Xiya Yan , Jinghua Hou , Siyu Yan , Wei Chang , Lisi Zhang , Zhanliang Wang , Sheng Yang
{"title":"New metabolites of methyltrienolone by in vitro human microsome and characterized using Liquid Chromatography/High Resolution Mass Spectrometry for doping control purposes","authors":"Xiya Yan , Jinghua Hou , Siyu Yan , Wei Chang , Lisi Zhang , Zhanliang Wang , Sheng Yang","doi":"10.1016/j.jpba.2024.116552","DOIUrl":"10.1016/j.jpba.2024.116552","url":null,"abstract":"<div><div>Methyltrienolone (17β-hydroxy-17α-methylestra-4,9,11-trien-3-one) is one of the anabolic androgenic steroids (AAS) banned by the World Anti-Doping Agency (WADA). The biotransformation of methyltrienolone is performed in vitro by human hepatocytes microsomes. Both phase I and phase II experiments are investigated. The incubation samples were extracted and injected to Liquid Chromatography/High Resolution Mass Spectrometry (LC-HRMS), or reacted with methoxylamine (29 Da added) or hydroxylamine (15 Da added), to increase the detection sensitivity. The extracted ion chromatograms of the negative control and the positive samples are compared, and 7 groups of phase I metabolites were found. The metabolic pathways including 17-epimerization, mono-hydroxylation, dihydroxylation, reduced combining mono- or dihydroxylation, as well as 18-nor which are observed and tentatively identified according to the mass spectra by high resolution mass spectrometry. The 18-nor metabolites will potentially be the long-term metabolite in doping control analysis. Its main phase II metabolites, glucuronides of metabolites are all obtained and analyzed.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"253 ","pages":"Article 116552"},"PeriodicalIF":3.1,"publicationDate":"2024-10-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142546063","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}
Dunfang Wang , Lin Zhu , Haifan Liu , Xue Feng , Caijuan Zhang , Bin Liu , Tao Li , Li Liu , Hao Chang , Jingwei Sun , Lei Yang , Weipeng Yang
{"title":"Altered gut metabolites and metabolic reprogramming involved in the pathogenesis of colitis-associated colorectal cancer and the transition of colon \"inflammation to cancer\"","authors":"Dunfang Wang , Lin Zhu , Haifan Liu , Xue Feng , Caijuan Zhang , Bin Liu , Tao Li , Li Liu , Hao Chang , Jingwei Sun , Lei Yang , Weipeng Yang","doi":"10.1016/j.jpba.2024.116553","DOIUrl":"10.1016/j.jpba.2024.116553","url":null,"abstract":"<div><div>Colitis-associated colorectal cancer (CAC) is fatal and can develop spontaneously or as a complication of inflammatory bowel diseases. Although co-administration of azoxymethane/dextran sulfate sodium (AOM/DSS) is a classic method for CAC modeling, its limitations need to be addressed. Accordingly, we aimed to optimize the AOM/DSS model to study CAC extensively and further investigate its pathogenic mechanisms relative to microbiota and metabolism. We optimized the CAC model via a single or enhanced injection of AOM combined with different administration modes and varying DSS concentrations. Subsequently, the fecal-microbiota composition was examined using 16S RNA sequencing, and fecal-colon-metabolome profiles were evaluated via ultra-high performance liquid chromatography-mass spectrometry. Two interval injections of AOM combined with 1.5 % DSS-free drinking resulted in a high tumor formation rate, uniform tumor formation, and low mortality. Based on this model, we innovatively divided the pathogenesis of CAC into three stages, namely inflammation induction, proliferation initiation, and tumorigenesis, and examined the pathological characteristics in each stage. Gut microbial dysbiosis and metabolic alteration drove colorectal tumorigenesis by aggravating inflammation while promoting cell proliferation and carcinogenesis in mice. For the first time, we dynamically demonstrated the process of colon \"inflammation to cancer\" transformation and provided novel insights to clarify the role of amino acid metabolism in the formation of CAC.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"253 ","pages":"Article 116553"},"PeriodicalIF":3.1,"publicationDate":"2024-10-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142561382","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}
Xiu Gu , Yanping Li , Yang Li , Xiaohui Duan , Youfan Hu , Jialuo Chen , Huan Du , Jing Bai , Chengyan He , Caihong Bai , Jinlin Guo , Jiahui Yang , Kaifeng Hu
{"title":"Integrating 2D NMR-based metabolomics and in vitro assays to explore the potential viability of cultivated Ophiocordyceps sinensis as an alternative to the wild counterpart","authors":"Xiu Gu , Yanping Li , Yang Li , Xiaohui Duan , Youfan Hu , Jialuo Chen , Huan Du , Jing Bai , Chengyan He , Caihong Bai , Jinlin Guo , Jiahui Yang , Kaifeng Hu","doi":"10.1016/j.jpba.2024.116551","DOIUrl":"10.1016/j.jpba.2024.116551","url":null,"abstract":"<div><div><em>Ophiocordyceps sinensis</em> is widely used to treat various diseases and as a health supplement. The present study comprehensively compared the metabolic differences between wild and cultivated <em>O. sinensis</em> through 2D <sup>1</sup>H-<sup>13</sup>C HSQC-based metabolomics, and assessed their anti-lung cancer activity on A549 cells. To characterize the global metabolic profile, sample preparation was scrutinously optimized, and both polar (1:4 methanol-water) and non-polar (1:4 methanol-chloroform) extracts of <em>O. sinensis</em> were investigated. A total of 47 and 10 metabolites were identified in the polar and non-polar extracts, respectively. Principal Component Analysis (PCA) revealed greater differences between the two types of <em>O. sinensis</em> in the polar extracts than in the non-polar extracts. Orthogonal Partial Least Squares-Discriminant Analysis (OPLS-DA) together with univariate tests captured 23 and 19 differential spectral features (with 22 and 11 of them assigned) between wild and cultivated <em>O. sinensis</em> in the polar and non-polar extracts, respectively. Meanwhile, the anti-lung cancer activities of both polar and non-polar extracts of wild and cultivated <em>O. sinensis</em> were assessed by MTS assay on A549 cells, and the sterols found in non-polar extracts, such as ergosterol, ergosterol peroxide, and 9,11-dehydroergosterol peroxide, and β-sitosterol, are the active ingredients with potential anti-lung cancer properties. In this study, we introduced a comprehensive strategy integrating 2D NMR-based metabolomics with <em>in vitro</em> assays for comparing the chemical composition and assessing the pharmacological activity of wild and cultivated <em>O. sinensis</em>. Our results provided a scientific basis for the potential viability of cultivated <em>O. sinensis</em> as an alternative to the wild counterpart.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"253 ","pages":"Article 116551"},"PeriodicalIF":3.1,"publicationDate":"2024-10-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142568974","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}
Jingxin Hou , Cong Hu , Hanyin Li , Hongmei Liu , Yangjiayi Xiang , Gou Wu , Yan Li
{"title":"Nanomaterial-based magnetic solid-phase extraction in pharmaceutical and biomedical analysis","authors":"Jingxin Hou , Cong Hu , Hanyin Li , Hongmei Liu , Yangjiayi Xiang , Gou Wu , Yan Li","doi":"10.1016/j.jpba.2024.116543","DOIUrl":"10.1016/j.jpba.2024.116543","url":null,"abstract":"<div><div>Magnetic solid-phase extraction (MSPE) holds significant scientific and technological interest as a novel sample preparation method for complex samples due to its easy operation, swift separation, high adsorption efficiency, and environmental friendliness. As the core of MSPE, magnetic sorbents have captured tremendous attention in recent years. Various promising nanomaterials, such as metal-organic frameworks and covalent organic frameworks, have been synthesized and utilized as sorbents in pharmaceutical and biomedical analysis. This review intends to (1) summarize recent progress of magnetic sorbents applied in this area and discuss their advantages, disadvantages, possible interaction mechanisms with the target substances; (2) explore their innovative applications in the analysis of pharmaceuticals, proteins, peptides, nucleic acids, nucleosides, metabolites, and other disease biomarkers from 2021 to 2024; (3) present the integration of MSPE with emerging analytical technologies; and (4) discuss the current challenges and future perspectives. It is expected to provide references and insights for the development of novel magnetic sorbents and their applications in bioanalysis.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"253 ","pages":"Article 116543"},"PeriodicalIF":3.1,"publicationDate":"2024-10-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142561381","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}
{"title":"Metabolomics of Withania somnifera L. extracts by an integrated LC-MS and NMR approach and evaluation of their tyrosinase inhibitory activity","authors":"Luciana Maria Polcaro , Antonietta Cerulli , Milena Masullo , Sonia Piacente","doi":"10.1016/j.jpba.2024.116520","DOIUrl":"10.1016/j.jpba.2024.116520","url":null,"abstract":"<div><div><em>Withania somnifera</em> L. (Solanaceae), for over 3000 years, has been considered an essential herb in Ayurvedic medicine. The roots of <em>W. somnifera</em> contain metabolites mainly belonging to steroidal lactones called withanolides, which possess various pharmacological activities such as neuroprotective, cardioprotective, anti-diabetic, antioxidant and anti-inflammatory. Since the demand on the market for <em>W. somnifera</em> extracts is increasing, with the aim to find an ecological and environmentally friendly strategy of extraction, the roots were submitted to different extraction techniques (macerations, ultrasound-assisted extraction and solid-liquid dynamic extraction) using EtOH:H<sub>2</sub>O 50:50, 75:25, 100:0. <em>W. somnifera</em> extracts were investigated by an integrated LC-ESI/QExactive/MS/MS and NMR approach to obtain comprehensive metabolite profiles. Principal Component Analysis of LC-MS and NMR data revealed how the extraction method and the solvent can affect the chemical profile of the extracts. Extracts obtained by maceration exhibited the highest amount of withanolides and withanosides, while the SLDE-Naviglio EtOH extract showed the highest amount of metabolites as benzoic acid, tropane alkaloids and sarcosine, reported for their CNS activity. Moreover, based on the use of this plant in the treatment of neurological disorders, the tyrosinase inhibitory activity of all the extracts was herein tested by spectrophotometric assay, showing IC<sub>50</sub> values in a range of 32.86–85.36 µg/ml.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"253 ","pages":"Article 116520"},"PeriodicalIF":3.1,"publicationDate":"2024-10-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142587245","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}
Xin Ding , Min Xu , Ya Zhang , Cuiping Long , Xuemei Su , Yang Zhang , Yan Qiao , Xingxing Zhang , Qian Zhou , Guangguo Tan , Jing Ma
{"title":"Integration of four-dimensional proteomics and network pharmacology to reveal molecular mechanisms of multi-components multi-targets effects of Sini decoction on myocardial infarction","authors":"Xin Ding , Min Xu , Ya Zhang , Cuiping Long , Xuemei Su , Yang Zhang , Yan Qiao , Xingxing Zhang , Qian Zhou , Guangguo Tan , Jing Ma","doi":"10.1016/j.jpba.2024.116526","DOIUrl":"10.1016/j.jpba.2024.116526","url":null,"abstract":"<div><div><em>Sini</em> Decoction (SND) has been proven to be an effective formula to alleviate cardiac injury of myocardial infarction (MI). However, the potential mechanism of SND remains unclear. In this study, the MI rat model was established by ligating the left anterior descending coronary artery. A total of 17 SND-distributed components in heart were identified by using ultra-high performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry (UHPLC-Q-TOFMS). The combination of four-dimensional (4D) proteomics and network pharmacology was employed to find the potential targets for therapeutic intervention, and molecular docking and cellular thermal shift assay (CETSA) were used to reveal the interactions between the potential targets and the potential active components distributed in heart of SND. 33 SND-effected proteins were identified by 4D proteomics, which was involved in carbon metabolism, fatty acid metabolism, valine, leucine and isoleucine degradation, tricarboxylic acid (TCA) cycle and PPAR signaling pathway. 17 potential SND-targeted direct proteins were screened by comparing SND-effected proteins generated from 4D proteomics with the MI-related proteins obtained from disease database. The potential relationships between 17 components and 17 potential SND-targeted direct proteins were established by molecular docking analysis, in which songorine, benzoylhypaconine, hypaconine, formononetin, and liquiritigenin could be bound to the surrounding amino acid residues in the binding pocket of Mtor, Parp1, Acadm, Crat, and Aldh2. Then, CETSA analysis further confirmed that songorine and benzoylhypaconine could increase the heat stability of Mtor and Parp1 in cardiac tissue lysate, respectively, which suggested that there existed direct interactions between songorine and Mtor, and benzoylhypaconine and Parp1. In summary, this work concluded that SND produced cardioprotective effects mainly through preserving energy metabolism, also demonstrated that the combination of 4D proteomics and network pharmacology was a promising tool for uncovering the molecular mechanisms of multi-components multi-targets effects of TCM.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"253 ","pages":"Article 116526"},"PeriodicalIF":3.1,"publicationDate":"2024-10-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142561383","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}
Xina Yu , Shanshan Song , Zhanhua Li , Tiantian Wang , Hui Huang , Qing Shen , Zongyuan Wu , Pei Luo
{"title":"Targeted LC-MS/MS method of oxylipin profiling reveals differentially expressed serum metabolites in type 2 diabetes mice with panaxynol","authors":"Xina Yu , Shanshan Song , Zhanhua Li , Tiantian Wang , Hui Huang , Qing Shen , Zongyuan Wu , Pei Luo","doi":"10.1016/j.jpba.2024.116540","DOIUrl":"10.1016/j.jpba.2024.116540","url":null,"abstract":"<div><div>Panaxynol is a bioactive polyacetylene in food plants; however, its specific benefits in diabetes and metabolic disorders remain unclear. Previous studies have mainly focused on biochemical indicators and clinical evaluations. Limited research has systematically elucidated the beneficial effects of panaxynol from the oxylipins perspective. In this study, we employed an oxylipin analysis platform we previously established using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) based on the multiple reaction monitoring (MRM) method for the profiling of oxylipins. After a 7-week administration of panaxynol to db/db mice, significant alterations in serum oxylipins and potential benefits to hyperglycemia, insulin resistance, and hepatic steatosis were observed. Our analysis also revealed correlations among epoxygenase products derived from arachidonic acid (AA), linoleic acid (LA), and α-linolenic acid (ALA) via cytochrome P450 (CYP) pathways. Furthermore, six potential oxylipins were identified, as offering insights into the mechanisms by which panaxynol may modulate diabetes. These results provide the first <em>in vivo</em> evidence of the impact of panaxynol on oxylipin metabolism and lay the foundation for developing panaxynol as a nutraceutical for diabetes management.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"253 ","pages":"Article 116540"},"PeriodicalIF":3.1,"publicationDate":"2024-10-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142546064","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}
Baiyun Zhao , Jing Zhang , Kaiyue Zhao , Bin Wang , Jing Liu , Chaoxuan Wang , Ling Zeng , Xin Zeng , Yan Luo
{"title":"Effect of rapamycin on hepatic metabolomics of non-alcoholic fatty liver rats based on non-targeted platform","authors":"Baiyun Zhao , Jing Zhang , Kaiyue Zhao , Bin Wang , Jing Liu , Chaoxuan Wang , Ling Zeng , Xin Zeng , Yan Luo","doi":"10.1016/j.jpba.2024.116541","DOIUrl":"10.1016/j.jpba.2024.116541","url":null,"abstract":"<div><div>Rapamycin (Rapa) is an inhibitor of mTOR complex, and its therapeutic effect on liver function was examined in non-alcoholic fatty liver disease (NAFLD) rats here. And the possible mechanism of Rapa in NAFLD was preliminarily elucidated based on the non-targeted metabolomics analysis. Adult male SD rats were fed with a high-fat and high-cholesterol diet (HFD) to establish NAFLD model. For Rapa group, 0.8 mg/(kg.d) Rapa was given to the HFD rats. Ultra-performance liquid chromatography and Q-Tof-mass spectrometry (UPLC and Q-TOF/MS) analysis were applied for the identification of metabolites in the serum of rats, which were annotated using Kyoto Encyclopedia of Genes and Genomes (KEGG). NAFLD rats presented with disturbed liver function, lipid metabolism and oxidative stress, but Rapa exerted a mitigating influence on the disorders. The metabolite profile data identified 579 metabolites that varied remarkably between the Rapa and HFD groups, with the main classes of amino acids and peptides, benzene, lipids and fatty acids. The differential metabolites were mainly involved in biosynthesis of cofactors, bile secretion, and glycerophospholipid metabolism were mainly enriched. In conclusion, Rapa has a potential protective effect against HFD-induced NAFLD, its hepatoprotective effect may achieved through mediating bile secretion and glycerophospholipid metabolism.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"253 ","pages":"Article 116541"},"PeriodicalIF":3.1,"publicationDate":"2024-10-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142531589","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}
{"title":"Terminal deoxynucleotidyl transferase (TdT) based template-free signal amplification for the detection of exosomes in MUC1-positive cells","authors":"Wenchang Fu , Kaige Yang , Mingyuan Wu , Yan Wang","doi":"10.1016/j.jpba.2024.116539","DOIUrl":"10.1016/j.jpba.2024.116539","url":null,"abstract":"<div><div>The Mucin1 (MUC1) protein, involved in cytoprotective and signaling pathways, is abnormally elevated in various cancers, making it a key cancer indicator. Exosomes, which reflect the status of their originating cells, offer potential for cancer diagnosis. Thus, developing a method to detect MUC1-positive exosomes is crucial for the early diagnosis of certain cancers. In this study, we developed a highly sensitive, specific, and simple UV–visible signal amplification method to detect MUC1-positive exosomes using terminal deoxynucleotidyl transferase (TdT). Initially, exosomes were captured on magnetic beads using a CD63 aptamer(apt). The Primer-AuNPs-MUC1 apt complex which we synthesized by low pH loading method was then attached MUC1 proteins on the surface of the exosomes to create a sandwich structure. TdT catalyzed the extension of Biotin-dATP at the 3′ end of the primer, introducing multiple biotin sites into the sandwich structure. These sites subsequently bound multiple streptavidin-horseradish peroxidase (streptavidin-HRP), which catalyzed the oxidative color change of the substrate, which can be detected by colorimetric method. This method can detect A549 exosomes in the range of 1.4E+6 to 4.2E+8 particles/mL and shows high specificity for cell lines with different MUC1 expression. Additionally, it successfully distinguished cholangiocarcinoma (CCA) patients (n=11) from healthy individuals (n=7) in clinical serum assays, demonstrating good performance in real sample detection.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"253 ","pages":"Article 116539"},"PeriodicalIF":3.1,"publicationDate":"2024-10-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142502481","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}
Yang Hu , Xin Jiang , Xiefeng Zhang , Yuxin Lan , Shaohui Cai , Taotao Xu , Xinyue Zhuang , Morili Asheng , Jing Zeng , Yongping Qin , Guangsheng Qian
{"title":"A novel quantitative method for the determination of 10B-carrier boronophenylalanine in rat plasma by UHPLC-MS/MS and comparison with ICP-MS","authors":"Yang Hu , Xin Jiang , Xiefeng Zhang , Yuxin Lan , Shaohui Cai , Taotao Xu , Xinyue Zhuang , Morili Asheng , Jing Zeng , Yongping Qin , Guangsheng Qian","doi":"10.1016/j.jpba.2024.116538","DOIUrl":"10.1016/j.jpba.2024.116538","url":null,"abstract":"<div><div>L-Boronophenylalanine (BPA), a widely used <sup>10</sup>B carrier for clinical boron neutron capture therapy (BNCT), was quantified in rat plasma through a simple, effective and stable ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method. Chromatographic separation was performed on an ACQUITY UPLC HSS T3 (100 mm × 2.1 mm, 1.8 μm) column with the mobile phase of 0.5 % formic acid aqueous solution and acetonitrile. For the detector, the <em>m/z</em> ion pairs used for quantification were 209.1→120.1 for BPA and 210.1→120.1 for internal standard in a positive mode by electrospray ionization (ESI) using multiple reaction monitoring (MRM). The method is specific and robust with rare affection by endogenous substances in the matrix. A good linear relationship was observed over 80–80000 ng/mL (r<sup>2</sup> = 0.9993). The values of inter- and intra-day accuracy and precision were within the acceptance criteria of ±15 %. BPA was found to be stable under different experimental conditions. This developed method was successfully applied on a pharmacokinetic experiment on Sprague-Dawley rats (intravenous injection, 125 mg/kg) and a comparation between UHPLC-MS/MS and ICP-MS for BPA was carried out.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"253 ","pages":"Article 116538"},"PeriodicalIF":3.1,"publicationDate":"2024-10-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142502445","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}