Xiao Yang , Yingjin Wang , Shuangyi Gong , Tingjian Xiong , Lihang Xie
{"title":"Integrated metabolomics and network pharmacology reveal the procoagulant mechanisms of Cirsium setosum extracts","authors":"Xiao Yang , Yingjin Wang , Shuangyi Gong , Tingjian Xiong , Lihang Xie","doi":"10.1016/j.jchromb.2024.124335","DOIUrl":"10.1016/j.jchromb.2024.124335","url":null,"abstract":"<div><div>As a medicinal plant, <em>Cirsium setosum</em> has excellent procoagulant effects and has long been used as a cure for hemoptysis, epistaxis, uremia and metrorrhagia caused by blood heat. However, the key medicinal part of <em>C. setosum</em>, as well as the biologically active substances that play a major role, are not known. In this study, the aboveground, underground and whole grass portions of <em>C. setosum</em> were subjected to a coagulation comparison experiment to determine the primary active procoagulant compounds. The main active procoagulant compounds of <em>C. setosum</em> were then screened using a comparative metabolomics analysis between aboveground and underground. Network pharmacology analysis was used to construct the “active ingredient-disease target-pathway” network. Finally, molecular docking was used to verify the binding ability and affinity between the key active ingredients obtained from the screening and the targets. The results indicated that the aboveground part of <em>C. setosum</em> could significantly shorten activated partial thromboplastin time (APTT) and that this part exerts substantial procoagulant effects. The total phenol, total flavonoid and total alkaloid content of the aboveground part was measured to be higher than those of the underground part and whole grass. Furthermore, comparative metabolomics analysis as well as the Traditional Chinese Medicine Systems Pharmacology Database and Analysis Platform (TCMSP) database and literature search screening yielded 10 active substances, including naringenin, guanine, 2,4-di-<em>tert</em>-butylphenol, calycosin-7-O-beta-D-glucoside, flavone, vitexin, and tiliroside, which may be related to the coagulation-promoting properties of <em>C. setosum</em> and its therapeutic effects on coagulation-related disorders. Network pharmacological analysis revealed that <em>C. setosum</em> may exert procoagulant effects mainly through tiliroside, calycosin-7-O-beta-D-glucoside, and flavone, which act on key target proteins, such as SRC, PRKACA, EGFR, AKT1, MAPK3, and GSK3B. In summary, <em>C. setosum</em> exerts its procoagulant and therapeutic effects on coagulation-related diseases through multiple compounds, targets, and pathways.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124335"},"PeriodicalIF":2.8,"publicationDate":"2024-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142418162","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":"Generation of affinity maps for thiazolidinediones with human serum albumin using affinity microcolumns. II. Effects of advanced glycation end products on multisite drug binding","authors":"Sadia Sharmeen, Ashley G. Woolfork, David S. Hage","doi":"10.1016/j.jchromb.2024.124333","DOIUrl":"10.1016/j.jchromb.2024.124333","url":null,"abstract":"<div><div>Multisite protein interactions by the thiazolidinedione-class drugs pioglitazone and rosiglitazone were examined by using high-performance affinity microcolumns that contained normal human serum albumin (HSA) vs HSA that had been modified to form advanced glycation end products by glyoxal (Go) or methylglyoxal (MGo). The results were used to generate an affinity map for these drugs at several key regions on HSA. Strong binding (∼10<sup>5</sup> M<sup>−1</sup>) by these drugs was seen at both Sudlow sites I and II. About a 50 % decrease in the affinities at Sudlow site II was observed for pioglitazone for Go-modified HSA, while either a 47 % decrease or 1.6-fold increase in affinity was seen for MGo-modified HSA, depending on the extent of modification. The binding affinity for rosiglitazone at Sudlow site II had a 40–83 % decrease for Go-modified HSA and either a non-significant change or 1.4-fold increase for MGo-modified HSA. At Sudlow site I, pioglitazone gave a 41 % decrease in affinity for either Go or MGo-modified HSA, and for rosiglitazone up to a 55 % decrease or 1.3-fold increase in affinity was noted. Positive allosteric effects were seen by these drugs with the tamoxifen site of HSA, and neither drug had any notable binding at the digitoxin site for the normal or modified forms of HSA. Rosiglitazone also had weak interactions at a site in subdomain IB, which increased in affinity by up to 5.0-fold with the Go- or MGo-modified HSA. This study illustrated how affinity microcolumns can be used to provide a detailed analysis of solute-protein systems that involve complex interactions. The data obtained should also be valuable in providing a better understanding of how drug interactions with HSA and other proteins can be altered by modifications of these binding agents in diseases such as diabetes.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124333"},"PeriodicalIF":2.8,"publicationDate":"2024-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142418163","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":"Serum metabolome alterations in hyperhomocysteinemia based on targeted and non-targeted MS-platforms","authors":"Xinshu Zhao , Xiaowei Liu , Liyan Liu , Rui Chen","doi":"10.1016/j.jchromb.2024.124336","DOIUrl":"10.1016/j.jchromb.2024.124336","url":null,"abstract":"<div><h3>Background and aims</h3><div>Hyperhomocysteinemia (Hhcy) is a pathological condition marked by increased level of homocysteine and serves as an independent risk factor for a range of diseases including cardiovascular diseases and Alzheimer’s disease. This study aims to examine alterations in Hhcy-related metabolites using serum metabolomics and unravel the distinct metabolic pathways involved, thereby offering a theoretical foundation for the early prevention and treatment of Hhcy.</div></div><div><h3>Methods</h3><div>Serum samples were collected from 56 individuals with Hhcy and 44 healthy controls. Metabolic alterations in Hhcy were assessed through multi-platform serum metabolomics analyses. Through multivariate statistical analysis and regression modeling, distinct metabolites in the serum were identified, and various metabolic pathways associated with Hhcy were investigated.</div></div><div><h3>Results</h3><div>Our findings revealed 21 significant different metabolites that distinguished Hhcy from healthy controls. These varied metabolites primarily comprised 10 organic acids, 4 amino acids, 2 fatty acids, and 5 other metabolites. The key differential metabolic pathways identified were the TCA cycle, pyruvate metabolism, arginine biosynthesis, as well as alanine, aspartate, and glutamate metabolism.</div></div><div><h3>Conclusions</h3><div>This study elucidated the variances in metabolic profiles between Hhcy and healthy control groups, highlighting distinct metabolic pathways that may help explain the etiology of Hhcy. These findings offer valuable insights to address the knowledge gaps related to the metabolic alterations associated with Hhcy.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124336"},"PeriodicalIF":2.8,"publicationDate":"2024-10-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142386953","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":"Efficient purification of soluble receptor for advanced glycation end-products from Sus scrofa lung tissue and synthesis of its binding ligand, glycated bovine serum albumin","authors":"Tamás Madarász, Miklós Nyitrai, Edina Szabó-Meleg","doi":"10.1016/j.jchromb.2024.124326","DOIUrl":"10.1016/j.jchromb.2024.124326","url":null,"abstract":"<div><div>A receptor for advanced glycation end products (RAGE) has emerged as a crucial player in various pathological conditions due to its involvement in inflammation and cellular dysfunction. Its soluble isoform, sRAGE, has garnered significant attention for its competitive inhibitory effects and potential therapeutic applications. However, obtaining sRAGE with appropriate glycosylation patterns for binding to glycated proteins has been challenging, often requiring costly expression systems. Here, we present a novel approach for producing and purifying sRAGE from Sus scrofa lungs, bypassing the need for expensive expression systems. Previous protocols for sRAGE extraction faced reproducibility issues due to high viscosity and haemoglobin content of the solution. To address this, we developed a method for selective haemoglobin precipitation using a zinc-containing buffer, enabling purification via various chromatographic methods. Through a combination of chromatographic techniques, we obtained sRAGE in suitable purity, identified using HPLC-MS/MS. Additionally, producing glycated proteins for RAGE receptor activation often involved lengthy protocols or inadequate separation from reactants. Thus, we devised a rapid method for producing and purifying pure BSA glycated with ribose, addressing a critical gap in the field. Functional studies, conducted using Native PAGE, demonstrated the capability of purified proteins to bind to each other.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124326"},"PeriodicalIF":2.8,"publicationDate":"2024-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142379722","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}
Na Zhang , Dong Guo , Na Guo , Dawei Yang , Han Yan , Jingchun Yao , He Xiao , Mingguo Shao , Yongxia Guan , Guimin Zhang
{"title":"Integration of UPLC-MS/MS-based metabolomics and desorption electrospray ionization-mass spectrometry imaging reveals that Shouhui Tongbian Capsule alleviates slow transit constipation by regulating bile acid metabolism","authors":"Na Zhang , Dong Guo , Na Guo , Dawei Yang , Han Yan , Jingchun Yao , He Xiao , Mingguo Shao , Yongxia Guan , Guimin Zhang","doi":"10.1016/j.jchromb.2024.124331","DOIUrl":"10.1016/j.jchromb.2024.124331","url":null,"abstract":"<div><div>Slow transit constipation (STC) is a common intestinal disorder. Some studies reported that Shouhui Tongbian Capsule (SHTB) can effectively mitigate STC symptoms. A detailed understanding of the changes in the endogenous metabolite profile of rats is crucial for a more accurate comprehension of the molecular pathological characteristics of SHTB in treating STC. In the present study, a method integrating metabolomics based on Ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) and Desorption electrospray ionization (DESI)-mass spectrometry imaging (MSI) was proposed to investigate serum, feces and colon tissue metabolic alterations of STC rats induced by diphenoxylate and the effect of SHTB treatment on metabolism. Then, Enzyme-linked immunosorbent assay (ELISA) and Western blot (WB) analysis for verifying the potential mechanism of SHTB in treating STC. As a result, we first indicated that SHTB significantly improved intestinal peristalsis and low fecal water content in STC rats. Furthermore, after treatment with SHTB, the thickness of muscle layers was increased, demonstrated SHTB’s effectiveness in reducing intestinal injury in STC rats. Besides, bile acid (BA) metabolomics based on UPLC-MS/MS revealed significant increase in serum levels of Cholic acid (CA), Deoxycholic acid (DCA), Chenodeoxycholic acid (CDCA), Ursodeoxycholic acid (UDCA), and Glycolithocholic acid (GLCA), whereas the contents of CA and DCA in feces were significantly decreased in STC rats. Nonetheless, they returned to the control levels after the SHTB administration. ELISA results showed that SHTB significantly hindered the excessive reabsorption of BAs by inhibiting apical sodium-dependent bile acid transporter (ASBT), organic solute transporter alpha (OSTα) and organic solute transporter beta (OSTβ) in the ileum tissue of STC rats. Furthermore, the DESI-MSI analysis revealed that SHTB remarkably enhanced DCA in the colon tissue of STC rats. The WB results indicated that SHTB reinstated Takeda G-protein–coupled receptor 5 (TGR5) expression, a receptor for BAs and a key regulator of colonic motility. Consequently, DCA exerted its effects on TGR5, leading to the promotion of colonic motility. This study provided more comprehensive and detailed information about the BA metabolomics in the serum, feces and colon of STC rats. These findings highlighted the promising potential of metabolomics based on UPLC-MS/MS and DESI-MSI method for application in the study of STC diseases.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124331"},"PeriodicalIF":2.8,"publicationDate":"2024-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142379723","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}
Alpeshkumar Kachhadia, Therese Burkhardt, Gerhard Scherer, Max Scherer, Nikola Pluym
{"title":"Development of an LC-HRMS non-targeted method for comprehensive profiling of the exposome of nicotine and tobacco product users – A showcase for cigarette smokers","authors":"Alpeshkumar Kachhadia, Therese Burkhardt, Gerhard Scherer, Max Scherer, Nikola Pluym","doi":"10.1016/j.jchromb.2024.124330","DOIUrl":"10.1016/j.jchromb.2024.124330","url":null,"abstract":"<div><div>The global prevalence of electronic cigarettes, heated tobacco products, and other smokeless alternatives has grown significantly in the last ten years. These products have been suggested as combustion-free alternatives for conventional tobacco products like cigarettes, aiming to reduce the negative health impacts associated with smoking. However, the impact of those products on the health and safety of the general population are still unclear, as the absolute exposure from those products has not been thoroughly studied, yet. In this project, a non-targeted LC-HRMS method was developed comprising four different analytical modes for the investigation of the exposure profile in urine of the product users. The method is characterized by its high sensitivity and reproducibility, as shown during method validation. As a proof of concept, we first applied this method to detect significant differences in biomarkers of exposure (BoEs) between smokers and non-smokers. We observed a total of 171 BoEs significantly elevated in smokers, including several well-known biomarkers of smoke exposure like nicotine and its metabolites, mercapturic acid derivatives, and phenolic compounds. Some of the detected biomarkers are present at low ng/mL concentrations in urine, proving the high sensitivity needed for a holistic exploration of the exposome. Moreover, we were able to identify BoEs that have not been reported previously for smoking, such as 2,6-dimethoxyphenol and 7-methyl-1-naphthol glucuronide.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124330"},"PeriodicalIF":2.8,"publicationDate":"2024-09-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142374847","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}
Abdulfataah A.A. Mohamed , Peter Walland , Jasper Stevens , Marco van Londen , Hiddo J.L. Heerspink , Ron T. Gansevoort , Nico C. van de Merbel
{"title":"A validated LC-MS/MS method for the simultaneous quantification of iothalamate and hippuran in serum and urine for non-radioactive kidney function assessment","authors":"Abdulfataah A.A. Mohamed , Peter Walland , Jasper Stevens , Marco van Londen , Hiddo J.L. Heerspink , Ron T. Gansevoort , Nico C. van de Merbel","doi":"10.1016/j.jchromb.2024.124329","DOIUrl":"10.1016/j.jchromb.2024.124329","url":null,"abstract":"<div><div>A novel liquid chromatography-tandem mass spectrometry method is described for the quantitative determination of the kidney function markers iothalamate and hippuran in human serum and urine. It is based on protein precipitation with methanol followed by dilution of the supernatant for serum and simple dilution for urine. The polar analytes are chromatographically separated by a 6.5-min gradient on a low-ligand density reversed-phase column; detection is performed by electrospray ionization tandem mass spectrometry in the positive ion mode against stable-isotope labeled internal standards.</div><div>The results of a thorough method validation show that iothalamate and hippuran can be simultaneously quantified in the concentration ranges 0.500–30.0 ng/mL and 10.0–5000 ng/mL for serum and urine, respectively, with values for CV and absolute bias not exceeding 10 %, and with sufficient stability in all relevant matrices and solvents. The method was successfully applied for the analysis of serum and urine samples of multiple individuals who received both iothalamate and hippuran.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124329"},"PeriodicalIF":2.8,"publicationDate":"2024-09-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142386952","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}
Mrunal Ingawale , Mohammad Riaz , Yves Durocher , Raja Ghosh
{"title":"An unconventional strategy for purifying recombinant SARS-CoV-2 spike protein","authors":"Mrunal Ingawale , Mohammad Riaz , Yves Durocher , Raja Ghosh","doi":"10.1016/j.jchromb.2024.124328","DOIUrl":"10.1016/j.jchromb.2024.124328","url":null,"abstract":"<div><div>The soluble domain of the trimeric SARS-CoV-2 spike protein is a promising candidate for a COVID-19 vaccine. Purification of this protein from mammalian cell culture supernatant using conventional resin-based chromatography is challenging as its large size (∼550 kDa) restricts its access and mobility within the pores of the resin particles. This reduces binding capacity and process robustness very significantly as extremely low flow rates need to be used during purification. Convection-based ion-exchange membrane chromatography has been found to be suitable in this respect. However, the high ionic strength of mammalian cell culture supernatant makes it difficult to bind this protein on charged membranes without dilution with a suitable buffer. An unconventional strategy involving size-exclusion chromatography as the first step, followed by cation exchange membrane chromatography as the second step is proposed in this paper. In the size exclusion chromatography step, the spike protein is excluded from the pores and can therefore be isolated in the void volume fraction. This step removes small molecule impurities and also serves as a desalting and buffer exchange step, making the partially purified material suitable for the cation exchange membrane chromatography step. The proposed process is variant-independent, fast and scalable and addresses some of the challenges associated with the currently used purification methods.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124328"},"PeriodicalIF":2.8,"publicationDate":"2024-09-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142370544","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}
Bharti Jain , Rajeev Jain , Abuzar Kabir , Nemat Ali , Mohammad Rashid Khan , Shweta Sharma
{"title":"Greener analysis of eleven basic drugs in blood and urine using carbowax 20M based biofluid sampler (BFS) device","authors":"Bharti Jain , Rajeev Jain , Abuzar Kabir , Nemat Ali , Mohammad Rashid Khan , Shweta Sharma","doi":"10.1016/j.jchromb.2024.124327","DOIUrl":"10.1016/j.jchromb.2024.124327","url":null,"abstract":"<div><div>For the first time, a novel biofluid sampler (BFS) and sample preparation device is applied for the analysis of 11 basic drugs (i.e., pheniramine, chlorpheniramine, fluoxetine, tramadol, amitriptyline, ketamine, diazepam, chlordiazepoxide, clozapine, chlorpromazine, dothiepin) in biological matrices (i.e., blood and urine). BFS utilizes advanced, highly effective sorbents derived from sol-gel sorbent coating technology onto cellulose fabric substrate, improving sample collection and retention. BFS has the capability to retain a biological sample from 10 to 1000 µL without requiring any dilution or pre-treatment of the sample. The biological samples were pipetted onto the BFS device and dried at room temperature. Subsequently, adsorbed analytes were back-extracted into 1000 µL of methanol without requiring any imposed external diffusion process and then analyzed by gas chromatography-mass spectrometry (GC-MS). A one-factor-at-a-time (OFAT) screening procedure was used to extensively screen and optimize several parameters, including sample volume, elution time, solvent volume, and solvent type. Under the optimal conditions of the study, the method was found to be linear within the range 0.1–10 µg mL<sup>−1</sup> for both blood and urine. Quantification limits were established for blood samples within the range of 0.072–0.095 μg mL<sup>−1</sup> and for urine samples within the range of 0.050–0.069 μg mL<sup>−1</sup>. The precisions within and between days were less than 7% and 10%, respectively. The target analytes showed good recoveries utilizing the recommended protocol, with ranges of 45.1%–103.4%. Furthermore, the methodology has been effectively implemented in forensic toxicology case work. Moreover, the green characteristics and applicability of the suggested methodology was evaluated using softwares i.e., AGREE and BAGI.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124327"},"PeriodicalIF":2.8,"publicationDate":"2024-09-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142358144","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}
Aysan Changizi Kecheklou , Mohammad Reza Afshar Mogaddam , Saeed Mohammad Sorouraddin , Mir Ali Farajzadeh , Ali Akbar Fathi
{"title":"Thin film microextraction of apixaban from plasma based on the covalent organic framework coated on a mesh prior to liquid chromatography-tandem mass spectrometry","authors":"Aysan Changizi Kecheklou , Mohammad Reza Afshar Mogaddam , Saeed Mohammad Sorouraddin , Mir Ali Farajzadeh , Ali Akbar Fathi","doi":"10.1016/j.jchromb.2024.124302","DOIUrl":"10.1016/j.jchromb.2024.124302","url":null,"abstract":"<div><div>In this research, a new covalent organic framework was synthesized and utilized as a coating in thin film microextraction for the extraction of apixaban from plasma samples. This coating was applied to the mesh modified through immersion in a HF solution. The extracted drug was then analyzed using liquid chromatography-tandem mass spectrometry. By combining the high specific surface area and selectivity of the covalent organic framework, along with integrating the innovative thin film microextraction method and a sensitive analysis system, an efficient analytical approach was achieved. The target analyte was preconcentrated and extracted by immersing of the covalent organic framework-coated mesh as an absorbent into the biological sample. Subsequently, a sonication process was conducted for a specific duration. Following this, the extracted analyte was desorbed using acetonitrile as the elution solvent. The effective parameters of the proposed technique were optimized by using “one-parameter-at-a-time” strategy and the optimal conditions were selected. By integrating the developed method notable achievements were made in the terms of low limits of detection and quantification (0.17 and 0.56 µg/L, respectively), a wide linear range (0.05–250 µg/L), intra- and inter day precisions (with relative standard deviations of ≤14 %), as well as satisfactory extraction recoveries (53 % and 54 % in plasma and deionized water, respectively). Hence, it can be concluded that the introduced technique exhibits high efficiency and reliability when applied to biological samples.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124302"},"PeriodicalIF":2.8,"publicationDate":"2024-09-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142370545","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}