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Simultaneous determination of thirteen related substances in lenalidomide API by a stability-indicating RP-HPLC method
IF 3.1 3区 医学
Journal of pharmaceutical and biomedical analysis Pub Date : 2025-03-17 DOI: 10.1016/j.jpba.2025.116823
Zhiling Cao, Maolong Huang, Luye Bi, Ling Zhang, Siyi Xia, Yuhan Sun, Yang Yu, Xudong Yu, Dahua Sh, Fan Xu
{"title":"Simultaneous determination of thirteen related substances in lenalidomide API by a stability-indicating RP-HPLC method","authors":"Zhiling Cao,&nbsp;Maolong Huang,&nbsp;Luye Bi,&nbsp;Ling Zhang,&nbsp;Siyi Xia,&nbsp;Yuhan Sun,&nbsp;Yang Yu,&nbsp;Xudong Yu,&nbsp;Dahua Sh,&nbsp;Fan Xu","doi":"10.1016/j.jpba.2025.116823","DOIUrl":"10.1016/j.jpba.2025.116823","url":null,"abstract":"<div><div>The purpose of this study was to develop and validate a high performance liquid chromatography (HPLC) method for the separation and determination of related impurities and potential genotoxic impurity in the lenalidomide API. Chromatographic separation was performed on a Zorbax SB-AQ column (250 mm × 4.6 mm, 5 μm) at a wavelength of 220 nm using pH 4.0 phosphate buffer-acetonitrile as the mobile phase in gradient elution mode. The validation results demonstrate that the method has acceptable specificity, linearity, accuracy, precision and robustness. The detection limits and quantitation limits ranged from 2 to 17 ng/mL and from 6 to 50 ng/mL, respectively. A linear relationship was observed between the peak area and concentration of lenalidomide and impurities, with a correlation coefficient value of <em>r</em> ≥ 0.999. The formation and chemical structures of oxidation and base degradation products of lenalidomide have also been confirmed. The newly developed HPLC method is suitable for use in quality-control laboratories for qualitative and quantitative assessment of thirteen kinds of related substances in the lenalidomide API.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"260 ","pages":"Article 116823"},"PeriodicalIF":3.1,"publicationDate":"2025-03-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143687078","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}
引用次数: 0
In vitro metabolism and metabolite identification of eutylone using rat liver microsomes 利用大鼠肝脏微粒体对丁酮进行体外代谢和代谢物鉴定
IF 3.1 3区 医学
Journal of pharmaceutical and biomedical analysis Pub Date : 2025-03-17 DOI: 10.1016/j.jpba.2025.116827
Alexandre Barcia Godoi , Natalícia de Jesus Antunes , Leonardo Costalonga Rodrigues , Aline Franco Martins , José Luiz Costa
{"title":"In vitro metabolism and metabolite identification of eutylone using rat liver microsomes","authors":"Alexandre Barcia Godoi ,&nbsp;Natalícia de Jesus Antunes ,&nbsp;Leonardo Costalonga Rodrigues ,&nbsp;Aline Franco Martins ,&nbsp;José Luiz Costa","doi":"10.1016/j.jpba.2025.116827","DOIUrl":"10.1016/j.jpba.2025.116827","url":null,"abstract":"<div><div>The determination of toxicokinetic parameters allows the characterization of the toxicological profile of a wide range of substances. Several models have been employed to <em>in vitro</em> kinetic evaluations, in which liver microsomes stands out due to its simple handling and obtaining. Eutylone is a New Psychoactive Substance (NPS) classified as a synthetic cathinone with stimulant effects on central nervous system. This substance was initially synthesized for pharmaceutical applications but ultimately became subject to recreational use, with constant seizures worldwide. Herein, the <em>in vitro</em> metabolism and the production of eutylone phase I and phase II metabolites was investigated using rat liver microsomes (RLM). Eutylone presented a low metabolic stability showing an <em>in vitro</em> elimination half-life (t<sub>1/2</sub>) of 2.27 min. The unbound fractions of eutylone in microsomal (f<sub>u-mic</sub>) and plasma (f<sub>u-p</sub>) proteins were 0.93 and 0.15, respectively. A sigmoidal profile defined by Hill equation were observed, allowing kinetic parameters calculations. The Hill coefficient (H) was 1.21, <em>in vitro</em> maximum velocity (V<sub>max</sub>) was 19.40 μmol/mg/min, substrate concentration at half V<sub>max</sub> (S<sub>50</sub>) was 4.78 μM, intrinsic maximum clearance (CL<sub>max, in vitro</sub>) was 3.36 mL/min/mg, <em>in vivo</em> intrinsic clear-ance (CL<sub>int, in vivo</sub>) was 8.20 mL/min/kg, hepatic clearance (CL<sub>H</sub>) was 1.29 mL/min/kg, and hepatic extraction rate (E<sub>H</sub>) was 0.02. Eight eutylone metabolites were identified, four produced by phase I reactions and four by phase I followed by phase II reactions. Demethylenation and O-glucuronidation were pivotal in eutylone’s metabolism. These findings provide valuable information about the metabolism of eutylone, allowing practical implications for evaluating its safety and toxicity.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"260 ","pages":"Article 116827"},"PeriodicalIF":3.1,"publicationDate":"2025-03-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143687065","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}
引用次数: 0
Transitioning from concept to application: Comprehensive analytical validation of antibody-based smart sampling 从概念到应用的过渡:基于抗体的智能采样的全面分析验证
IF 3.1 3区 医学
Journal of pharmaceutical and biomedical analysis Pub Date : 2025-03-17 DOI: 10.1016/j.jpba.2025.116825
Ago Mrsa , Ridja Ishaq, Laila Brandoli, Trine Grønhaug Halvorsen , Léon Reubsaet
{"title":"Transitioning from concept to application: Comprehensive analytical validation of antibody-based smart sampling","authors":"Ago Mrsa ,&nbsp;Ridja Ishaq,&nbsp;Laila Brandoli,&nbsp;Trine Grønhaug Halvorsen ,&nbsp;Léon Reubsaet","doi":"10.1016/j.jpba.2025.116825","DOIUrl":"10.1016/j.jpba.2025.116825","url":null,"abstract":"<div><div>Smart sampling, introduced in 2018, is a technique that integrates crucial sample preparation steps for LC-MS protein analysis directly into the sampling process, improving efficiency. Currently most studies in this area are limited to proof of concept with a brief evaluation. Therefore, our objective is to fully validate the utility of smart samplers for quantitative analysis of bioactive proteins in biological matrices. This study builds on previous work where a paper-based antibody sampler was developed, and human chorionic gonadotropin (hCG) was used as a model protein. hCG is both a biomarker, a drug, and on the doping list for male athletes. Initially, the fabrication of the sampler was optimized, resulting in a reduction of antibody amount per sampler from 50 µg to 5 µg, reducing manufacturing cost while maintaining acceptable performance. It was also shown that removing the sampler before trypsination, but after reduction and alkylation greatly improved signal output while reducing the peptide background, suggesting a cleanser extract was achieved. The optimized smart sampler was validated for hCG in human serum using EMA’s ICH M10 guidelines on bioanalytical methods as a guide. Three calibration curves (seven levels) were made in the concentration range of 0.5 ng/mL to 75 ng/mL all displaying excellent linearity (r<sup>2</sup> ≥ 0.9955). The accuracy and precision both for the between-run (precision ≤ 10 % CV and accuracy 91–105 % (n = 3)) and within-run (precision ≤ 14 % CV and accuracy 94–105 % (n = 5)) runs were all well within the guideline's acceptance limits. The samplers also showed to be stable for at least ten weeks at room temperature. The optimization and validation of the antibody sampler detailed in this paper marks a notable progression, advancing the concept of \"smart sampling\" a step closer from the lab to practical application.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"260 ","pages":"Article 116825"},"PeriodicalIF":3.1,"publicationDate":"2025-03-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143687066","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Rapid quality evaluation of moutan cortex (Paeonia suffruticosa Andrews) by near-infrared spectroscopy and bionic swarm intelligent optimization algorithm
IF 3.1 3区 医学
Journal of pharmaceutical and biomedical analysis Pub Date : 2025-03-15 DOI: 10.1016/j.jpba.2025.116822
Ying Qiao , Yatong Kang , Tingze Long , Han Yi , Feng Wang , Chao Chen
{"title":"Rapid quality evaluation of moutan cortex (Paeonia suffruticosa Andrews) by near-infrared spectroscopy and bionic swarm intelligent optimization algorithm","authors":"Ying Qiao ,&nbsp;Yatong Kang ,&nbsp;Tingze Long ,&nbsp;Han Yi ,&nbsp;Feng Wang ,&nbsp;Chao Chen","doi":"10.1016/j.jpba.2025.116822","DOIUrl":"10.1016/j.jpba.2025.116822","url":null,"abstract":"<div><div>Moutan Cortex (MC), recognized as a traditional Chinese medicinal herb, possesses significant therapeutic properties. The existing quality assessment method only measures the content of one component in MC, which is obviously not comprehensive enough. Besides, the determination process is time-consuming and laborious.Thus, this article presents a novel approach for the rapid, precise, and efficient quality assessment of MC based on near-infrared spectroscopy (NIR) technology in combination with the bionic swarm intelligent optimization algorithms. First, MC samples were collected and acquired with the NIR spectra in diffuse reflectance mode. Second, the content of paeonol, paeoniflorin, and gallic acid in MC was determined by high-performance liquid chromatography, and the content of total flavonoids and phenols was determined by UV–visible spectrophotometry. Afterward, all the measured content was analyzed in correlation with the NIR spectra of MC, and the partial least squares regression method was utilized to build the models. Especially, to improve the models’ performance, five famous bionic swarm intelligent optimization algorithms were investigated to perform the wavelength selection. As a result, the models’ performance was significantly enhanced. The coefficient of determination (<em>R</em><sup><em>2</em></sup>) &gt; 0.9 and residual prediction deviation (<em>RPD</em>) &gt; 3 were observed on the calibration set and the prediction set. Thus, we believe that bionic swarm intelligent optimization algorithms have the potential to enhance the performance of quantitative models considerably, which offers substantial support for the quality assessment of MC and shows promising applications in the domain of NIR analysis.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"260 ","pages":"Article 116822"},"PeriodicalIF":3.1,"publicationDate":"2025-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143674013","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}
引用次数: 0
Letter to Editor: Critical commentary on the study of Siddig et al: Pharmacovigilance of drug-drug interactions: A pharmacokinetic study on the combined oral administration of lurasidone and clozapine in rats by using LC-MS/MS 致编辑的信对 Siddig 等人研究的评论:药物相互作用的药物警戒:利用LC-MS/MS对大鼠联合口服鲁拉西酮和氯氮平的药代动力学研究。
IF 3.1 3区 医学
Journal of pharmaceutical and biomedical analysis Pub Date : 2025-03-14 DOI: 10.1016/j.jpba.2025.116799
Jan Juřica
{"title":"Letter to Editor: Critical commentary on the study of Siddig et al: Pharmacovigilance of drug-drug interactions: A pharmacokinetic study on the combined oral administration of lurasidone and clozapine in rats by using LC-MS/MS","authors":"Jan Juřica","doi":"10.1016/j.jpba.2025.116799","DOIUrl":"10.1016/j.jpba.2025.116799","url":null,"abstract":"","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"260 ","pages":"Article 116799"},"PeriodicalIF":3.1,"publicationDate":"2025-03-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143674007","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}
引用次数: 0
Deciphering the mechanism of Annona muricata leaf extract in alloxan-nicotinamide-induced diabetic rat model with 1H-NMR-based metabolomics approach
IF 3.1 3区 医学
Journal of pharmaceutical and biomedical analysis Pub Date : 2025-03-12 DOI: 10.1016/j.jpba.2025.116806
Siti Norliyana Zubaidi , Pei Lou Wong , Wasim S.M. Qadi , Esraa Adnan Dawoud Dawoud , Hamizah Shahirah Hamezah , Syarul Nataqain Baharum , Faidruz Azura Jam , Faridah Abas , Andres Moreno , Ahmed Mediani
{"title":"Deciphering the mechanism of Annona muricata leaf extract in alloxan-nicotinamide-induced diabetic rat model with 1H-NMR-based metabolomics approach","authors":"Siti Norliyana Zubaidi ,&nbsp;Pei Lou Wong ,&nbsp;Wasim S.M. Qadi ,&nbsp;Esraa Adnan Dawoud Dawoud ,&nbsp;Hamizah Shahirah Hamezah ,&nbsp;Syarul Nataqain Baharum ,&nbsp;Faidruz Azura Jam ,&nbsp;Faridah Abas ,&nbsp;Andres Moreno ,&nbsp;Ahmed Mediani","doi":"10.1016/j.jpba.2025.116806","DOIUrl":"10.1016/j.jpba.2025.116806","url":null,"abstract":"<div><div>The leaves of <em>Annona muricata</em> Linn. have long been utilized in traditional medicine for diabetes treatment, and there is no study that has employed a metabolomics approach to investigate the plant's effects in managing the disease. We aimed to explore the antidiabetic effects of the standardised <em>A. muricata</em> leaf extract on diabetes-induced rats by alloxan monohydrate (Ax) and nicotinamide (NA) using a proton nuclear magnetic resonance (¹H-NMR)-based metabolomics approach. Absolute quantification was performed on the leaf extract using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Two different doses of the extract were administered orally for four weeks to diabetic rats induced with Ax + NA, and physical evaluations, biochemical analyses, and ¹H-NMR metabolomics of urine and serum were assessed. The results showed that quercetin 3-rutinoside was the most abundant compound in the 80 % ethanolic extract of <em>A. muricata</em> leaf. The induction of type 2 diabetes mellitus (T2DM) in the rat model was confirmed by the clear metabolic distinction between normal rats, diabetic rats, and metformin-treated diabetic rats. The low-dose of <em>A. muricata</em> leaf extract (200 mg/kg) was found to exhibit better results, significantly reducing serum urea levels in diabetic rats, with effects comparable to those of metformin. Additionally, metabolite analysis from ¹H-NMR metabolomics of serum and urine showed a slight shift toward normal metabolic profiles in the treated diabetic rats. Pathway analysis revealed alterations in the tricarboxylic acid cycle (TCA), pyruvate metabolism, and glycolysis/gluconeogenesis pathways in the diabetic rat model, which were improved following treatment with the <em>A. muricata</em> leaf extract. Overall, this study provides scientific support for its traditional use in diabetes management and offers new insights into the underlying molecular mechanisms.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"260 ","pages":"Article 116806"},"PeriodicalIF":3.1,"publicationDate":"2025-03-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143637173","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}
引用次数: 0
Elucidating the mechanisms of Shenwu Capsule in improving the cognitive decline in aging based on the UPLC-Q-TOF-MS, network pharmacology, and experimental validation
IF 3.1 3区 医学
Journal of pharmaceutical and biomedical analysis Pub Date : 2025-03-12 DOI: 10.1016/j.jpba.2025.116818
Zizhao Cheng , Shengyao Wang , Xuesi Hua , Li Zhang , Boya Li , Huiling Li , Yunya Bai , Yali Li , Jinping Hao , Jianxiong Wang , Lingyi Zhao , Dan Gao , Lan Zhang
{"title":"Elucidating the mechanisms of Shenwu Capsule in improving the cognitive decline in aging based on the UPLC-Q-TOF-MS, network pharmacology, and experimental validation","authors":"Zizhao Cheng ,&nbsp;Shengyao Wang ,&nbsp;Xuesi Hua ,&nbsp;Li Zhang ,&nbsp;Boya Li ,&nbsp;Huiling Li ,&nbsp;Yunya Bai ,&nbsp;Yali Li ,&nbsp;Jinping Hao ,&nbsp;Jianxiong Wang ,&nbsp;Lingyi Zhao ,&nbsp;Dan Gao ,&nbsp;Lan Zhang","doi":"10.1016/j.jpba.2025.116818","DOIUrl":"10.1016/j.jpba.2025.116818","url":null,"abstract":"<div><div>Given the growing incidence of dementia-related disorders in the aging population, identifying effective treatments for age-related cognitive decline (ARCD) is crucial. Shenwu Capsule (SWC), shown to have therapeutic efficacy in phase III clinical trials for senile dementia, has unclear mechanisms and active ingredients. Aged mice were administered SWC orally for three months, and behavioral tests, including the Morris water maze, Y maze, and novel object recognition, assessed learning and memory. Neuronal damage was evaluated using histopathology, and the levels of Aβ and phosphorylated tau proteins were measured. UPLC-Q-TOF-MS identified 11 components of SWC capable of crossing the blood-brain barrier (BBB), and network pharmacology was employed to explore their potential mechanisms. Through various detection methods, including transmission electron microscopy, Western blotting, qRT-PCR, ELISA, and immunofluorescence, six key targets (AKT1, TNF, TP53, SRC, EGFR, BCL2) were elucidated. GO and KEGG pathway analyses revealed that the PI3K/Akt signaling pathway plays a crucial role in the pharmacological effects of SWC. SWC was found to suppress neuronal apoptosis by activating the PI3K/Akt/Bcl-2 signaling pathway, as demonstrated by changes in mRNA and protein levels. Histological analysis further showed that SWC treatment restored mitochondrial morphology in the hippocampus of aged mice. Molecular docking simulations confirmed strong binding affinities between the active components and key targets. Psoralidin, a component with strong molecular docking potential, was shown in vitro to activate the PI3K/Akt/Bcl-2 pathway, reduce ROS, decrease apoptosis, improve mitochondrial morphology, and stabilize mitochondrial membrane potential. These protective effects were blocked by the PI3K inhibitor LY294002. Overall, SWC ameliorates ARCD through modulation of the PI3K/Akt/Bcl-2 signaling pathway, with psoralidin identified as a potential active ingredient.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"260 ","pages":"Article 116818"},"PeriodicalIF":3.1,"publicationDate":"2025-03-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143674004","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Impact of ultralow oxygen preservation on the quality of Atractylodis Macrocephalae Rhizoma evaluated by multi-chromatographic determination of small molecules and polysaccharides
IF 3.1 3区 医学
Journal of pharmaceutical and biomedical analysis Pub Date : 2025-03-11 DOI: 10.1016/j.jpba.2025.116813
Yu-Qing Zhu , Jing-Wen Liu , Jing Zhou , Cheng-Ying Wu , Fang Long , Jin-Di Xu , Shan-Shan Zhou , Qian Mao , Ming Kong , Song-Lin Li , Hong Shen
{"title":"Impact of ultralow oxygen preservation on the quality of Atractylodis Macrocephalae Rhizoma evaluated by multi-chromatographic determination of small molecules and polysaccharides","authors":"Yu-Qing Zhu ,&nbsp;Jing-Wen Liu ,&nbsp;Jing Zhou ,&nbsp;Cheng-Ying Wu ,&nbsp;Fang Long ,&nbsp;Jin-Di Xu ,&nbsp;Shan-Shan Zhou ,&nbsp;Qian Mao ,&nbsp;Ming Kong ,&nbsp;Song-Lin Li ,&nbsp;Hong Shen","doi":"10.1016/j.jpba.2025.116813","DOIUrl":"10.1016/j.jpba.2025.116813","url":null,"abstract":"<div><div>Atractylodis Macrocephalae Rhizoma (AMR) is one of the commonly used medicinal and edible herbs in China. To prevent infestation of moths and mildew, chemical-fumigation is applied during post-harvest processing, which would produce harmful substances. Ultralow oxygen (ULO) storage, as a potential controlled atmosphere preservation method for Traditional Chinese Medicines (TCMs), has no residue of chemical hazards, but its impact on chemical composition of TCMs is unclear. Here, to evaluate the impact of ULO preservation on the quality of AMR, a UPLC-QTOF-MS/MS-based non-targeted metabolomics approach was employed to screen out the differential components after AMR had been stored under ULO conditions for 18 months. The differential components were identified, and further semi-quantified with peak areas. Additionally, the differential components with known activity were quantified using HPLC-DAD and GC-TQ-MS/MS analysis. The molecular weight distribution and monosaccharide composition of polysaccharides were analyzed using HPGPC-ELSD and HPLC-DAD to assess the impact of ULO on the carbohydrates. As it showed, 20 differential components of AMR under ULO were screened and identified when compared to normal atmosphere (NA) with 21 % oxygen concentration. As storage duration increased, the levels of atractylenolides I, II, and III in both ULO and NA storage conditions increased, with significant differences in their total content (16.06 mg/g in ULO vs. 47.57 mg/g in NA). Confirmatory experiments revealed that atractylone is the precursor compound of atractylenolides and the total content of atractylenolides I, II, and III produced from atractylone in ULO storage was only 62.12 % of that in NA at 18th month. The total sugar content of AMR polysaccharides in ULO storage was 107.28 % of that in NA and the molar ratios of monosaccharides were also relatively constant. All the results indicated that ULO preservation slowed down the chemical transformation of AMR, including small molecules and polysaccharides. Therefore, the quality of AMR stored in ULO is more stable and it is proposed to be an efficient preservation method for AMR.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"260 ","pages":"Article 116813"},"PeriodicalIF":3.1,"publicationDate":"2025-03-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143620191","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}
引用次数: 0
Reverse traceability analysis of estrogenic active ingredients in Cuscutae semen based on intestinal and hepatic metabolism
IF 3.1 3区 医学
Journal of pharmaceutical and biomedical analysis Pub Date : 2025-03-11 DOI: 10.1016/j.jpba.2025.116819
Xiangming Sun , Mingyao Zhao , Wei Liang , Hui Song , Zhongyuan Qu , Liyang Sui , Wenlan Li
{"title":"Reverse traceability analysis of estrogenic active ingredients in Cuscutae semen based on intestinal and hepatic metabolism","authors":"Xiangming Sun ,&nbsp;Mingyao Zhao ,&nbsp;Wei Liang ,&nbsp;Hui Song ,&nbsp;Zhongyuan Qu ,&nbsp;Liyang Sui ,&nbsp;Wenlan Li","doi":"10.1016/j.jpba.2025.116819","DOIUrl":"10.1016/j.jpba.2025.116819","url":null,"abstract":"<div><div>As a traditional Chinese medicine for reinforcing kidney, Cuscutae semen can be applied in regulating the level of estrogen. And nine direct-acting substances <em>in vivo</em> with estrogenic effect has been figured out according to our previous research. However, their transformation relationship and the prototype forms of some metabolites are still not clear, impeding the elucidation of the effective substances of Cuscutae semen. In this study, to reveal the metabolic pathways of nine direct-acting substances <em>in vivo</em>, the hepatic and intestinal metabolism of nine monomer components from Cuscutae semen were investigated using liver microsomes of female rats and intestinal flora in ovariectomized rats. Based on ultra performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UPLC/Q-TOFMS) method, a total of 35 hepatic metabolites and three intestinal metabolites were tentatively identified respectively. The proposed metabolic pathways of main metabolites were discussed. Glucuronidation binding reactions played a dominant role in the hepatic metabolism. While in the intestinal metabolism, flavonoid glycosides were hydrolyzed into the aglycones without further phase II metabolic reaction. According to the achievements above, a reverse traceability analysis of the direct-acting substances <em>in vivo</em> was conducted, and the metabolic transformation relationship between the components was clarified except for methylated quercetin glucuronide. It is tentatively speculated that kaempferol, quercetin, apigenin, hyperin, astragalin and isoquercitrin in Cuscutae semen are potential estrogenic effective substances, which can be used as reference for quality control.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"260 ","pages":"Article 116819"},"PeriodicalIF":3.1,"publicationDate":"2025-03-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143627841","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}
引用次数: 0
The cutting edge of surveillance: Exploring high-resolution mass spectrometry in wastewater-based epidemiology for monitoring forensic samples
IF 3.1 3区 医学
Journal of pharmaceutical and biomedical analysis Pub Date : 2025-03-11 DOI: 10.1016/j.jpba.2025.116821
Asmaa Kamal El-Deen , Chaudhery Mustansar Hussain
{"title":"The cutting edge of surveillance: Exploring high-resolution mass spectrometry in wastewater-based epidemiology for monitoring forensic samples","authors":"Asmaa Kamal El-Deen ,&nbsp;Chaudhery Mustansar Hussain","doi":"10.1016/j.jpba.2025.116821","DOIUrl":"10.1016/j.jpba.2025.116821","url":null,"abstract":"<div><div>Criminal activity has always been detected through forensic evidence. However, the potential for using such evidence to stop crimes in their tracks or slow them down has not yet been completely realized. There is a lot of potential for assessing trace quantities of chemicals in wastewater systems to provide effective forensic information. Wastewater-based epidemiology (WBE) has emerged in the last decades as a crucial epidemiological information source for collecting data on community-wide health. It can add important knowledge about illicit drug consumption and/or disposal, exposure to pathogens, infectious diseases, industrial pollutants, and antibiotic resistance. The use of high-resolution mass spectrometry (HRMS) in WBE has revolutionized the field by enabling the detection and quantification of these compounds. This review article explores the cutting edge of surveillance in WBE through applying HRMS techniques for forensic sample monitoring. It delves into the most recent WBE applications, examining their advantages and disadvantages. It also explores the potential for obtaining a more comprehensive evaluation of forensic samples. Furthermore, the application of these approaches to generate “forensic intelligence” for surveillance and criminal interruption is discussed, with examples of how this data can be integrated into future work.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"260 ","pages":"Article 116821"},"PeriodicalIF":3.1,"publicationDate":"2025-03-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143601449","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}
引用次数: 0
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