic level. We use LC-MS and GC-MS techniques to characterize metabolic pathway alterations in pa...
Urinary tract infections (UTIs) and urosepsis necessitate a deeper understanding of host-pathogen interactions at the metabolic level. We use LC-MS and GC-MS techniques to characterize metabolic pathway alterations in patients and Escherichia coli isolates during UTI and urosepsis. Our findings reveal substantial metabolic adaptations in the human host, including increased porphyrin metabolism, suggesting oxidative stress response or tissue damage. Activation of the pentose phosphate pathway (PPP) and tricarboxylic acid cycle (TCA) highlights the host's heightened immune and energy demands during infection. Additionally, enhanced malate-aspartate shuttle activity suggests a greater reliance on glycolysis for energy production, while increased pyruvaldehyde degradation indicates active detoxification of harmful metabolic byproducts. In E. coli, distinct metabolic shifts depended on the extracellular/intracellular niche and infection stage. Intracellular metabolites of E. coli during urosepsis exhibited upregulated purine and biotin metabolism, reflecting a focus on replication and essential metabolic functions. Conversely, intracellular metabolites of E. coli during UTI displayed increased aspartate metabolism, TCA cycle activity, Warburg effect, fatty acid biosynthesis, and glycine/serine metabolism, indicative of urinary tract adaptation. Extracellular metabolites of E. coli during urosepsis exhibited a broad activation of sugar metabolism, highlighting its ability to exploit diverse nutrient sources in systemic infection. In contrast, extracellular metabolites of E. coli during UTI demonstrated specific metabolic changes, including propanoate metabolism activation and homocysteine dysregulation, reflecting unique urinary tract conditions. These findings provide insights into the metabolic pathways employed by host and pathogen during UTI and urosepsis, uncovering potential metabolic vulnerabilities in E. coli.
Unraveling the heterogeneity of hyperuricemia using untargeted metabolomics and statistical modeling.
Wang J, Zeng Z, Duan W … +3 more , Man Z, Wang M, Yang Z
J Pharm Biomed Anal · 2026 Aug · PMID 41791282 · Publisher ↗
Hyperuricemia is the second most prevalent metabolic disorder globally and exhibits pronounced heterogeneity in clinical practice. Only about 10% of individuals with asymptomatic hyperuricemia (HUA) progress to gout, yet...
Hyperuricemia is the second most prevalent metabolic disorder globally and exhibits pronounced heterogeneity in clinical practice. Only about 10% of individuals with asymptomatic hyperuricemia (HUA) progress to gout, yet the lack of specific biomarkers and precise therapeutic targets hinders accurate prediction of disease progression. This work focuses on investigating the heterogeneity of hyperuricemia, aiming to elucidate potential mechanisms underlying its transition from asymptomatic to symptomatic stages. A total of 107 serum samples were analyzed, including 36 healthy controls (Con), and 30, 32 and 9 patients with HUA, gouty arthritis (gout), and gout complicated by uric acid nephrolithiasis (UAN), respectively. Using an advanced SCIEX ZenoTOF 7600-based untargeted metabolomics platform, 925 metabolites were identified in both positive and negative ionization modes. The assessment of quality control (QC) samples showed high precision in instrumental measurement with RSD values of the ion features less than 30% achieving 91.76% and 89.73% respectively in the two ionization modes. A total of 46, 37, 28, and 26 differential metabolites were identified among the four groups. Among them, four metabolites showed high sensitivity and specificity in the analysis of the first three groups. Five metabolic pathways remained consistently dysregulated throughout disease progression, which indicates their potential as mechanistic drivers. These findings provide novel biological insights for the early diagnosis and precision treatment of gout and its complications, and offer a crucial foundation for understanding the metabolic basis of hyperuricemia heterogeneity.
Development of a MS binding assay to analyze the interactions of drugs with the ifenprodil binding site of NMDA receptors with GluN2B subunit.
Grey L, Fabian J, Schepmann D … +1 more , Wünsch B
J Pharm Biomed Anal · 2026 Jul · PMID 41764828 · Publisher ↗
Negative allosteric modulators interacting with the ifenprodil binding site of NMDA receptors with GluN2B subunit are of particular interest for the treatment of psychiatric and neurodegenerative disorders. In order to e...
Negative allosteric modulators interacting with the ifenprodil binding site of NMDA receptors with GluN2B subunit are of particular interest for the treatment of psychiatric and neurodegenerative disorders. In order to eliminate the radioligand [H]ifenprodil in the standard radioactive binding assay, a novel MS binding assay was established and validated making use of the quantitative determination of non-radioactive ifenprodil by triple quadrupole MS. Kinetic, saturation and competitive experiments were carried out in a stepwise and iterative manner to optimize the final assay conditions. Under optimized assay conditions, the MS binding assay provided a K value for the marker ifenprodil (K = 11 nM), which is comparable with the K value obtained in the radioligand binding assay for [H]ifenprodil (K = 7.6 nM). Although the MS binding assay led to higher K values for known NMDA receptor antagonists, both assays showed the same trend of K values for these inhibitors.
Development and validation of an efficient and sensitive LC-MS/MS assay for simultaneous determination of the high frequency used antibody drug conjugate payload MMAE and anti-vascular tyrosine kinase inhibitor lenvatinib in human plasma.
Wen Y, Wang W, Ma X … +4 more , Liu H, Yin Y, Li R, Jiao Y
J Pharm Biomed Anal · 2026 Jul · PMID 41762484 · Publisher ↗
Antibody drug conjugates (ADCs)-based combination therapies are increasingly studied in clinics. Monomethyl auristatin E (MMAE) is the most frequently used payload in approved ADCs and lenvatinib is a classic anti-vascul...
Antibody drug conjugates (ADCs)-based combination therapies are increasingly studied in clinics. Monomethyl auristatin E (MMAE) is the most frequently used payload in approved ADCs and lenvatinib is a classic anti-vascular tyrosine kinase inhibitor. This study aimed to develop a liquid chromatography tandem mass spectrometry (LC-MS/MS) assay for simultaneous determining these two analytes in human plasma. Protein precipitation by methanol was used in sample preparation with deuterated agents as internal standards. A Kinetex C18 column (3.0 × 50 mm, 2.6 μm) was used with gradient elution (0.5 mL/min, 40 °C). Positive electrospray ionization in multiple reaction monitoring (MRM) mode was used for detection. Each run needs 50 μL sample and 3 min. The developed assay was linear over 0.20-100 ng/mL for MMAE and over 1.00-500 ng/mL for lenvatinib, which covered reported pharmacokinetic (PK) ranges for both agents. This assay was validated according to ICH M10 and was qualified in terms of selectivity, linearity, accuracy (-6.7 % to 4.5 %), precision (1.5-7.4 %), matrix effects, dilution test, carry-over and stability in human plasma. The in vitro studies suggested no significant in-process release for conjugated MMAE from two ADCs with protease-cleavable maleimidocaproylvaline-citrulline-p-aminobenzyloxycarbonyl linker. Clinical samples were efficiently analyzed and values fell in reported PK ranges. Overall, the developed method is robust and efficient and will potentially support clinical PK studies or therapeutic drug monitoring (TDM) for MMAE-containing ADCs and lenvatinib alone or in combinations. This method also serves as a starting point to build cassette assay by including more tyrosine kinase inhibitors.
Pharmaceutical insights into nanoscale drug delivery systems and chromatographic approaches for melanoma treatment.
Deljavan Ghodrati A, Gebrehiwot W, Amasya G … +2 more , Gumustas M, Sengel-Turk CT
J Pharm Biomed Anal · 2026 Jul · PMID 41762483 · Publisher ↗
Due to its potential for metastasis and resistance to standard treatments, melanoma, a very aggressive type of skin cancer, presents substantial challenges in clinical care. Nanocarrier based approaches have become a via...
Due to its potential for metastasis and resistance to standard treatments, melanoma, a very aggressive type of skin cancer, presents substantial challenges in clinical care. Nanocarrier based approaches have become a viable tactic to overcome these limitations. This review offers a thorough analysis of melanoma, its molecular basis, and innovative therapeutic strategies. It emphasizes the revolutionary potential of nanoparticles in melanoma therapy, leveraging their unique properties for targeted drug delivery and imaging. Several nanoparticle formulations are explored, demonstrating how they can improve treatment efficacy, reduce adverse effects, and overcome drug resistance mechanisms. These formulations include liposomes, polymeric nanoparticles, and inorganic nanoparticles. In addition, chromatographic analyses of these nanoscale systems are reviewed, highlighting their essential role in characterizing drug-nanocarrier interactions, assessing stability, and ensuring quality control in pharmaceutical development. Furthermore, novel tactics including personalized nanomedicine and combination therapies are investigated to maximize treatment results. Despite notable progress, challenges such as nanoparticle stability and translational barriers necessitate further research efforts. Overall, nanoparticle-based therapies offer a promising avenue for advancing melanoma treatment, ushering in a new era of precision medicine and improved patient care.
Investigation of distinct metabolic profiles in the phloem and xylem of Rehmanniae Radix using untargeted metabolomics coupled with quantification of glycosides.
Shang T, Liu H, Zhu J … +7 more , Su C, Wang R, Zhang J, Gong H, Yang C, Xie C, Lei J
J Pharm Biomed Anal · 2026 Jul · PMID 41762482 · Publisher ↗
This study aimed to investigate the composition and differences in phytochemicals between the phloem and xylem of Rehmanniae Radix (RR). The metabolic profiles of two tissues were comprehensively characterized using unta...
This study aimed to investigate the composition and differences in phytochemicals between the phloem and xylem of Rehmanniae Radix (RR). The metabolic profiles of two tissues were comprehensively characterized using untargeted metabolomics, and the relative abundance of metabolites was analyzed. Subsequently, the primary differential components, identified as glycosides, were quantified in two tissues using ultra-high-performance liquid chromatography (UHPLC). Using the untargeted metabolomic approach, 3854 metabolites were identified in two tissues, categorized into 21 classes including glycolipids, heterocyclic compounds, terpenoids, phenolic acids, and amino acids and derivatives. Principal component analysis (PCA) revealed significant differences in the metabolite profiles between two tissues of RR, and 1279 different metabolites were screened, of which 1098 were up-regulated and 181 were down-regulated. Kyoto Encyclopedia of Genes and Genomes (KEGG) enrichment analysis indicated that these differential metabolites were involved in 72 metabolic pathways, with the majority being associated with plant metabolism. Quantification analysis of glycosides resulted in the identification of 5 iridoid glycosides and 6 phenylethanoid glycosides in two tissues of RR, with the total glycosides content found to be higher in the phloem. The key components differentiating the quality of the phloem and xylem were the iridoid glycosides catalpol and the phenylethanoid glycosides acteoside and echinacoside. Collectively, these findings elucidate the similarities and differences in chemical constituents between the phloem and xylem of RR, thereby providing the scientific foundation for its quality evaluation and the selection of superior cultivars.
Ultra-sensitive HPLC-ESI-MS/MS quantitation of N-nitroso-phenylephrine in phenylephrine-containing anticold products.
Szabó PT, Darcsi A, Turczel G … +1 more , Keserű GM
J Pharm Biomed Anal · 2026 Jul · PMID 41762481 · Publisher ↗
Phenylephrine is widely used in anticold medications and contains a secondary amine moiety capable of forming N-nitroso-phenylephrine (NNPE), a potentially carcinogenic nitrosamine impurity. Despite increasing attention...
Phenylephrine is widely used in anticold medications and contains a secondary amine moiety capable of forming N-nitroso-phenylephrine (NNPE), a potentially carcinogenic nitrosamine impurity. Despite increasing attention to nitrosamine contamination in pharmaceuticals, no dedicated analytical method has been reported for the determination of NNPE at trace levels in complex drug formulations. In this study, a highly sensitive and selective HPLC-ESI-MS/MS method was developed and validated for the quantitation of NNPE in phenylephrine-containing anticold products. Chromatographic separation was achieved using reversed-phase conditions, and detection was performed by triple-quadrupole mass spectrometry operated in multiple-reaction monitoring mode. Method validation followed the ICH Q2(R2) guideline and demonstrated excellent linearity, accuracy, and precision, with a limit of detection of 1.95 pg/mL and a limit of quantification of 3.9 pg/mL. Sample preparation was intentionally kept simple and representative of routine quality control practice, relying on direct aqueous dissolution without extensive clean-up. Matrix effects were systematically evaluated and shown not to compromise quantitative performance due to effective compensation by the isotopically labelled internal standard. The validated method was applied to commercially available anticold products, revealing measurable NNPE levels in all samples analysed, with several products exceeding currently applied acceptable intake limits. The proposed method provides a reliable analytical tool for trace-level NNPE determination and is suitable for routine quality control and safety assessment of phenylephrine-containing pharmaceutical products.
Pharmacokinetic profiling of the bioactive components of Sijunzi Decoction in a rat model of breast cancer: Insights into herb-drug interactions with cyclophosphamide.
Zhang Z, Zhang Y, Gao R … +3 more , Zhao C, Zhao M, Huang Y
J Pharm Biomed Anal · 2026 Jul · PMID 41762480 · Publisher ↗
This study investigated the pharmacokinetics of Sijunzi Decoction (SJZD) components and their interactions with cyclophosphamide (CTX) in breast cancer (BC) rats. The BC model was induced using 7,12-dimethylbenz[a]anthra...
This study investigated the pharmacokinetics of Sijunzi Decoction (SJZD) components and their interactions with cyclophosphamide (CTX) in breast cancer (BC) rats. The BC model was induced using 7,12-dimethylbenz[a]anthracene (DMBA). Using UPLC-Orbitrap-MS/MS, we identified 23 SJZD-derived compounds in rat plasma. Subsequently, a validated UPLC-TQ-MS/MS method was developed to quantify seven bioactive analytes. Compared with normal rats, BC model rats exhibited significantly altered pharmacokinetics: ginsenosides Rb1 and Rc showed enhanced systemic exposure and prolonged elimination, whereas the clearance of glycyrrhetinic acid was accelerated. Co-administration with CTX further increased the absorption of ginsenosides but markedly reduced the exposure and accelerated the clearance of licorice-derived compounds (liquiritin, isoliquiritigenin, formononetin, and glycyrrhetinic acid). These findings indicate that breast cancer pathology significantly alters the in vivo disposition of SJZD components, and that CTX induces complex herb-drug interactions. This study provides a critical pharmacokinetic basis for the rational clinical application of SJZD as an adjuvant therapy in breast cancer patients, particularly when combined with chemotherapy.
Identification of characteristic volatile compounds in Artemisiae argyi Levl. et Vant. from diverse origins using E-nose and HS-GC-IMS.
Ma R, Zhang R, Feng W … +6 more , Liu X, Lian C, Liu J, Yang J, Gui X, Chen S
J Pharm Biomed Anal · 2026 Jul · PMID 41762479 · Publisher ↗
Artemisia argyi Levl. et Vant., a traditional Chinese medicinal herb, is highly regarded for its therapeutic properties, including antimicrobial, anti-inflammatory, analgesic, and anticancer effects. However, the quality...
Artemisia argyi Levl. et Vant., a traditional Chinese medicinal herb, is highly regarded for its therapeutic properties, including antimicrobial, anti-inflammatory, analgesic, and anticancer effects. However, the quality of A. argyi varies considerably due to factors such as climate, cultivation practices, and harvest timing. This study investigated the volatile compound profiles of A. argyi from six different regions using an electronic nose (E-nose) and headspace gas chromatography-ion mobility spectrometry (HS-GC-IMS). A total of 106 volatile compounds were identified by HS-GC-IMS, and terpenoids accounted for 39.62 % of the total, underscoring their importance in the chemical composition of A. argyi. E-nose sensor responses indicated that W1W and W2W exhibited the highest sensitivity, with the strongest signals observed in samples from Qichun (QC). By integrating variable importance in projection (VIP ≥ 1) and OPLS-DA results (P < 0.05), 28 key volatile compounds and 2 E-nose sensors (W1W and W2W) were identified as significant contributors to regional variations. Correlation analysis between HS-GC-IMS and E-nose data revealed 15 significantly differentiated compounds, six of which were common to both datasets, indicating their potential as reliable markers for geographic origin identification. These findings provide a methodological reference for the differentiation and quality control of A. argyi from diverse geographical regions.
Corrigendum to "High-throughput quantitation of serological dimethylarginines by LC/MS/MS: Potential cardiovascular biomarkers for rheumatoid arthritis", [J. Pharm. Biomed. Anal., vol. 232, Article Number 115336].
Huang Q, Liu Y, Cheng Y … +11 more , Jia F, Pu C, Yan Q, Chang Z, Liao P, Ma D, Xu L, Zhang H, Lu Y, Liu X, Liu K
J Pharm Biomed Anal · 2026 Jul · PMID 41747490 · Publisher ↗
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Systematic characterization of chemical constituents and in vivo metabolites of Jiuwei Qianghuo Granules by UPLC-Q-TOF-MS/MS.
Xu Z, Zhou C, Wu M … +7 more , Sun S, Wu H, Xia J, Zhou M, Zhu Y, Xiang B, Yao Y
J Pharm Biomed Anal · 2026 Jul · PMID 41747489 · Publisher ↗
Jiuwei Qianghuo Granules (JWQHG), a classical traditional Chinese medicinal preparation composed of nine herbs, has been widely used in clinical practice for centuries. However, its chemical composition and metabolic fat...
Jiuwei Qianghuo Granules (JWQHG), a classical traditional Chinese medicinal preparation composed of nine herbs, has been widely used in clinical practice for centuries. However, its chemical composition and metabolic fate in vivo remain insufficiently characterized, which limits our understanding of its therapeutic mechanisms. Therefore, this study aims to systematically characterize its chemical constituents and identify the absorbed and metabolized components in vivo following oral administration in rats. To facilitate compound identification and investigate the potential pharmacodynamic material basis, we further summarized the mass spectrometric fragmentation patterns and metabolic pathways of representative compounds across different structural classes. UPLC-Q-TOF-MS/MS was employed for qualitative analysis of both prototype components in vitro and metabolites in vivo, with compound identification performed using Masslynx 4.2 software based on retention time, accurate mass, and MS/MS data. Consequently, a total of 144 chemical constituents were identified in the JWQHG extract, while 62 prototype compounds and 38 metabolites were detected in rat plasma, urine, and feces post-administration. The chemical constituents are primarily classified into coumarins, flavonoids, chromones, triterpenoids, and organic acids. Notably, prototype compounds predominate in vivo, whereas the metabolites are mainly flavonoids and organic acids formed through hydroxylation, methylation, demethylation, glucuronidation, and related metabolic processes. This research provides relatively comprehensive chemical and metabolic characterization of JWQHG, which is expected to offer reference for subsequent elucidation of its pharmacodynamic material basis, refinement of quality control standards, and promotion of rational clinical application.
Plasma-based near-infrared spectroscopy combined with aquaphotomics for colorectal cancer screening.
Chen Z, Zhang W, Ni J … +2 more , Zhu J, Zheng J
J Pharm Biomed Anal · 2026 Jul · PMID 41747488 · Publisher ↗
Fast, noninvasive and cost-effective methods for screening colorectal cancer (CRC) before uncomfortable colonoscopy are highly desirable. This study aimed to explore the feasibility of using near-infrared spectroscopy (N...
Fast, noninvasive and cost-effective methods for screening colorectal cancer (CRC) before uncomfortable colonoscopy are highly desirable. This study aimed to explore the feasibility of using near-infrared spectroscopy (NIRS) combined with aquaphotomics for CRC screening. Forty-nine CRC patients and forty-seven healthy controls (HC) were enrolled, and their plasma samples were measured via NIRS. Aquaphotomics analysis, including principal component analysis, partial least squares discriminant analysis (PLS-DA), and difference spectra calculation, was performed to identify water matrix coordinates and form water absorption spectral patterns (WASPs) with aquagrams. The aquaphotomics results demonstrated that the PLS-DA diagnostic model with Savitzky-Golay second derivative preprocessing yielded a high predictive accuracy of 97 %, with sensitivity and specificity of 100 % and 94 % in the independent test set. The aquagrams displayed an evident shift in WASPs of CRC comparing to HC in both train and test sets. These findings reveal that combing NIRS with aquaphotomics is effective and visually interpretable, and the distinct differences between water of strong (1482 nm, 1486 nm) and weak (1429 nm, 1436 nm) hydrogen bonds in the WASPs may serve as a biomarker for CRC screening.
In-depth source characterization and analytical control strategy for the charge variants of antibody drug conjugates: Case study and discussion.
Xu G, Wei S, Wu G … +6 more , Du J, Yu X, Yang Y, Duan M, Cui C, Yu C
J Pharm Biomed Anal · 2026 Jul · PMID 41747487 · Publisher ↗
Antibody-drug conjugates (ADCs) combine the dual characteristics of antibody targeting and high payload potency. ADCs represent a key technology in targeted therapy and have become a major direction in "precision" medici...
Antibody-drug conjugates (ADCs) combine the dual characteristics of antibody targeting and high payload potency. ADCs represent a key technology in targeted therapy and have become a major direction in "precision" medicine. Charge variants are a major source of ADC variability with potential effects on efficacy and safety, which necessitates comprehensive characterization to guide analytical control strategies. We employed two orthogonal methods, ion exchange chromatography (IEX) fraction collection and imaged capillary isoelectric focusing-mass spectrometry (iCIEF-MS), to characterize ADC charge variants via "top-down" and "bottom-up" approaches. Beyond inherent the post-translational modifications and fragmentation profile of the monoclonal antibody, conjugation properties, drug-to-antibody ratio (DAR), DAR distribution, and position isomers, drove ADC charge variants. This is the first systematic study on the origins of ADC charge variants. The method of IEX fraction collection and iCIEF-MS were compared in terms of principle and experimental results. Challenges in interpreting the causes of charge variants and the possible reasons for incomplete interpretation of acidic peaks were discussed. Our study provides an insight into the source, in-depth characterization, and risk-based analytical control strategy of ADC charge variants.
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