Pub Date : 2025-12-15Epub Date: 2025-07-30DOI: 10.1016/j.jpba.2025.117086
Chee Leong Kee, Jing Quan Lim, Hui Ling Lim, Seo Hua Lau, Xiaowei Ge, Min Yong Low
A selective GC-Orbitrap method has been developed for analysing ethylene glycol (EG) and diethylene glycol (DEG) in four different categories of oral liquid products: Western medicines (WM), traditional medicines (TM), health supplements (HS) and Chinese proprietary medicines (CM). These glycols were chemically ionised to their respective deprotonated ions using methane gas in negative mode and analysed by targeted selected ion monitoring (t-SIM), maintaining a mass error window of ±5 ppm. Internal calibration was performed using matrix-assisted standard solutions ranging from 5 to 100 µg/mL, with 1,4-butanediol-2,2,3,3-D4 serving as the internal standard (IS). The limits of detection and quantification for both glycols (1.0 µg/mL; 3.0 µg/mL) are comparable with those achieved using gas chromatography tandem with triple quadrupole mass spectrometer (GC-MS/MS) at 0.4 µg/mL and 1.0 µg/mL, respectively. Results showed that most samples were free of EG and DEG. The trace levels of EG and/or DEG detected were below the safety limit of 0.1 % w/w. This methodology not only resolves the false positive identification issues previously encountered with gas chromatography-flame ionisation detection (GC-FID) but also demonstrates broader applicability across different sample matrices, such as oral gel, as evidenced in this study.
{"title":"Analysis of ethylene glycol (EG) and diethylene glycol (DEG) in oral liquid products using gas chromatography in tandem with Orbitrap spectrometer (GC-Orbitrap).","authors":"Chee Leong Kee, Jing Quan Lim, Hui Ling Lim, Seo Hua Lau, Xiaowei Ge, Min Yong Low","doi":"10.1016/j.jpba.2025.117086","DOIUrl":"10.1016/j.jpba.2025.117086","url":null,"abstract":"<p><p>A selective GC-Orbitrap method has been developed for analysing ethylene glycol (EG) and diethylene glycol (DEG) in four different categories of oral liquid products: Western medicines (WM), traditional medicines (TM), health supplements (HS) and Chinese proprietary medicines (CM). These glycols were chemically ionised to their respective deprotonated ions using methane gas in negative mode and analysed by targeted selected ion monitoring (t-SIM), maintaining a mass error window of ±5 ppm. Internal calibration was performed using matrix-assisted standard solutions ranging from 5 to 100 µg/mL, with 1,4-butanediol-2,2,3,3-D<sub>4</sub> serving as the internal standard (IS). The limits of detection and quantification for both glycols (1.0 µg/mL; 3.0 µg/mL) are comparable with those achieved using gas chromatography tandem with triple quadrupole mass spectrometer (GC-MS/MS) at 0.4 µg/mL and 1.0 µg/mL, respectively. Results showed that most samples were free of EG and DEG. The trace levels of EG and/or DEG detected were below the safety limit of 0.1 % w/w. This methodology not only resolves the false positive identification issues previously encountered with gas chromatography-flame ionisation detection (GC-FID) but also demonstrates broader applicability across different sample matrices, such as oral gel, as evidenced in this study.</p>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"266 ","pages":"117086"},"PeriodicalIF":3.1,"publicationDate":"2025-12-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144816970","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-12-14DOI: 10.1016/j.jpba.2025.117318
Rongfeng Kang , Xiaoping Bai , Delai Zhou , Cong Tang , Xin Wang , Jiayu Xi , Shijun Shao , Shuqing Dong , Fude Yang
Mercury sulfide (HgS) is one of the primary constituents of the Tibetan medicine “Zuo Tai,” and its content directly impacts the drug's efficacy and safety. Therefore, developing rapid, direct, and highly sensitive detection methods is of significant importance. In this study, a novel electrochemical sensor based on graphene/silver sulfide (G/Ag2S) nanocomposites was developed for the rapid detection of HgS in Tibetan medicine “Zuo Tai.” The G/Ag2S nanocomposite was prepared using the hydrothermal synthesis method. Cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) analysis indicated that the G/Ag2S nanocomposite enhanced the electrochemical signal response and improved the electrochemical activity of the glassy carbon electrode (GCE) after modification. Under optimized conditions, linear detection of HgS was achieved using differential pulse voltammetry (DPV). The DPV oxidation peak current decreased with increasing HgS concentration due to its adsorption onto the G/Ag2S-modified electrode, which altered the redox properties. The detection range of this analytical method was 0.1–10 mg/L, with a detection limit of 0.0194 mg/L. Further studies revealed that the modified electrode prepared in this paper exhibited excellent selectivity toward HgS. When detecting the HgS content in the “Zuo Tai” sample, the sensor demonstrated high sensitivity, with an average HgS content of 54.38 % in the sample and a relative standard deviation (RSD) of 1.07 %, consistent with the results reported in the literature. This analytical method provides a rapid and reliable quality control method for traditional medicines containing HgS.
{"title":"Electrochemical sensors based on graphene/silver sulfide nanocomposites for the indirect detection of mercury sulfide in the Tibetan medicine “Zuo Tai”","authors":"Rongfeng Kang , Xiaoping Bai , Delai Zhou , Cong Tang , Xin Wang , Jiayu Xi , Shijun Shao , Shuqing Dong , Fude Yang","doi":"10.1016/j.jpba.2025.117318","DOIUrl":"10.1016/j.jpba.2025.117318","url":null,"abstract":"<div><div>Mercury sulfide (HgS) is one of the primary constituents of the Tibetan medicine “Zuo Tai,” and its content directly impacts the drug's efficacy and safety. Therefore, developing rapid, direct, and highly sensitive detection methods is of significant importance. In this study, a novel electrochemical sensor based on graphene/silver sulfide (G/Ag<sub>2</sub>S) nanocomposites was developed for the rapid detection of HgS in Tibetan medicine “Zuo Tai.” The G/Ag<sub>2</sub>S nanocomposite was prepared using the hydrothermal synthesis method. Cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) analysis indicated that the G/Ag<sub>2</sub>S nanocomposite enhanced the electrochemical signal response and improved the electrochemical activity of the glassy carbon electrode (GCE) after modification. Under optimized conditions, linear detection of HgS was achieved using differential pulse voltammetry (DPV). The DPV oxidation peak current decreased with increasing HgS concentration due to its adsorption onto the G/Ag<sub>2</sub>S-modified electrode, which altered the redox properties. The detection range of this analytical method was 0.1–10 mg/L, with a detection limit of 0.0194 mg/L. Further studies revealed that the modified electrode prepared in this paper exhibited excellent selectivity toward HgS. When detecting the HgS content in the “Zuo Tai” sample, the sensor demonstrated high sensitivity, with an average HgS content of 54.38 % in the sample and a relative standard deviation (RSD) of 1.07 %, consistent with the results reported in the literature. This analytical method provides a rapid and reliable quality control method for traditional medicines containing HgS.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"271 ","pages":"Article 117318"},"PeriodicalIF":3.1,"publicationDate":"2025-12-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145760866","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Although electronic cigarettes (e-cigarettes) that enable inhalation of caffeine (Caf) are commercially available, the pharmacokinetic (PK) properties of Caf intake via e-cigarette smoking are unclear. The present study used a validated LC-MS/MS method to compare the PK parameters of Caf and its metabolites (Cafs) in rat plasma after oral (p.o.) administration of Caf and exposure to e-cigarette smoke. The LC-MS/MS method was validated for Caf and metabolites such as paraxanthine (PX), theophylline (TP), theobromine, 1,3,7-trimethyluric acid, 3-methylxanthine, 1,3-dimethyluric acid, and 1,7-dimethyluric acid. Quantitation of Cafs in deproteinated rat plasma was achieved. Rats were exposed to e-cigarette smoke for 1 and 3 min, and then plasma was collected until 90 min. Although the Caf exposure dose for rats was estimated as very low, quantitation of Caf, PX, and TP was possible using the proposed LC-MS/MS method. The maximum concentrations of Caf after 1 and 3 min of exposure to e-cigarette smoke were similar to those observed after p.o. administration of 40 and 90 μg/kg, respectively. Furthermore, PK parameters such as the concentration peak time (3.0 min for 1- and 3-min exposure) and absorption rate constant (0.62 for 1 min and 0.91 min−1 for 3 min) for e-cigarette smoke exposure differed significantly from p.o. administration (50.0 min and 36.7 min, and 0.045 and 0.070 min−1) (P < 0.05). By contrast, no difference was observed between PX and TP. This is the first report demonstrating the rapid appearance of Caf in rat plasma after exposure to e-cigarette smoke.
{"title":"Rapid appearance of caffeine in plasma of rats exposed to e-cigarette smoke, analyzed using a validated LC-MS/MS method","authors":"Keisuke Muranaka , Junpei Mutoh , Makoto Takada , Yutaro Yanagita , Kanta Noguchi , Ken Tachibana , Naoya Kishikawa , Naotaka Kuroda , Mitsuhiro Wada","doi":"10.1016/j.jpba.2025.117317","DOIUrl":"10.1016/j.jpba.2025.117317","url":null,"abstract":"<div><div>Although electronic cigarettes (e-cigarettes) that enable inhalation of caffeine (Caf) are commercially available, the pharmacokinetic (PK) properties of Caf intake via e-cigarette smoking are unclear. The present study used a validated LC-MS/MS method to compare the PK parameters of Caf and its metabolites (Cafs) in rat plasma after oral (<em>p.o.</em>) administration of Caf and exposure to e-cigarette smoke. The LC-MS/MS method was validated for Caf and metabolites such as paraxanthine (PX), theophylline (TP), theobromine, 1,3,7-trimethyluric acid, 3-methylxanthine, 1,3-dimethyluric acid, and 1,7-dimethyluric acid. Quantitation of Cafs in deproteinated rat plasma was achieved. Rats were exposed to e-cigarette smoke for 1 and 3 min, and then plasma was collected until 90 min. Although the Caf exposure dose for rats was estimated as very low, quantitation of Caf, PX, and TP was possible using the proposed LC-MS/MS method. The maximum concentrations of Caf after 1 and 3 min of exposure to e-cigarette smoke were similar to those observed after <em>p.o</em>. administration of 40 and 90 μg/kg, respectively. Furthermore, PK parameters such as the concentration peak time (3.0 min for 1- and 3-min exposure) and absorption rate constant (0.62 for 1 min and 0.91 min<sup>−1</sup> for 3 min) for e-cigarette smoke exposure differed significantly from p.o. administration (50.0 min and 36.7 min, and 0.045 and 0.070 min<sup>−1</sup>) (<em>P</em> < 0.05). By contrast, no difference was observed between PX and TP. This is the first report demonstrating the rapid appearance of Caf in rat plasma after exposure to e-cigarette smoke.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"271 ","pages":"Article 117317"},"PeriodicalIF":3.1,"publicationDate":"2025-12-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145781430","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-12-12DOI: 10.1016/j.jpba.2025.117307
Jiawei Feng , Guirong Bu , Xigui Song , Peiyu Wu , Zhiyuan Yan , Shenfei Chen , Qi Yao
Identification of the authenticity of herbal medicines is crucial to ensure their safety and efficacy, yet quantitative, accurate, and practical identification methods remain limited. This work introduces a fluorescence-based approach for distinguishing authentic and counterfeit herbal medicines by analyzing their spectral and chromaticity features under 365 nm UV excitation. A hyperspectral imaging camera was employed to collect the spectral data from three groups of herbal medicines, Ziziphi Spinosae Semen (ZSS), Aurantii Fructus (AF), Carthami Flos (CF) and their common counterfeits (a total of 326 pieces of spectral data in the three groups, 158, 80, 88 respectively). The critical difference between ZSS, AF, CF and their counterfeits was obtained by extracting the fluorescence spectrum features. The mapping relationships between the spectrum features of ZSS and the colorimetric features were established by using the Fast Formula Fitting (FFF) and Neural Network Fitting (NNF) methods. The correlation coefficients of the two fitting methods in three groups were 0.985, 0.995, 0.999 and 0.992, 0.998, 0.989 respectively. The spectral power distribution in the range of 400–780 nm (good for AF, CF and their counterfeits) and 470–780 nm (good for ZSS and its counterfeits) were identified as optimal for color-based discrimination, guiding future filter selection for portable devices. Both methods enabled pixel-level authentication with high precision, supported by a defined chromaticity visualization zone. This non-destructive, quantitative technique facilitates simple and accurate herbal medicine verification, paving the way for low-cost, portable authenticity detection systems.
{"title":"Fluorescence spectral-chromaticity mapping for non-destructive authentication of herbal medicines","authors":"Jiawei Feng , Guirong Bu , Xigui Song , Peiyu Wu , Zhiyuan Yan , Shenfei Chen , Qi Yao","doi":"10.1016/j.jpba.2025.117307","DOIUrl":"10.1016/j.jpba.2025.117307","url":null,"abstract":"<div><div>Identification of the authenticity of herbal medicines is crucial to ensure their safety and efficacy, yet quantitative, accurate, and practical identification methods remain limited. This work introduces a fluorescence-based approach for distinguishing authentic and counterfeit herbal medicines by analyzing their spectral and chromaticity features under 365 nm UV excitation. A hyperspectral imaging camera was employed to collect the spectral data from three groups of herbal medicines, Ziziphi Spinosae Semen (ZSS), Aurantii Fructus (AF), Carthami Flos (CF) and their common counterfeits (a total of 326 pieces of spectral data in the three groups, 158, 80, 88 respectively). The critical difference between ZSS, AF, CF and their counterfeits was obtained by extracting the fluorescence spectrum features. The mapping relationships between the spectrum features of ZSS and the colorimetric features were established by using the Fast Formula Fitting (FFF) and Neural Network Fitting (NNF) methods. The correlation coefficients of the two fitting methods in three groups were 0.985, 0.995, 0.999 and 0.992, 0.998, 0.989 respectively. The spectral power distribution in the range of 400–780 nm (good for AF, CF and their counterfeits) and 470–780 nm (good for ZSS and its counterfeits) were identified as optimal for color-based discrimination, guiding future filter selection for portable devices. Both methods enabled pixel-level authentication with high precision, supported by a defined chromaticity visualization zone. This non-destructive, quantitative technique facilitates simple and accurate herbal medicine verification, paving the way for low-cost, portable authenticity detection systems.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"271 ","pages":"Article 117307"},"PeriodicalIF":3.1,"publicationDate":"2025-12-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145760867","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-12-12DOI: 10.1016/j.jpba.2025.117314
Laerissa Reveil , Maria Lasaosa , Amanda Furman , A.M. Iqbal O’Meara , Matthew S. Halquist
{"title":"Corrigendum to “Validation and quantitation of six neurotransmitters in rat plasma and brain using liquid chromatography quadrupole-time-of-flight mass spectrometry” [J. Pharm. Biomed. Anal., 267 (2026) 117145]","authors":"Laerissa Reveil , Maria Lasaosa , Amanda Furman , A.M. Iqbal O’Meara , Matthew S. Halquist","doi":"10.1016/j.jpba.2025.117314","DOIUrl":"10.1016/j.jpba.2025.117314","url":null,"abstract":"","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"270 ","pages":"Article 117314"},"PeriodicalIF":3.1,"publicationDate":"2025-12-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145733399","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-12-11DOI: 10.1016/j.jpba.2025.117316
Berfu Bekmez , Fatma Budak , Ahmet Cetinkaya , Sibel A. Ozkan
Cardiovascular disease, one of the leading causes of death in developing countries, is mainly caused by the combination of arterial hypertension and dyslipidemia as major risk factors. Amlodipine (AML) is a calcium channel blocker that inhibits extracellular calcium influx across the membranes of myocardial and vascular smooth muscle cells, thereby reducing contraction and dilating coronary and systemic arteries. This study aimed to design a nanoparticle-supported molecularly imprinted polymer (MIP)-based electrochemical sensor with selective and sensitive sensitivity for the quantitative analysis of both binary drug mixtures and AML. The modified sensor was produced by the electropolymerization (EP) method in the presence of 4-aminobenzoic acid (4-ABA) as the functional monomer, pyrrole (Py) as the copolymerization monomer, and the target molecule AML. The incorporation of silver nanoparticles (AgNPs) into the MIP-based electrochemical sensor increased its active surface area and porosity. The AML/4-ABA-co-Py@AgNPs/MIP-GCE sensor was characterized both electrochemically (electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV)) and by surface morphology (scanning electron microscopy (SEM)). The quantification of AML was performed using differential pulse voltammetry (DPV) with the direct method in a 5.0 mM [Fe(CN)6]3-/4 solution, yielding a linear range of 0.1–1.0 pM. The applicability and accuracy of the sensor were evaluated by recovery studies in tablet forms containing binary mixtures. In addition, to demonstrate the sensor's selectivity, a selectivity study was performed in the presence of components with chemical structures similar to those of AML, and its high selectivity was confirmed by the relative suppression factors for AML. In conclusion, this newly developed sensor for AML offers many advantages, such as selective, sensitive, fast, and inexpensive analysis.
心血管疾病是发展中国家的主要死亡原因之一，主要由动脉高血压和血脂异常共同引起，是主要危险因素。氨氯地平（AML）是一种钙通道阻滞剂，可抑制细胞外钙通过心肌和血管平滑肌细胞膜流入，从而减少冠状动脉和全身动脉的收缩和扩张。本研究旨在设计一种基于纳米颗粒支撑的分子印迹聚合物（MIP）的电化学传感器，该传感器具有选择性和敏感性，可用于二元药物混合物和AML的定量分析。以4-氨基苯甲酸（4-ABA）为功能单体，吡咯（Py）为共聚单体，目标分子AML为目标分子，采用电聚合（EP）法制备了改性传感器。将银纳米颗粒（AgNPs）加入到基于mip的电化学传感器中，增加了其活性表面积和孔隙率。对AML/4-ABA-co-Py@AgNPs/MIP-GCE传感器进行了电化学（电化学阻抗谱（EIS）和循环伏安法（CV））和表面形貌（扫描电镜（SEM））表征。AML的定量采用差分脉冲伏安法（DPV），在5.0 mM [Fe(CN)6]3-/4溶液中直接测定，线性范围为0.1-1.0 pM。通过对含二元混合物片剂的回收率研究，评价了该传感器的适用性和准确性。此外，为了证明该传感器的选择性，在与AML化学结构相似的成分存在下进行了选择性研究，并通过AML的相对抑制因子证实了其高选择性。总之，这种新开发的AML传感器具有选择性、敏感性、快速和廉价等优点。
{"title":"Selective and sensitive determination of amlodipine in binary mixtures using a nanomaterial-assisted molecularly imprinted electrochemical sensor","authors":"Berfu Bekmez , Fatma Budak , Ahmet Cetinkaya , Sibel A. Ozkan","doi":"10.1016/j.jpba.2025.117316","DOIUrl":"10.1016/j.jpba.2025.117316","url":null,"abstract":"<div><div>Cardiovascular disease, one of the leading causes of death in developing countries, is mainly caused by the combination of arterial hypertension and dyslipidemia as major risk factors. Amlodipine (AML) is a calcium channel blocker that inhibits extracellular calcium influx across the membranes of myocardial and vascular smooth muscle cells, thereby reducing contraction and dilating coronary and systemic arteries. This study aimed to design a nanoparticle-supported molecularly imprinted polymer (MIP)-based electrochemical sensor with selective and sensitive sensitivity for the quantitative analysis of both binary drug mixtures and AML. The modified sensor was produced by the electropolymerization (EP) method in the presence of 4-aminobenzoic acid (4-ABA) as the functional monomer, pyrrole (Py) as the copolymerization monomer, and the target molecule AML. The incorporation of silver nanoparticles (AgNPs) into the MIP-based electrochemical sensor increased its active surface area and porosity. The AML/4-ABA-co-Py@AgNPs/MIP-GCE sensor was characterized both electrochemically (electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV)) and by surface morphology (scanning electron microscopy (SEM)). The quantification of AML was performed using differential pulse voltammetry (DPV) with the direct method in a 5.0 mM [Fe(CN)<sub>6</sub>]<sup>3-/4</sup> solution, yielding a linear range of 0.1–1.0 pM. The applicability and accuracy of the sensor were evaluated by recovery studies in tablet forms containing binary mixtures. In addition, to demonstrate the sensor's selectivity, a selectivity study was performed in the presence of components with chemical structures similar to those of AML, and its high selectivity was confirmed by the relative suppression factors for AML. In conclusion, this newly developed sensor for AML offers many advantages, such as selective, sensitive, fast, and inexpensive analysis.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"270 ","pages":"Article 117316"},"PeriodicalIF":3.1,"publicationDate":"2025-12-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145733477","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-12-09DOI: 10.1016/j.jpba.2025.117315
Hou-Xu Ma , Na-Wei Qi , Xiao-Lin Yang , Fei Li
Bufei Formula (BF), consisting of nine traditional Chinese medicinal herbs, is clinically applied to tonify qi, nourish the lung, relieve cough, and alleviate asthma. However, the chemical complexity of BF has hindered a clear understanding of its pharmacodynamic material basis and underlying in vivo mechanisms. This study aims to systematically elucidate the pharmacokinetics, tissue distribution, and metabolic profiles of BF in rats, thereby laying the groundwork for understanding its pharmacodynamic material basis. First, ultra-performance liquid chromatography (UPLC) was used to identify 18 major active constituents of BF. Subsequently, ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was employed to identify prototype compounds and metabolites in rat plasma, urine, feces, and tissues following oral administration of BF. In addition, a validated UPLC-MS/MS method was established for quantifying 14 active constituents. In total, 63 constituents were identified in vivo, including 17 prototype compounds and 46 metabolites. Among them, eight compounds showed the mean time to maximum plasma concentration (Tmax) of 0.112–0.987 h, maximum plasma concentrations (Cmax) of 4.995–213.333 μg/L, and the area under the plasma concentration–time curve (AUC) of 7.557–692.082 μg·h/L. Tissue distribution analysis revealed that the 14 quantified compounds were widely distributed in multiple organs, with predominant accumulation in the lung and colon, suggesting them as potential target organs. These findings provide a valuable reference for the clinical application of BF and evidence for elucidating its pharmacodynamic material basis.
{"title":"Comprehensive characterization of the pharmacokinetics, tissue distribution, and metabolism of Bufei Formula in rats","authors":"Hou-Xu Ma , Na-Wei Qi , Xiao-Lin Yang , Fei Li","doi":"10.1016/j.jpba.2025.117315","DOIUrl":"10.1016/j.jpba.2025.117315","url":null,"abstract":"<div><div>Bufei Formula (BF), consisting of nine traditional Chinese medicinal herbs, is clinically applied to tonify qi, nourish the lung, relieve cough, and alleviate asthma. However, the chemical complexity of BF has hindered a clear understanding of its pharmacodynamic material basis and underlying <em>in vivo</em> mechanisms. This study aims to systematically elucidate the pharmacokinetics, tissue distribution, and metabolic profiles of BF in rats, thereby laying the groundwork for understanding its pharmacodynamic material basis. First, ultra-performance liquid chromatography (UPLC) was used to identify 18 major active constituents of BF. Subsequently, ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was employed to identify prototype compounds and metabolites in rat plasma, urine, feces, and tissues following oral administration of BF. In addition, a validated UPLC-MS/MS method was established for quantifying 14 active constituents. In total, 63 constituents were identified <em>in vivo</em>, including 17 prototype compounds and 46 metabolites. Among them, eight compounds showed the mean time to maximum plasma concentration (T<sub>max</sub>) of 0.112–0.987 h, maximum plasma concentrations (C<sub>max</sub>) of 4.995–213.333 μg/L, and the area under the plasma concentration–time curve (AUC) of 7.557–692.082 μg·h/L. Tissue distribution analysis revealed that the 14 quantified compounds were widely distributed in multiple organs, with predominant accumulation in the lung and colon, suggesting them as potential target organs. These findings provide a valuable reference for the clinical application of BF and evidence for elucidating its pharmacodynamic material basis.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"270 ","pages":"Article 117315"},"PeriodicalIF":3.1,"publicationDate":"2025-12-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145733397","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-12-08DOI: 10.1016/j.jpba.2025.117311
Carlos Pernas-Fraguela , Rosario Rodil , José Benito Quintana , Antonio Saez , Ruth Olmos , Joan Mestre , Manuel Isorna , Rosa Montes
Chemsex is a practice mostly extended between men who have sex with men under drugs effects to enhance and/or prolong sexual activities. Within chemsex, slamming consists of intravenous consumption of substances such as cathinones and amphetamines. Syringe residue analysis is a relatively new alternative for knowing with accuracy the substances consumed by the users. Although several studies have been carried out applying the technique, none of them was focused on this population group. In this work, syringes were obtained from a drug addiction assistance centre from Madrid (Spain). Samples were processed by rinsing with methanol and injected in a liquid chromatography coupled to high resolution mass spectrometry system. Data (acquired in data dependent mode) were processed using a suspect screening approach. In total, 122 syringes from three sampling campaigns were analyzed. The compounds belonging to the cathinones’ group were the most frequently detected (99 %), followed by amphetamines and cocaine. The most consumed cathinone was chloromethcathinone, but also others as methylmethcathinone, pentedrone or N,N-dimethylpentylone were identified. Furthermore, temporal trends were detected during the different sampling campaigns. Thus, this technique allowed us to determine in an accurate way the substances consumed during slamming sessions, which may differ from the self-declared ones in surveys. Moreover, temporal trends were observed, that align with the market changes and regulation of cathinones.
{"title":"The role of syringe residue analysis in identifying substances consumed in sexualized drug use practices","authors":"Carlos Pernas-Fraguela , Rosario Rodil , José Benito Quintana , Antonio Saez , Ruth Olmos , Joan Mestre , Manuel Isorna , Rosa Montes","doi":"10.1016/j.jpba.2025.117311","DOIUrl":"10.1016/j.jpba.2025.117311","url":null,"abstract":"<div><div><em>Chemsex</em> is a practice mostly extended between men who have sex with men under drugs effects to enhance and/or prolong sexual activities. Within <em>chemsex</em>, <em>slamming</em> consists of intravenous consumption of substances such as cathinones and amphetamines. Syringe residue analysis is a relatively new alternative for knowing with accuracy the substances consumed by the users. Although several studies have been carried out applying the technique, none of them was focused on this population group. In this work, syringes were obtained from a drug addiction assistance centre from Madrid (Spain). Samples were processed by rinsing with methanol and injected in a liquid chromatography coupled to high resolution mass spectrometry system. Data (acquired in data dependent mode) were processed using a suspect screening approach. In total, 122 syringes from three sampling campaigns were analyzed. The compounds belonging to the cathinones’ group were the most frequently detected (99 %), followed by amphetamines and cocaine. The most consumed cathinone was chloromethcathinone, but also others as methylmethcathinone, pentedrone or N,N-dimethylpentylone were identified. Furthermore, temporal trends were detected during the different sampling campaigns. Thus, this technique allowed us to determine in an accurate way the substances consumed during <em>slamming</em> sessions, which may differ from the self-declared ones in surveys. Moreover, temporal trends were observed, that align with the market changes and regulation of cathinones.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"270 ","pages":"Article 117311"},"PeriodicalIF":3.1,"publicationDate":"2025-12-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145733401","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-12-08DOI: 10.1016/j.jpba.2025.117308
Xiang Li , Ting Yang , Fan Zhang , Guoxiang Sun , Mingxiao Hou , Yunen Liu
Kangfuxin Liquid (KFX), a complex zoogenic medicine, faces challenges in quality control due to its multi-component nature and batch-to-batch variability. This study presents a novel integrated quality assessment strategy combining Four-wavelength maximization profiling (Four-WMP) HPLC with electrochemical fingerprinting (ECFP) for comprehensive evaluation of KFX. The Four-WMP method integrated chromatographic data from four wavelengths (236, 254, 265, and 280 nm) into a unified fingerprint, significantly enhancing chemical comprehensiveness compared to conventional single-wavelength approaches. Concurrently, ECFP provided unique insights into redox-active properties. Strong correlations were established between chemical fingerprints and antioxidant efficacy through Partial Least Squares (PLS) modeling (R2=0.8672, Q2=0.789), identifying critical quality markers including protocatechuic acid and adenosine. Substantial inter-manufacturer variation was observed, particularly in sodium benzoate content, highlighting significant quality inconsistencies. This multi-parametric framework provides a holistic and robust paradigm for quality control of KFX and similar complex medicines, effectively bridging chemical composition with bioactive relevance.
{"title":"Integrating multi–wavelength HPLC fingerprinting and electrochemical profiling with chemometrics for comprehensive quality assessment of Kangfuxin Liquid","authors":"Xiang Li , Ting Yang , Fan Zhang , Guoxiang Sun , Mingxiao Hou , Yunen Liu","doi":"10.1016/j.jpba.2025.117308","DOIUrl":"10.1016/j.jpba.2025.117308","url":null,"abstract":"<div><div>Kangfuxin Liquid (KFX), a complex zoogenic medicine, faces challenges in quality control due to its multi-component nature and batch-to-batch variability. This study presents a novel integrated quality assessment strategy combining Four-wavelength maximization profiling (Four-WMP) HPLC with electrochemical fingerprinting (ECFP) for comprehensive evaluation of KFX. The Four-WMP method integrated chromatographic data from four wavelengths (236, 254, 265, and 280 nm) into a unified fingerprint, significantly enhancing chemical comprehensiveness compared to conventional single-wavelength approaches. Concurrently, ECFP provided unique insights into redox-active properties. Strong correlations were established between chemical fingerprints and antioxidant efficacy through Partial Least Squares (PLS) modeling (R<sup>2</sup>=0.8672, Q<sup>2</sup>=0.789), identifying critical quality markers including protocatechuic acid and adenosine. Substantial inter-manufacturer variation was observed, particularly in sodium benzoate content, highlighting significant quality inconsistencies. This multi-parametric framework provides a holistic and robust paradigm for quality control of KFX and similar complex medicines, effectively bridging chemical composition with bioactive relevance.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"270 ","pages":"Article 117308"},"PeriodicalIF":3.1,"publicationDate":"2025-12-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145733479","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-12-08DOI: 10.1016/j.jpba.2025.117313
Lingyu Shen , Wenxing Li , Yupeng Chen , Daogang Guan , Aiping Lu , Anqi Xu
SuHeXiang Wan (SHXW) is a renowned traditional Chinese medicine (TCM) prescription for treating stroke, but its active components remain largely unidentified. This study aimed to screen potential active compounds of SHXW and reveal their underlying mechanisms in stroke treatment. Ingredients and compounds in SHXW were obtained from TCM databases and subjected to initial screening based on ADMET and physicochemical properties, followed by target gene prediction for each filtered compound. A comprehensive network of filtered compound–target gene–stroke pathogenic gene was constructed and optimized using a multi-objective optimization algorithm. Seventeen potential active compounds were identified, which primarily influenced neuroactive ligand-receptor interactions, arachidonic acid metabolism, and several signaling pathways including PI3K-Akt, calcium, and cAMP. Using an oxygen-glucose deprivation and reoxygenation (OGD/R) model, cirsiliol was identified as the lead compound, significantly enhancing cell viability and morphology, decreasing apoptosis, and reducing oxidative stress and inflammatory responses. Molecular docking and dynamics simulations revealed that cirsiliol stably binds to the NADPH binding pocket of CBR1 protein. Further experiments demonstrated that cirsiliol decreased 4-hydroxynonenal (4-HNE, a substrate of CBR1) levels. This study provides a methodological framework for screening active compounds in TCM prescriptions. The neuroprotective effects of cirsiliol against ischemic stroke merit further investigation.
{"title":"SuHeXiang Wan in the treatment of stroke: Prediction potentially active metabolites using a combination of in silico analysis and experimental viability assessment","authors":"Lingyu Shen , Wenxing Li , Yupeng Chen , Daogang Guan , Aiping Lu , Anqi Xu","doi":"10.1016/j.jpba.2025.117313","DOIUrl":"10.1016/j.jpba.2025.117313","url":null,"abstract":"<div><div>SuHeXiang Wan (SHXW) is a renowned traditional Chinese medicine (TCM) prescription for treating stroke, but its active components remain largely unidentified. This study aimed to screen potential active compounds of SHXW and reveal their underlying mechanisms in stroke treatment. Ingredients and compounds in SHXW were obtained from TCM databases and subjected to initial screening based on ADMET and physicochemical properties, followed by target gene prediction for each filtered compound. A comprehensive network of filtered compound–target gene–stroke pathogenic gene was constructed and optimized using a multi-objective optimization algorithm. Seventeen potential active compounds were identified, which primarily influenced neuroactive ligand-receptor interactions, arachidonic acid metabolism, and several signaling pathways including PI3K-Akt, calcium, and cAMP. Using an oxygen-glucose deprivation and reoxygenation (OGD/R) model, cirsiliol was identified as the lead compound, significantly enhancing cell viability and morphology, decreasing apoptosis, and reducing oxidative stress and inflammatory responses. Molecular docking and dynamics simulations revealed that cirsiliol stably binds to the NADPH binding pocket of CBR1 protein. Further experiments demonstrated that cirsiliol decreased 4-hydroxynonenal (4-HNE, a substrate of CBR1) levels. This study provides a methodological framework for screening active compounds in TCM prescriptions. The neuroprotective effects of cirsiliol against ischemic stroke merit further investigation.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"270 ","pages":"Article 117313"},"PeriodicalIF":3.1,"publicationDate":"2025-12-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145733402","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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