Victor Pereira Francisco , Muriel Cerny , Romain Valentin , Franck Milone-Delacourt , Alexandra Paillard , Marion Alignan
{"title":"Development of GC–MS coupled to GC–FID method for the quantification of cannabis terpenes and terpenoids: Application to the analysis of five commercial varieties of medicinal cannabis","authors":"Victor Pereira Francisco , Muriel Cerny , Romain Valentin , Franck Milone-Delacourt , Alexandra Paillard , Marion Alignan","doi":"10.1016/j.jchromb.2024.124316","DOIUrl":"10.1016/j.jchromb.2024.124316","url":null,"abstract":"<div><p>Cannabis terpenes and terpenoids are among the major classes of pharmacologically active secondary metabolites of therapeutic interest. Indeed, these hydrocarbon molecules, responsible for the characteristic aroma of cannabis flowers, are thought to be involved in a synergistic effect known as the “entourage effect”, together with cannabinoids. Numerous analytical studies have been carried out to characterize the terpene and terpenoid contents of some cannabis varieties, but they have not proposed any real quantification or have described a limited number of analytical standards or average response factors, which may have led to over- or underestimation of the real content of the cannabis flowers. Real and reliable quantification is necessary to justify the entourage effect. Here, we report a rigorous and precise GC–FID and GC–MS method for the identification and quantification of cannabis terpenes and terpenoids. This method is distinguished by the use of a high number of analytical standards, the determination of retention indices for all compounds studied, an exhaustive comparison of databases and scientific literature, the use of relevant response factors, and internal calibration for reliable results. It was applied to the study of terpenic compounds in five commercial varieties of medicinal cannabis produced by Bedrocan International: a CBD-rich (Bedrolite®), a THC/CBD balanced (Bediol®), and three THC-dominant (Bedrocan®, Bedica® and Bedrobinol®). Two extraction solvents are described (ethanol and hexane) to compare their selectivity towards target molecules, and to describe as exhaustively as possible the terpenic profile of the five pharmaceutical-grade varieties. Twenty-three standards were used for accurate dosages. This work highlights that the choice of solvent and the analysis method reliability are critical for the study of these terpenic compounds, regarding their contribution to the entourage effect.</p></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124316"},"PeriodicalIF":2.8,"publicationDate":"2024-09-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S1570023224003258/pdfft?md5=b534067b7e837343bd206d7061a97505&pid=1-s2.0-S1570023224003258-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142272510","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}
{"title":"Anion exchange-HPLC method for evaluating the encapsulation efficiency of mRNA-loaded lipid nanoparticles using analytical quality by design","authors":"Shoki Hara, Shuntaro Arase, Syusuke Sano, Takuya Suzuki, Iori Mizogaki, Shinya Sato, Koji Ukai","doi":"10.1016/j.jchromb.2024.124317","DOIUrl":"10.1016/j.jchromb.2024.124317","url":null,"abstract":"<div><p>Lipid nanoparticles (LNPs) are emerging nucleic acid delivery systems in the development of mRNA therapeutics such as the severe acute respiratory syndrome coronavirus 2 vaccines. However, a suitable analytical method for evaluating the encapsulation efficiency (EE) of the LNPs is required to ensure drug efficacy, as current analytical methods exhibit throughput issues and require long analysis times. Hence, we developed and validated an anion-exchange HPLC method using Analytical Quality by Design. Three critical method parameters (CMPs) were identified using risk assessment and Design of Experiments: column temperature, flow rate, and sodium perchlorate concentration. The CMPs were optimized using Face-Centered Central Composite Design. The discriminating power of the optimized HPLC method and RiboGreen assay was comparable. The main advantage of this method is that LNPs can be directly injected into the HPLC system without bursting the LNPs loaded with encapsulated poly(A). The optimized HPLC method was validated as robust, high-throughput, and sufficiently sensitive according to the ICH Q2 guidelines. We believe our findings could promote efficient LNPs-based drug development.</p></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124317"},"PeriodicalIF":2.8,"publicationDate":"2024-09-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142238799","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":"Identification of fentanyl analogs and potential biomarkers in urine using liquid chromatography-tandem mass spectrometry (LC-MS/MS) and liquid chromatography-quadrupole/time of flight mass spectrometry (LC-Q/TOF-MS)","authors":"Madison Schackmuth, Sarah Kerrigan","doi":"10.1016/j.jchromb.2024.124303","DOIUrl":"10.1016/j.jchromb.2024.124303","url":null,"abstract":"<div><div>Novel synthetic opioids are a class of drugs abused for their potent analgesic effect and are responsible for many fatal intoxications, particularly within the United States. A targeted assay was developed and validated using LC-MS/MS, capable of identifying nineteen fentalogs. Solid phase extraction was used to isolate analytes of interest from urine. Limits of detection ranged from 0.05 to 0.1 ng/mL and the limit of quantitation was 0.5 ng/mL. Extraction efficiencies using the optimized procedure were 77–88 % for all targeted species. Bias, precision, matrix effects and interferences were within acceptable thresholds for all analytes. The validated assay was used to identify analytes of interest from thirty-seven individuals that had used fentanyl and related substances. In addition to quantitative analyses, a non-targeted liquid chromatography quadrupole time-of-flight mass spectrometry (LC-Q/TOF-MS) assay was also used to identify additional substances and potential biomarkers. Additional N-oxide and N-dealkylated species were identified using this approach, and the potential for biomarker use is presented, given the stability of some analytes within this class.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124303"},"PeriodicalIF":2.8,"publicationDate":"2024-09-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142322517","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}
Richard K.T. Kam, Jenny Y.K. Cheng, Shreenidhi R. Subramaniam, Jeffrey S.S. Kwok
{"title":"Semi-quantitative analysis of serum and cerebrospinal fluid transferrin glycoforms by top-down liquid chromatography mass spectrometry","authors":"Richard K.T. Kam, Jenny Y.K. Cheng, Shreenidhi R. Subramaniam, Jeffrey S.S. Kwok","doi":"10.1016/j.jchromb.2024.124306","DOIUrl":"10.1016/j.jchromb.2024.124306","url":null,"abstract":"<div><p>Detection of β-2 transferrin in body fluid could help identify cerebrospinal fluid (CSF) leakage. The most common method, isoelectric focusing, was qualitative and could not provide detailed <em>N</em>-glycan structural information. We presented an alternative method using top-down liquid chromatography-time of flight mass spectrometry (LC-TOF MS). After immunoaffinity enrichment<strong>,</strong> fluid transferrin glycoforms were analyzed by a high-resolution LC-TOF MS, and the <em>N</em>-glycan structure predicted by accurate mass. The performance was validated with imprecision at 15%, with a cut-off of 0.04 for β-2 transferrin to tetrasialotransferrin ratio to confirm the presence of CSF in fluid samples.</p></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124306"},"PeriodicalIF":2.8,"publicationDate":"2024-09-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142238800","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}
Aristeidis Lentzas , Nikkie Venekamp , Jos H. Beijnen , Olaf van Tellingen
{"title":"Development and validation of an LC-MS/MS method for simultaneous quantification of eight drugs in plasma and brain: Application in a pharmacokinetic study in mice","authors":"Aristeidis Lentzas , Nikkie Venekamp , Jos H. Beijnen , Olaf van Tellingen","doi":"10.1016/j.jchromb.2024.124308","DOIUrl":"10.1016/j.jchromb.2024.124308","url":null,"abstract":"<div><p>A selective and sensitive liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS) method was developed and validated for simultaneous quantitation of a cassette of 8 drugs, including docetaxel, erlotinib, loperamide, riluzole, vemurafenib, verapamil, elacridar and tariquidar. Stable isotopically labeled compounds were available for use as internal standards for all compounds, except for tariquidar for which we used elacridar-d4. Sample pre-treatment involved liquid–liquid extraction using <em>tert</em>-butyl-methyl ether as this resulted in good recovery and low ion suppression. Chromatographic separation was achieved using a Zorbax Extend C18 analytical column and a linear gradient from 20 % to 95 % methanol in 0.1 % (v/v) formic acid in water. MS/MS detection using multiple reaction monitoring was done in positive ionization mode. We validated this assay for human and mouse plasma and mouse brain homogenates. The calibration curves were linear over a range 1–200 nM for each drug in the mix, except for tariquidar probably due to the lack of a stable isotope labeled analog. The intra-day and inter-day accuracies were within the 85–115 % range for all compounds at low, medium and high concentrations in the three different matrices. Similarly, the precision for all compounds at three different concentration levels ranged below 15 %, with the exception of tariquidar in mouse plasma and brain homogenate and riluzole in brain homogenate. Pilot studies have confirmed that the method is suitable for the analysis of mouse plasma samples and brain homogenates following cassette dosing of this mixture in mice.</p></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124308"},"PeriodicalIF":2.8,"publicationDate":"2024-09-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142238966","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}
Guannan Wang , Jiaxue Wang , Tao Zhen , Hongjin Wang , Lixin Sun
{"title":"Identification of chemical constituents and pharmacokinetic characteristics of Xiaoyan Tuire Granule in rats","authors":"Guannan Wang , Jiaxue Wang , Tao Zhen , Hongjin Wang , Lixin Sun","doi":"10.1016/j.jchromb.2024.124309","DOIUrl":"10.1016/j.jchromb.2024.124309","url":null,"abstract":"<div><p>Xiaoyan Tuire Granule is a type of Chinese patent medicine that has been proven effective in treating respiratory tract infections. However, while it has been successfully introduced into clinical use, more knowledge is still needed regarding its chemical components and pharmacokinetics. This study investigated the chemical profile in the medicine and rat plasma by ultra high-performance liquid chromatography coupled with Q Exactive hybrid quadrupole-orbitrap high-resolution accurate mass spectrometry (UHPLC-Orbitrap-MS/MS). Subsequently, it developed a validated ultra high-performance liquid chromatography coupled with quadrupole mass spectrometry (UHPLC-MS/MS) method for determining five components in rat plasma after oral administration of Xiaoyan Tuire Granule. As a result, a total of 106 constituents were inferred, including 9 terpenoids, 29 flavonoids, 33 organic acids, 12 phenylpropanoids and 23 other compounds. After administration, 86 compounds were inferred in rat plasma, including 73 prototypes and 13 metabolites. The metabolic pathways were primarily hydrogenation, glucuronic acid conjugation, sulfate conjugation, hydrolysis and methylation. The established method determined the contents of esculetin, esculin, isovitexin, caffeic acid and p-coumaric acid had a good separation, and all the legal verification met the requirements. The pharmacokinetic results indicate that the absorption rate of the five compounds <em>in vivo</em> was rapid, with a T<sub>max</sub> of less than 0.25 h, and the elimination rate was also fast, with a half-time (T<sub>1/2</sub>) ranging from 1.22 h to 2.19 h. It is worth noting that esculin and esculetin have similar half-time <em>in vivo</em> due to their structural similarities. Among these five compounds, the AUC<sub>0-∞</sub> and MRT<sub>0-∞</sub> of p-coumaric acid and esculetin were relatively higher, indicating higher exposure and longer residence time of both compounds <em>in vivo</em>. In conclusion, this paper researched the chemical constituents and pharmacokinetics of Xiaoyan Tuire Granule, which provided the reference for further study.</p></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124309"},"PeriodicalIF":2.8,"publicationDate":"2024-09-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142167826","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":"Quantification of mycolic acids in different mycobacterial species by standard addition method through liquid chromatography mass spectrometry","authors":"Zeeshan Fatima , Meenakshi Chugh , Gaurav Nigam , Saif Hameed","doi":"10.1016/j.jchromb.2024.124297","DOIUrl":"10.1016/j.jchromb.2024.124297","url":null,"abstract":"<div><p><em>Mycobacteria</em> possess unique and robust lipid profile responsible for their pathogenesis and drug resistance. Mycolic acid (MA) represents an attractive diagnostic biomarker being absent in humans, inert and known to modulate host-pathogen interaction. Accurate measurement of MA is significant to design efficient therapeutics. Despite considerable advances in Liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS) based approaches, quantification of mycobacterial lipids including MA is still challenging mainly because of ion suppression effects due to complex matrix and non-availability of suitable internal standards for MA. The current study demonstrates the use of standard addition method (SAM) to circumvent this problem and provides a reliable and exhaustive analytical method to quantify mycobacterial MA based on reversed-phase ultra-high-performance liquid chromatography- mass spectrometry data acquisition. In this method, multiple reaction monitoring (MRM) has been applied, wherein 16 MRM channels or transitions have been chosen for quantification of alpha-, methoxy- and keto-MAs with C-24 and C-26 hydrocarbon chains that are actually best suited for TB diagnostics. We found that the overall methodological limit of detection and limit of quantification were in the range 0.05–0.71 ng/µl and 0.16–2.16 ng/µl. Taken together, SAM quantitative technique could serve as promising alternative for relative concentration determination of MA to aid medical research.</p></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124297"},"PeriodicalIF":2.8,"publicationDate":"2024-09-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142238899","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}
Sara I. Aboras , Mohamed A. Korany , Shaza A. Ebied , Rim S. Haggag , Mohamed M.A. Hamdy
{"title":"Hyphenating sustainability with chemometrics in chromatographic analysis of COVID combo therapy, nirmatrelvir and Molnupiravir, in presence of their overlapping degradation products; blue-green dual evaluation tools","authors":"Sara I. Aboras , Mohamed A. Korany , Shaza A. Ebied , Rim S. Haggag , Mohamed M.A. Hamdy","doi":"10.1016/j.jchromb.2024.124304","DOIUrl":"10.1016/j.jchromb.2024.124304","url":null,"abstract":"<div><p>Our manuscript managed to hyphenate the novelty and sustainability in one method. A novel combination of molnupiravir (MNP) and nirmatrelvir (NTV) was found to be a potential symbiotic therapy against SARS-CoV-2. Yet, there is no analytical method published for either determination or stability investigation of this combination simultaneously. So, the proposed HPLC technique focused on determination of MNP and NTV in presence of their degradation products. The sustainability was achieved in our method by using chemometrics tools to quantify NTV in presence of its co-eluted degradation product (NTV-D) without excessive time and solvent usage for separation (run time 5 min.). Moreover, the linearity parameters of both MNP and NTV, including correlation coefficient, LOD and LOQ, have been enhanced significantly after chemometrics treatment through convolution of the resultant derivative curves using trigonometric Fourier function. For example, LOQ of MNP decreased from 3.53 to 0.31 µg/mL and for NTV, LOQ decreased from 4.98 to 2.10 µg/mL after chemometrics treatment. The stability results of the proposed method indicates that no interaction or change in stability behavior of both drugs when co-administered with each other. Thus, this can be used as an empirical basis to initiate clinical trials of this combination for the treatment of COVID-19 patients.</p><p>Additionally, in order to determine the impact of chemometric methods in minimizing analysis time and reducing solvent, energy, and waste consumption, our chemometric methodology is evaluated in terms of greenness and blueness (dichromic assessment) using AGREE and BAGI, respectively. Besides, the method sustainability using Hexagon was evaluated.</p></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124304"},"PeriodicalIF":2.8,"publicationDate":"2024-09-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142167699","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}
Jianwei Ren , Hongzhong Liu , Yufang Ma , Wei Tian , Qinqin Li , Zhen Wu , Mengzhao Wang , Xiaoyun Liu , Xin Zheng , Xiaohong Han
{"title":"Development and validation of a UPLC-MS/MS method for rapid and simultaneous quantification of BPI-460372 and its metabolites BPI-460444 and BPI-460456 in human plasma","authors":"Jianwei Ren , Hongzhong Liu , Yufang Ma , Wei Tian , Qinqin Li , Zhen Wu , Mengzhao Wang , Xiaoyun Liu , Xin Zheng , Xiaohong Han","doi":"10.1016/j.jchromb.2024.124300","DOIUrl":"10.1016/j.jchromb.2024.124300","url":null,"abstract":"<div><p>In cancer development and progression, the Hippo signaling pathway functions. The transcriptional enhanced associate domain (TEAD) stands out as a pivotal transcription factor within this pathway, and the suppression of TEAD represents a promising approach for cancer treatment. The primary aim of the study was to establish an analytical method for the concurrent quantification of a novel TEAD target inhibitor, BPI-460372, and its principal metabolites, BPI-460444 and BPI-460456, in human plasma. The chromatographic separation utilized a XSelect™ HSS C<sub>18</sub> column (2.1 × 100 mm, 2.5 µm), while quantification was conducted on a SCIEX API 4000 mass spectrometer. 22 plasma samples were tested via the developed method. The calibration curve for BPI-460372 exhibited linearity from 2 to 2000 ng/mL, while its metabolites BPI-460444 and BPI-460456 had linearity between 1 and 1000 ng/mL (r > 0.99). The precision (RSD) was ≤ 17.1 %, and the accuracy (RE) fell within the range of −17.7 % to 15.0 %, all meeting acceptance criteria. The matrix effect was from 101.0 % to 105.8 %. The extraction recovery of analytes fell within the range of 96.8 % to 104.1 % with an RSD of less than 7.4 %. The developed method was effectively utilized in an advanced solid tumor patient, and the concentration trends of the three analytes in plasma were found to be largely consistent. The established analytical method showed great sensitivity, simplicity, accuracy, and reliability for the rapid and simultaneous analysis of the TEAD target inhibitor BPI-460372, alongside its major metabolites BPI-460444 and BPI-460456 in human plasma. This analytical method provided essential support for future clinical investigations and pharmacokinetic analysis.</p></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124300"},"PeriodicalIF":2.8,"publicationDate":"2024-09-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142162179","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}
Weijun Lv , Ying Yang , Yanxia Lv , Yifan Pan , Yunxiang Wang , Zhengzhong Zhu , Yi Tao
{"title":"Plasma metabolic profiling reveals that crude and processed Polygonatum cyrtonema hua extract ameliorates myocardial ischemia-induced damage by regulating branched-chain amino acid and energy metabolism","authors":"Weijun Lv , Ying Yang , Yanxia Lv , Yifan Pan , Yunxiang Wang , Zhengzhong Zhu , Yi Tao","doi":"10.1016/j.jchromb.2024.124301","DOIUrl":"10.1016/j.jchromb.2024.124301","url":null,"abstract":"<div><p><em>Polygonatum cyrtonema</em> Hua and its processed products have demonstrated cardio-protective effects, though the underlying mechanisms remain unclear. In this study, plasma metabolic profiling and pattern recognition were employed to explore the cardio-protective mechanisms of both crude and processed <em>P. cyrtonema</em> in a myocardial ischemia model induced by ligation, using gas chromatography-mass spectrometry. Post-modeling, plasma levels of creatine kinase-MB, lactate dehydrogenase, troponin T, and malondialdehyde were significantly elevated but were notably reduced after treatment. Conversely, plasma levels of glutathione peroxidase and superoxide dismutase, which were significantly decreased post-modeling, were restored following treatment. Hematoxylin-eosin (HE) and Masson staining revealed that both crude and processed <em>P. cyrtonema</em> effectively reduced inflammatory infiltration and fibrosis in cardiac tissue. Metabolic profiling identified 34 differential endogenous metabolites in the treatment groups, with 19 confirmed using standard compounds. The linear correlation coefficients (R2) for these standards ranged from 0.9960 to 0.9996, indicating high accuracy. The method exhibited excellent precision and repeatability, with relative standard deviation (RSD) values below 8.57%. Recovery rates were between 95.02% and 105.15%, and the stability of the standard compounds was confirmed after three freeze–thaw cycles, with RSD values under 4.42%. Both crude and processed <em>P. cyrtonema</em> were found to alleviate myocardial ischemia symptoms by regulating branched-chain amino acid metabolism and energy metabolism. These findings provide a solid foundation for the potential clinical use of this herb and its processed products in treating heart disease.</p></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124301"},"PeriodicalIF":2.8,"publicationDate":"2024-09-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142167698","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}