Journal of Chromatography B最新文献

{"title":"The optimization and validation of a gas chromatography-mass spectrometry method to analyze the concentration of acetate, propionate and butyrate in human plasma or serum","authors":"Greet Vandermeulen,&nbsp;Riet Rosseel ,&nbsp;Georgia Chatonidi,&nbsp;Lise Deroover ,&nbsp;Eef Boets ,&nbsp;Kristin Verbeke","doi":"10.1016/j.jchromb.2024.124299","DOIUrl":"10.1016/j.jchromb.2024.124299","url":null,"abstract":"<div><p>Fermentation-derived short-chain fatty acids (SCFA)<span><span>⁴</span></span> are potential mediators of the health benefits associated with dietary fiber intake. SCFA affect physiological processes locally in the gut and on distant organs via the systemic circulation. Since SCFA are used as energy source for colonocytes and substrate for the liver metabolism, their concentrations in the systemic circulation are low. Therefore, quantification of systemic SCFA requires sensitive analytical techniques. This article covers the optimization and validation of a gas chromatography-mass spectrometry method to measure systemic SCFA concentrations following derivatization with 2,4-difluoroaniline (DFA)<span><span>⁵</span></span> and extraction in ethyl acetate. Sample preparation was optimized by varying the amount of DFA, coupling agent 1,3-dicyclohexylcarbodiimide, ethyl acetate and sodium bicarbonate, which is used to quench derivatization. In addition, evaporation of the samples using a vacuum concentrator resulted in less contamination, notably of acetate, compared to drying with N₂ gas. The method showed excellent linearity with coefficient of variation (R²) &gt; 0.99 and a good precision (relative standard deviation &lt; 20 %) and accuracy. Finally, systemic concentrations of SCFA in human plasma samples could successfully be determined.</p></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124299"},"PeriodicalIF":2.8,"publicationDate":"2024-09-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142173102","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":"Development of a simple and reproducible HPTLC method on protective effect induced by bark of Acacia nilotica on poisoning caused by use of nicotine containing tobacco products","authors":"Avijit Jha ,&nbsp;Arun K.S. Parihar ,&nbsp;Umakant Sahu ,&nbsp;Yuvraj Kaushik ,&nbsp;S.R. Inchulkar ,&nbsp;N.S. Chauhan","doi":"10.1016/j.jchromb.2024.124295","DOIUrl":"10.1016/j.jchromb.2024.124295","url":null,"abstract":"<div><p>Tobacco <em>(Nicotiana tobacum</em>) and tobacco products are the most critical public health challenges today across the globe. Nicotine is the main chemical composition of tobacco and is associated with withdrawal syndrome. A laboratory animal is commonly employed as a model to investigate nicotine toxicity, drug dependence, reinforcing effects, and the protective effects of samples against nicotine-induced toxicity. The first in-vitro model was developed to prove the protective effect of Babbul (<em>Acacia<!--> <!-->nilotica Linn</em>.) against nicotine poisoning caused by consumption of tobacco products. The HPTLC method for estimating the protective effect against nicotine poisoning was performed by taking the solvent systems dichloromethane, methanol, and liquid ammonia (25 %)(9:1:0.04v/v/v). This in-vitro approach was done by treating the bark of the <em>Acacia nilotica</em> extract with a standard solution of nicotine, which reduced the concentration of nicotine by 39.12 %. The prescribed HPTLC method can be used successfully to assess <em>Acacia nilotica’s</em> protective impact against nicotine toxicity caused by intake of nicotine containing tobacco products.</p></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124295"},"PeriodicalIF":2.8,"publicationDate":"2024-09-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142167828","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":"Multivariate approach to assess the bioactive compounds of Atractylodes chinensis (DC.) Koidz in different harvest periods","authors":"Xiaokang Liu ,&nbsp;Liwen Liang ,&nbsp;Guangzhi Cai ,&nbsp;Yunlong Guo ,&nbsp;Jiyu Gong","doi":"10.1016/j.jchromb.2024.124298","DOIUrl":"10.1016/j.jchromb.2024.124298","url":null,"abstract":"<div><h3>Background</h3><p>The <em>Atractylodes chinensis</em> (DC.) Koidz (<em>A. chinensis</em>) Chinese herb possesses numerous therapeutic properties and is extensively utilized in the pharmaceutical industry. Its quality is closely associated with the harvest periods. However, the optimal quality and harvest periods of <em>A. chinensis</em> remain elusive.</p></div><div><h3>Methods</h3><p>The bioactive compounds of perennial <em>A. chinensis</em> were detected by ultra-high-performance liquid chromatography coupled with quadrupole Orbitrap mass spectrometry (UHPLC-Q-Orbitrap/MS) metabolomics, and differentially abundant compounds were selected by multivariate statistical analysis. Then, variations in the content of differential compounds in samples harvested at different periods were analyzed, while correlation analysis was carried out on the differential compounds to determine the suitable harvest period for distinct components.</p></div><div><h3>Results</h3><p>A total of 61 bioactive compounds were detected in all samples, grouped into 9 known classes. The results revealed that the chemical compositions of <em>A. chinensis</em> at different harvest periods were significantly different. The volatile oil content in the four-year-old and five-year-old samples was relatively high, at 31.92 mg/g and 32.42 mg/g, respectively. There were also significant differences in the content of the six active ingredients, for example, the five-year-old sample had the highest content of atractylodin (4.38 mg/g). Indeed, the harvest period was correlated with the abundance of most bioactive compounds. Specifically, quinquennial samples were significantly negatively correlated with the abundance of organic acids and aliphatics while moderately positively correlated with the abundance of other classes of bioactive compounds.</p></div><div><h3>Conclusions</h3><p>According to the results, the ideal harvest time for atractylenolide Ⅲ was 3 years. Regarding organic acids, the optimal harvest time was around 2–3 years. Taken together, these results offer valuable insights to producers for optimizing the harvest period for <em>A. chinensis</em>.</p></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1246 ","pages":"Article 124298"},"PeriodicalIF":2.8,"publicationDate":"2024-09-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142151421","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":"Synthesis and characterization of the trans- and cis-isomers of N-acetyl-S-(4-hydroxy-2-buten-1-yl)-L-cysteine and their attempted detection in human urine","authors":"Fei Yang ,&nbsp;Yi-Yi Cao ,&nbsp;Jing Xi ,&nbsp;Yang Luan ,&nbsp;Na Li ,&nbsp;Xin Dong ,&nbsp;Xin-Yu Zhang","doi":"10.1016/j.jchromb.2024.124294","DOIUrl":"10.1016/j.jchromb.2024.124294","url":null,"abstract":"<div><p>1,3-Butadiene (BD) is a carcinogenic air pollutant. <em>N</em>-acetyl-<em>S</em>-(4-hydroxy-2-buten-1-yl)-L-cysteine (MHBMA3 or 4HBeMA), an urinary BD metabolite with unspecified configuration, is considered the most sensitive BD biomarker and has been used in routine biomonitoring since 2012. However, two issues remain unaddressed: why its concentrations are unusually high relative to other urinary BD biomarkers and why some authors reported no detection of the biomarker whereas other authors readily quantitated it. To address the issues, we synthesized and structurally characterized the authentic <em>trans</em>- and <em>cis</em>-isomers of MHBMA3 (designated NE and NZ, respectively), developed an isotope-dilution LC-MS/MS method for their quantification, and examined 67 urine samples from barbecue restaurant personnel (n = 47) and hotel administrative staff (n = 20). The restaurant personnel were exposed to barbecue fumes, which contain relatively high concentrations of BD. The results showed that NE and NZ had highly similar NMR spectra, and were difficult to be well separated chromatographically. The NMR data showed that the MHBMA3 isomer investigated in most previous studies was NE. We did not detect NE and NZ in any samples; however, an interfering peak with varying heights was observed in most samples. Notably, under the chromatographic conditions used in the literature, the peak exhibited indistinguishable retention time from that of NE. Thus, it is highly likely that the interfering peak has been mis-identified as NE in previous studies, providing a reasonable explanation for the high MHBMA3 concentration in urine. The contradiction in the presence of MHBMA3 in urine was also caused by the mis-identification, because the researchers who reported the absence of MHBMA3 were actually detecting NZ. Thus, we clarified the confusion on MHBMA3 in previous studies through correctly identifying the two MHBMA3 isomers. The presence of NE and NZ in human urine warrants further investigations.</p></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1246 ","pages":"Article 124294"},"PeriodicalIF":2.8,"publicationDate":"2024-09-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142151515","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":"Transformation of 17β-estradiol to estrone by unknown wild-type enzyme in commercial arylsulfatase from Helix pomatia","authors":"Jun Zhang ,&nbsp;Ze-hua Liu ,&nbsp;Ke-meng Zhao ,&nbsp;Zhi Dang ,&nbsp;Yun Liu ,&nbsp;Yu Liu","doi":"10.1016/j.jchromb.2024.124293","DOIUrl":"10.1016/j.jchromb.2024.124293","url":null,"abstract":"<div><p>This work for the first time reported the complete transformation of 17β-estradiol (E2) to estrone (E1) by unknown wild-type enzyme present in the widely used commercial arylsulfatase derived from <em>Helix pomatia</em>. It was found that acetate could effectively inhibit the unknown enzyme with a half inhibitory concentration (IC₅₀) of 140.9 μM, while phosphate and citrate showed no inhibition. Since the buffer solutions with phosphate and citrate have been used in the enzymatic hydrolysis of natural estrogen conjugates for decades, the transformation of E2 to E1 likely occurred during such procedure, inevitably leading to overestimated E1, but underestimated E2. It was further suggested that acetate should be used to prevent this undesirable transformation during the enzymatic hydrolysis of natural estrogen conjugates.</p></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1246 ","pages":"Article 124293"},"PeriodicalIF":2.8,"publicationDate":"2024-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142137087","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":"Simultaneous determination of Obeticholic acid and its two major metabolites in human plasma after administration of Obeticholic acid tablets using ultra-high performance liquid chromatography tandem mass spectrometry","authors":"Sha Li,&nbsp;Min Yang,&nbsp;Jing-yao Zhang,&nbsp;Chang Liu,&nbsp;Bo-ping Wei,&nbsp;Qiang Wu,&nbsp;Wei-ying Tang,&nbsp;Shi Zeng","doi":"10.1016/j.jchromb.2024.124296","DOIUrl":"10.1016/j.jchromb.2024.124296","url":null,"abstract":"<div><p>Obeticholic acid (OCA), a semisynthetic bile acid derivative, was approved for its therapeutic use in primary biliary cirrhosis. OCA has a enterohepatic circulation and host-gut microbiota metabolic interaction, which produce various metabolites. Such metabolites, especially structural isomers of OCA, together with the need to achieve idea lower limit of quantitation (LLOQ) with minimum matrix interference, bring about significant difficulties to the bioanalysis of OCA. Herein, by applying a combination of solid-phase extraction (SPE) and ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS), we introduced an approach for the bioanalysis of OCA along with its two major metabolites—glyco-OCA (GOA) and tauro-OCA (TOA) in human plasma, the full validation results of which showed excellent performance. The <span><span>quantitative range</span><svg><path></path></svg></span> is 0.2506 ∼ 100.2 ng/mL for OCA, 0.2500 ∼ 100.0 ng/mL for GOA, as well as 0.1250 ∼ 50.00 ng/mL for TOA, respectively. This method was successfully applied to the pharmacokinetic studies in healthy subjects following administration of OCA tablets.</p></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1246 ","pages":"Article 124296"},"PeriodicalIF":2.8,"publicationDate":"2024-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142137088","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":"A proteomics-based study of the mechanism of oxymatrine to ameliorate hepatic fibrosis in mice","authors":"Jing Wu ,&nbsp;Xueqin Jin ,&nbsp;Weihua Li ,&nbsp;Enqi Liu","doi":"10.1016/j.jchromb.2024.124280","DOIUrl":"10.1016/j.jchromb.2024.124280","url":null,"abstract":"<div><h3>Objective</h3><p>This study investigated the protective effect of oxymatrine (OMT) on carbon tetrachloride (CCl₄)-induced hepatic fibrosis in mice and explored its possible targets and signaling pathways.</p></div><div><h3>Methods</h3><p>Male BALB/c mice were randomly divided into blank control, model, positive drug (silymarin), and OMT administration groups, respectively, with 10 mice in each group. Hepatic fibrosis was induced in mice using CCl₄ and the corresponding drug intervention was given. After the final administration, ultrasonography tests, blood tests, and analysis of liver differential proteins using tandem mass tag labeling and liquid chromatography-mass spectrometry were performed.</p></div><div><h3>Results</h3><p>OMT intervention ameliorated CCl₄-induced hepatic fibrosis in mice, significantly reduced serum alanine aminotransferase and aspartate aminotransferase levels, down-regulated the expression of fibrosis factors, such as type IV collagen IV, laminin, type III procollagen III, and alpha-smooth muscle actin, and improved liver function. The results of the proteomic analysis showed that the intervention of OMT significantly down-regulated 130 out of 440 up-regulated proteins and up-regulated 70 out of 294 down-regulated proteins, primarily involving the transient receptor potential (TRP) signaling pathway, the peroxisome proliferator-activated receptors (PPAR) signaling pathway, and the metabolic pathway of arachidonic acid. The main differential proteins involved were Cyp2c37, SCP-2, and Tbxas1. In addition, OMT intervention significantly reversed the expression of sterol carrier protein-2 (SCP2) and upregulated the expression of peroxisome proliferator-activated receptor gamma, Cyp2c37, and transient receptor potential cation channel subfamily V member 1 proteins.</p></div><div><h3>Conclusion</h3><p>OMT inhibited the proliferative capacity of hepatic stellate cells, induced apoptotic properties, and suppressed the development of fibrosis by elevating Cyp2c37/TRP signaling axis activity and upregulating PPAR pathway activity by inhibiting SCP2.</p></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124280"},"PeriodicalIF":2.8,"publicationDate":"2024-08-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142173320","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":"Comprehensive exploration of a traditional Chinese medicinal plant of Magnolia officinalis based on high-coverage mass spectrometry and multidimensional chemical-biological analysis","authors":"Wen-Yu Wang ,&nbsp;Ya-Mei Song ,&nbsp;Jia-Nuo Zhang ,&nbsp;Ming-Yue Zhao ,&nbsp;Wen-Han Pei ,&nbsp;Hui Zhang ,&nbsp;Hai-Bo Yin ,&nbsp;Zhi-Li Xu ,&nbsp;Gui-Zhong Xin ,&nbsp;Ming Xie ,&nbsp;Ting-Guo Kang ,&nbsp;Yue-Hua Chen ,&nbsp;Hui-Peng Song","doi":"10.1016/j.jchromb.2024.124290","DOIUrl":"10.1016/j.jchromb.2024.124290","url":null,"abstract":"<div><p>Magnolia bark is a traditional Chinese medicine used for hypoglycaemia. With the widespread use of Magnolia bark, its resources are facing a serious shortage. To address this issue, a strategy based on high-coverage mass spectrometry (HCMS) and multidimensional chemical-biological analysis (MCBA) was proposed for the comprehensive exploration of <em>Magnolia officinalis</em> which is the main source of Magnolia bark. The strategy is divided into three main steps. In the first step, the stem bark, stem xylem, root bark, root xylem, leaf and rootlet of <em>Magnolia officinalis</em> were comprehensively analyzed using high-coverage mass spectrometry. In the second step, multivariate statistical analysis was used to explore the heterogeneity of the six parts and detect differential chemical components. In the third step, a combination of experimental screening and molecular docking was used to explore α-glucosidase inhibitors from <em>Magnolia officinalis</em>. Multidimensional chemical-biological analysis (MCBA) of <em>Magnolia officinalis</em> was achieved by combining the last two steps. Finally, a total of 103 compounds were identified from the whole plant of <em>Magnolia officinalis</em>. Differential components of stem bark, stem xylem, leaf, root bark, root xylem and rootlet were systematically revealed. A pair of positional isomers, namely magnolol and honokiol, were found to be α-glucosidase inhibitors. The activity of their combination is superior to that of each single compound, indicating that magnolol and honokiol are in a synergistic relationship. This strategy contributes to comprehensive exploitation of functional plants and effective alleviation of resource shortage. This study also provides a research paradigm for other similar traditional Chinese medicinal plants.</p></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1246 ","pages":"Article 124290"},"PeriodicalIF":2.8,"publicationDate":"2024-08-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142087401","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":"Non-target metabolomics unravels the effect and mechanism of Lianpu Drink on spleen-stomach damp-heat syndrome","authors":"Jingbo Yu ,&nbsp;Henan Liu ,&nbsp;Jiarong Xiong ,&nbsp;Shanhe Qu ,&nbsp;Xin Xie ,&nbsp;Hongqing Zhao ,&nbsp;Zhengqing Zhu ,&nbsp;Yuhong Wang ,&nbsp;Yue Han","doi":"10.1016/j.jchromb.2024.124281","DOIUrl":"10.1016/j.jchromb.2024.124281","url":null,"abstract":"<div><h3>Background</h3><p>Lianpu Drink (LPY) is a classic prescription for treating spleen-stomach damp-heat syndrome (SSDHS), known for its ability to clear heat and eliminate dampness. However, the underlying mechanisms of LPY in treating SSDHS remain unclear.</p></div><div><h3>Objectives</h3><p>This study aims to use non-target metabolomics to unravel the effects and mechanisms of LPY on SSDHS.</p></div><div><h3>Methods</h3><p>A metabolomics technique based on ultra-high-performance liquid chromatography-tandem quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS) was used to identify the endogenous small-molecule metabolites in the urine of SSDHS model rats and find the metabolites associated with the LPY treatment of SSDHS. Furthermore, a network pharmacological analysis and molecular docking experiments were used to screen and validate the key metabolic pathways regulated by LPY.</p></div><div><h3>Results</h3><p>LPY exerted therapeutic effects on SSDHS by increasing the levels of motilin and gastrin, reducing the rectal temperature, alleviating the pathological changes in gastric and colonic tissues, and regulating the metabolic pattern in SSDHS rats. A total of 25 different metabolites, including L-histidine, citric acid and isocitric acid, were identified as the potential biomarkers for SSDHS via metabolomics. Among them, 11 metabolites were substantially reversed by LPY, including L-histidine, citric acid, isocitric acid, pantothenic acid, homovanillic acid sulfate, hippuric acid, indole-3-carboxilic acid-O-sulphate, 6-hydroxy-5-methoxyindole glucuronide, 2-phenylethan-ol glucuronide, 3-hydroxydodecanedioic acid and 3-methoxy-4-hydroxy-phenylethyleneglyclol sulfate. The results of network pharmacological analysis and molecular docking experiments validated that LPY ameliorated SSDHS by regulating the citrate cycle and histidine metabolism.</p></div><div><h3>Conclusion</h3><p>We preliminarily investigated the effects and mechanisms of LPY on SSDHS at the level of endogenous small-molecule metabolites. Furthermore, this study provides a novel perspective for objectively evaluating the therapeutic effects, and exploring the mechanisms of Chinese medicinal formulas on SSDHS.</p></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1246 ","pages":"Article 124281"},"PeriodicalIF":2.8,"publicationDate":"2024-08-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S1570023224002903/pdfft?md5=0f1f6c6c7de10fdc1a3526d7db13d1da&pid=1-s2.0-S1570023224002903-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142078026","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":"Quantification of florfenicol and its metabolites in fillets of Nile tilapia: Synthesis of metabolites and validation of an on-line solid-phase extraction-ultra high-performance liquid chromatography-tandem mass spectrometry method","authors":"Anna Paula Rocha de Queiroga ,&nbsp;Gabriela Freitas Pereira de Souza ,&nbsp;Inácio Mateus Assane ,&nbsp;Thiago Messias ,&nbsp;Fabiana Pilarski ,&nbsp;Michael Schloter ,&nbsp;Airton Gonçalves Salles Jr. ,&nbsp;Susanne Rath","doi":"10.1016/j.jchromb.2024.124282","DOIUrl":"10.1016/j.jchromb.2024.124282","url":null,"abstract":"<div><p>This study concerns the synthesis of the florfenicol (FF) metabolites florfenicol amine (FFA), florfenicol alcohol (FFOH), and monochloroflorfenicol (FFCl), for their subsequent use as reference standards in On-line solid-phase extraction-ultra high-performance liquid chromatography-tandem mass spectrometry (SPE-UHPLC-MS/MS) analysis. The metabolites were characterized using ¹H and ¹³C NMR, as well as HRMS, and their purities were confirmed by quantitative NMR to ensure analytical reliability. Validation of the developed analytical method showed that it presented acceptable performance, with linearity &gt;0.99 for all the target analytes, accuracies within ±10 % of nominal concentrations, and intra- and inter-day precisions within 15 %. Application of this method to fillets from fish that had been treated with florfenicol (dose of 10 mg/kg bw daily) demonstrated its effectiveness in consistently detecting FF and its metabolites throughout the treatment. The results emphasized the utility of the method for enhancing pharmacokinetic and residue depletion research. The ability to precisely monitor the drug and its metabolites in treated fish provides important insights into florfenicol metabolism, laying the groundwork for further comprehensive profiling studies of metabolites in fish tissue.</p></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1246 ","pages":"Article 124282"},"PeriodicalIF":2.8,"publicationDate":"2024-08-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142087403","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}