Journal of Chromatography B最新文献

{"title":"Integrated HPLC, pharmacodynamics, and immunoprofiling to explore active components and mechanism of Zhi Bai Heye Fang on glycolipid metabolic disorders in mice","authors":"Yao Li ,&nbsp;Yun-Yuan Tian ,&nbsp;Qian Yang ,&nbsp;Xu Yang ,&nbsp;Juan Wang ,&nbsp;Meng-Meng Zhang ,&nbsp;Yan-Hua Xie ,&nbsp;Jie Li ,&nbsp;Xu-Fang Wang ,&nbsp;Si-Wang Wang","doi":"10.1016/j.jchromb.2024.124446","DOIUrl":"10.1016/j.jchromb.2024.124446","url":null,"abstract":"<div><div>Zhi Bai Heye Fang (AR-PCC-NF) exerts a positive effect on glycolipid metabolic disorders in the clinical setting; however, its efficacy components and mechanisms of action remain unclear. Glycolipid metabolic disorders in mice were used to evaluate the therapeutic effects of AR-PCC-NF and its individual components, and the chemical components of AR-PCC-NF were detected by HPLC. An insulin-resistant cell model was then treated with 12 biological components <em>in vitro</em>, and seven candidate active components were administered to mice with glycolipid metabolic disorders to investigate the efficacy and mechanism of AR-PCC-NF. AR-PCC-NF improved glucolipid metabolism more effectively than did the individual components. The protein expression of INSR and GLUT4 was elevated, and FOXO1 expression and impaired mitochondrial debris in the liver were reduced by AR-PCC-NF. Furthermore, neomangiferin, chlorogenic acid, isomangiferin, 2-hydroxy-1-methoxyaporphine, hyperoside, nuciferine, and berberine improved glucose consumption or T-CHO <em>in vitro</em>. Interestingly, <em>in vivo</em>, neomangiferin, chlorogenic acid, isomangiferin, 2-hydroxy-1-methoxyaporphine, hyperoside, nuciferine, and berberine partially improved abnormal glucolipid metabolism in mice when used separately, but the effects were equivalent to those of AR-PCC-NF when the seven active components were used in combination. Moreover, AR-PCC-NF and its efficacy components upregulated the protein expression of p-AMPK/AMPK and PGC-1α, decreased the levels PPARα, and reduced mitochondrial debris in the liver. In conclusion, neomangiferin, chlorogenic acid, isomangiferin, 2-hydroxy-1-methoxyaporphine, hyperoside, nuciferine, and berberine are the main active components of AR-PCC-NF in the treatment of glycolipid metabolic diseases, and the mechanism is related to the regulation of the AMPK/PGC-1α.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124446"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142926117","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":"Recent research progress on the biological functions, synthesis and applications of selenium nanoparticles","authors":"Chunxia Chen ,&nbsp;Zhan Yang ,&nbsp;Jingjing Ma ,&nbsp;Weiqi Xie ,&nbsp;Zhizeng Wang","doi":"10.1016/j.jchromb.2024.124448","DOIUrl":"10.1016/j.jchromb.2024.124448","url":null,"abstract":"<div><div>Selenium is an essential trace element that is involved in a variety of complex biological processes and has a significant positive effect on the prevention and treatment of cardiovascular disease, inflammatory diseases, and cancer. Selenium in the body is mainly provided by daily meals. However, selenium has two sides, beneficial in moderation and harmful in excess. Selenium nanoparticles (SeNPs), which has better biocompatibility, safety and stability compared with other forms of selenium, is a good choice for selenium supplementing. Current researchers are exploring SeNPs in a variety of ways, including but not limited to antioxidant, antimicrobial, antiviral, inhibition of inflammation, anti-tumor, development of bio-diagnostic reagents, and nano-carrier systems. Also, efforts are being made to synthesize stable and efficient SeNPs for various applications. This study briefly describes how SeNPs are synthesized, summarizes in detail the wide range of uses of SeNPs, and provides an outlook on the future development of it. In addition, combined with the research results of our group, this study discusses the application and biological assays of SeNPs in diagnosis, which will provide inspiration and help for researchers to broaden the application of SeNPs.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124448"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142942173","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":"Preparation of molecularly imprinted polymer nanoparticles for the extraction and purification of progesterone combined with UPLC-ESI-MS mass spectrometry detection in royal jelly","authors":"Hui Li,&nbsp;Xiaoxia Pan,&nbsp;Kaiyue Zhang,&nbsp;Yuxin Guo,&nbsp;Meng Zhang,&nbsp;Zheng Li,&nbsp;Wei Wu","doi":"10.1016/j.jchromb.2025.124462","DOIUrl":"10.1016/j.jchromb.2025.124462","url":null,"abstract":"<div><div>This study aimed to develop molecularly imprinted polymer (MIP) nanoparticles specifically for the selective extraction and enrichment of progesterone (P) from royal jelly (RJ), and quantitatively analyzed them by ultra-performance-liquid chromatography electrospray ionization mass spectrometry (UPLC-ESI-MS). Gaussian software-based theoretical calculations identified methacrylic acid (MAA) as the optimal functional monomer for its strong binding affinity to P. MIP was synthesized by precipitation polymerization, and the preparation process of MIP was optimized by one-way variance design and response surface methodology. The optimal formulation was determined to be 0.26 mmol of P, 0.77 mmol of MAA, and 3.0 mmol of trimethylolpropane trimethacrylate (TRIM). The synthesized MIPs demonstrated a maximum adsorption capacity of 34.41 mg/g. The detection limit of P by mass spectrometry was 1 ng/ml. In RJ samples, P content ranged from 0.02 mg/g to 1.53 mg/g, with an average content of 0.266 mg/g. The study successfully developed a stable and reliable MIP, providing an effective method for the selective enrichment and detection of P in complex samples.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124462"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142997759","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":"Analytical quality by design guided white analytical chemistry driven green in the development of LC-ICP-MS method for arsenic speciation analysis in HEK-293 cells","authors":"Pothuraju Naresh ,&nbsp;Salona Devnath Roy ,&nbsp;Prashant Vilas Pawaskar ,&nbsp;Puja Shamrao Lokhande ,&nbsp;Rahul Laxman Gajbhiye ,&nbsp;Ramalingam Peraman","doi":"10.1016/j.jchromb.2025.124474","DOIUrl":"10.1016/j.jchromb.2025.124474","url":null,"abstract":"<div><div>An analytical quality by design-guided LC-ICP-MS method for simultaneous arsenic speciation analysis in HEK-293 cells was optimized and validated. Initially, critical method variables (CMVs) were identified to achieve the targeted critical quality attribute (CQA) of the analytical target profile (ATP). Based on knowledge and risk assessments, formic acid (X₁), citric acid (X₂), and pH (X₃) were studied for their effect on method responses such as resolutions (Y1, Y2) and retention time of As(V), As(III) and DMA (Y3, Y4, and Y5) using central composite design (CCD). ANOVA analysis indicated that variable interaction was significant in method responses with curvature effect on resolution (Y1 and Y2). The method operable design region (MODR) afforded a 0.1% formic acid, citric acid strength of 20–30 mM, and pH 5.6–6.8 as a robust region for the appropriate method performance. Hence, the final method was optimized on the ZORBAX RRHD SB-Aq column using a mobile phase consisting of 0.1% Formic acid: Citric acid (22.5 mM) (50:50 % v/v; pH 5.6). The optimized method eluted As(V), As(III), and DMA at 2.5 ± 0.1, 2.7 ± 0.1, and 3.1 ± 0.1 min, respectively, with an acceptable resolution. The LOD of the method was 4.78, 3.39, 5.35 ppb respectively for As(V), As(III), and DMA whilst the linearity was established at 30–1000 ppb for all species with respective r²-value of 0.9967, 0.9996, and 0.9972, respectively. The % recovery (77.11–99.64 %) and precision (0.25–1.95 %) were acceptable. The method has proven robust for method variables. Notably, we conducted the Green-white analytical chemistry assessment for the developed method by three different assessment tools viz., AGREES, GAPI, and RGB of 12 algorithms. The developed method demonstrated robustness, environmental friendliness, and user-friendliness.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124474"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143021697","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 and optimization of a high-throughput HPLC-MS/MS method for the simultaneous determination of Cedazuridine, Gemcitabine and its metabolite in mouse plasma","authors":"Qing Yan,&nbsp;Xiaolan Xu,&nbsp;Xiaohua Ran,&nbsp;Chenxia Bai,&nbsp;Qikun Jiang,&nbsp;Tianhong Zhang","doi":"10.1016/j.jchromb.2024.124436","DOIUrl":"10.1016/j.jchromb.2024.124436","url":null,"abstract":"<div><div>Gemcitabine (GEM) has been extensively applied in treating various solid tumors. Nonetheless, GEM is easily metabolized <em>in vivo</em> by cytidine deaminase (CDA) to inactive 2′, 2′-Difluorodeoxyuridine (dFdU) results in a low oral bioavailability, which limit its clinical application. It was found that Cedazuridine (CDZ) could effectively inhibit the deamination of the drug by CDA, and its combination with GEM might affect the oral bioavailability of GEM. To investigate the effect of CDZ on the bioavailability and metabolism of GEM after oral administration, an HPLC-MS/MS method was developed for the simultaneous determination of CDZ, GEM, and its metabolite dFdU in mouse plasma. The separation of CDZ, GEM and dFdU was performed on an acetonitrile and water containing 0.1 % formic acid in isocratic elution on a COSMOSIL® 5C18-PAQ packed column (150 × 4.6 mm, 2.6 µm). The three analytes and the internal standard were determined in a multiple reaction monitoring (MRM) mode under positive ion conditions. The three analytes showed good linearity in the range of 5–10,000 ng/mL, and all quality control samples showed good precision and accuracy. The method was successfully applied to the pharmacokinetic study of GEM with CDZ. The results showed that CDZ significantly improved the oral bioavailability of GEM by reducing the metabolism of CDA to GEM in mice, which will provide a reference for the combined application of GEM and CDZ in clinical therapy.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124436"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142926113","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":"Liquid chromatography coupled with high resolution mass spectrometry reveals the inhibitory effects of Huangkuisiwu formula on biosynthesis of protein-binding uremic toxins in rats with chronic kidney disease","authors":"Jianping Li ,&nbsp;Yumeng Wang ,&nbsp;Chengxi Li ,&nbsp;Jinao Duan ,&nbsp;Jianjing Liu ,&nbsp;Jianming Guo","doi":"10.1016/j.jchromb.2024.124445","DOIUrl":"10.1016/j.jchromb.2024.124445","url":null,"abstract":"<div><div>Chronic kidney disease (CKD) is recognized as a common disorder worldwide. Protein-binding uremic toxins that cannot be efficiently removed by extracorporeal renal replacement therapies, such as indoxyl sulfate (IS) and p-cresyl sulfate (PCS), are associated with high risks of cardiovascular complications and high mortality in CKD population. This study aimed to explore the therapeutical effects of Huangkuisiwu formula (HKSWF) on CKD rats. Moreover, the underlying mechanisms of HKSWF to inhibit the biosynthesis of IS and PCS were studied. Untargeted metabolomics based on UHPLC-QTOF/MS was conducted to analyze the alterations of endogenous metabolites in plasma. Levels of IS and PCS in plasma and peripheral tissues, as well as levels of amino acids in colonic contents were analyzed by UHPLC-TQ/MS. Levels of indole and p-cresol, the precursors of IS and PCS, in feces and colonic contents were quantified by HPLC-FLD. mRNA and protein expression of sulfotransferase 1 a1 (SULT1A1) were determined by qPCR and Western blotting, respectively. The ability of colonic microbiota to metabolize amino acids into precursors, as well as the activity of sulfotransferase to catalyze precursors into uremic toxins were evaluated by detecting corresponding products from specific substrates. 16S rRNA sequencing were conducted to analyze the profile of gut microbiota. The results showed that HKSWF significantly alleviated the structural and functional impairment of kidney, as well as improved the global metabolic disorders in CKD rats. IS and PCS were identified as the key differential metabolites that contributed to the effects of HKSWF. HKSWF significantly reduced the levels of IS and PCS in plasma, kidney, liver and heart of CKD rats. HKSWF showed no significant effects on the expression of SULT1A1 or the activity of sulfotransferase. HKSWF significantly decreased the levels of indole and p-cresol in the colonic contents and feces of CKD rats, by inhibiting the ability of colonic microbiota to metabolize tryptophan and tyrosine into indole and p-cresol. Alterations in the profile of amino acids and gut microbiota in CKD rats were significantly improved by HKSWF treatment. Conclusively, HKSWF inhibited gut-microbiota mediated biosynthesis of indole and p-cresol, to alleviate the accumulation of IS and PCS in CKD rats.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124445"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142918849","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":"Qualitative confirmation of 30 phencyclidine analogs in human blood and urine using GC-HRMS and a self-built library search","authors":"Zixuan Song ,&nbsp;Zhenshuo Guo ,&nbsp;Yiling Tang ,&nbsp;Miao Zhang ,&nbsp;Ping Xiang ,&nbsp;Wei Liu ,&nbsp;Hui Yan","doi":"10.1016/j.jchromb.2025.124464","DOIUrl":"10.1016/j.jchromb.2025.124464","url":null,"abstract":"<div><h3>Introduction</h3><div>Phencyclidine, a dissociative anesthetic with hallucinogenic effects, is commonly abused as a recreational drug. Phencyclidine analogs are compounds produced by substitutions of the phenyl and piperidine rings of phencyclidine. Illegal use of phencyclidine and its analogs has symptoms such as addiction, confusion, and increased tendencies toward violence. In this study, a novel high-throughput screening method was applied for GC-HRMS identification of 30 phencyclidine analogs in human blood and urine. Methods: After a simple extraction with ethyl ether and buffer, followed by centrifugation, the supernatant was injected into the system. Analytes were identified using a self-built library and searching against reference spectra. Phencyclopiperidine analogs in the samples were identified, and isomers were differentiated using the exact molecular mass and retention time (RT) of the characteristic fragment ions. Results: The method was fully validated, no exogenous or endogenous interferences were observed, and recovery ranged from 30 % to 123 %. The more than 100 % recovery of DMXE, HXE, ketamine, and Cl-634 may be due to matrix-induced response enhancement. The limits of detection ranged from 0.05 to 5 ng/mL. The analytical method was successfully applied for separation of three groups of isomers: 2-FDCK and 4-FDCK; 3-MeO-PCP, 4-MeO-PCP and 4-MeOH-PCP; and PCMPA and PCEEA. This analytical approach was successfully applied for the identification of phencyclidine analogs in blood and urine samples from 800 authentic forensic cases. Four phencyclidine analogs were detected—2-F-2-oxo-PCE, 3-MeO-PCE, O-PCE, and 2-FDCK—demonstrating the method’s suitability for sensitive and fast high-throughput screening of drugs in human blood and urine samples.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124464"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142982199","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":"Bioanalysis of protein-unbound prednisolone in serum using equilibrium dialysis followed by liquid chromatography-tandem mass spectrometry","authors":"J.E. Möhlmann ,&nbsp;M. van Luin ,&nbsp;E.G.W.M. Lentjes ,&nbsp;A.D.R. Huitema ,&nbsp;A.M. Punt","doi":"10.1016/j.jchromb.2024.124440","DOIUrl":"10.1016/j.jchromb.2024.124440","url":null,"abstract":"<div><h3>Introduction</h3><div>High-dose systemic prednisolone is the cornerstone treatment of many autoimmune- and inflammatory diseases. Since prednisolone shows non-linear protein binding at higher serum concentrations, quantification of the unbound prednisolone concentration is important to understand prednisolone pharmacokinetics. We developed a liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay to quantify protein-unbound prednisolone in serum.</div></div><div><h3>Methods</h3><div>Protein-unbound prednisolone was obtained using an equilibrium dialysis technique. Prednisolone was extracted from the dialysate using methyl <em>tert</em>-butyl ether. After evaporation to dryness, the organic phase residue was reconstituted and ready for injection onto the LC-MS/MS. Prednisolone was analysed by selected reaction monitoring with MS/MS operating in positive ion mode.</div></div><div><h3>Results and discussion</h3><div>The equilibrium between bound and unbound prednisolone was stable after 24 h. The calibration model for prednisolone in serum ranged from 0.25 to 811 µg/L and had an average linearity of 0.998. The coefficient of variation (CV) for precision at the lower limit of quantification was ≤ 4.3 % and for the other quality control samples ≤ 7.8 %. Prednisolone protein binding showed no significant degradation after 30 months of storage at −80 °C and was not influenced by multiple cycles of freezing and thawing. The recovery for the tested matrix effects in serum ranged from 85 % to 115 % (CV 10.3 %) and throughout the validation, no carry-over was observed.</div></div><div><h3>Conclusion</h3><div>An LC-MS/MS assay for prednisolone in serum was developed and validated, with a successful equilibrium dialysis technique to obtain protein-unbound prednisolone prior to quantification. This assay is considered suitable for pharmacokinetic studies.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124440"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142913459","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":"Development and validation of a UPLC–MS/MS method for simultaneous quantification of polymyxins and caspofungin in human plasma for therapeutic drug monitoring","authors":"Tong Wu ,&nbsp;Libin Pu ,&nbsp;Wenqing Liu ,&nbsp;Yinliang Bai ,&nbsp;Jingjing Ma ,&nbsp;Xia Song ,&nbsp;Aijia Cao ,&nbsp;Shunli Pan ,&nbsp;Jiahui Yang ,&nbsp;Chang Wang ,&nbsp;Wen Qiu","doi":"10.1016/j.jchromb.2025.124465","DOIUrl":"10.1016/j.jchromb.2025.124465","url":null,"abstract":"<div><h3>Objective</h3><div>To develop a rapid, convenient, accurate, and low-residual-effect ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method for the determination of polymyxin B sulfate and colistin sulfate in the blood of patients with multidrug-resistant bacterial infections, as well as caspofungin acetate in the blood of patients with fungal infections, thus facilitating the rational use of antibiotics in clinical applications.</div></div><div><h3>Methods</h3><div>All analytes were diluted with 0.2 % aqueous formic acid, and plasma proteins were precipitated using acetonitrile. The selected reaction monitoring (SRM) mode was used for measurement. Separation of all analytes was completed on a Hypersil GOLD C18 column (100 × 2.1 mm, 3.0 µm). They were quantitatively analyzed using electrospray ionization on a triple quadrupole mass spectrometer in the positive ion mode. The mobile phase consisted of water (containing 0.1 % formic acid) and acetonitrile, which was delivered by gradient elution at a flow rate of 0.3 ml/min. The internal standard was bacitracin zinc (BcZn), and the column temperature was maintained at 25 °C. The runtime for each analysis was 3.5 min.</div></div><div><h3>Results</h3><div>The procedure was validated following the recommendations of the U.S. Food and Drug Administration, which included measurements of accuracy (ranging from 83.27 % to 105.86 % for within-run and between-run accuracy), precision (with coefficients of variation from 2.50 % to 16.51 % for within-run precision and between-run precision), and matrix effects (ranging from 88.65 % to 103.94 %). The extraction recoveries ranged from 38.01 % to 42.76 for polymyxin B1 (PMB1), polymyxin B2 (PMB2), polymyxin E1 (PME1), polymyxin E2 (PME2), and 88.65 % to 89.84 % for caspofungin (CPF). Plasma samples were stable under various storage conditions, including three freeze–thaw cycles at −80 °C, 24-hour periods at room temperature and 4 °C, and 30 days of freezing at both −20 °C and −80 °C, with relative standard deviations (RSD) of less than 15 %.</div></div><div><h3>Conclusion</h3><div>In this study, a UPLC–MS/MS method was developed to simultaneously quantify PMB1, PMB2, PME1, PME2, and CPF in human plasma. The method was validated in blood samples from patients with multidrug-resistant bacteria combined with fungal infections and is suitable for therapeutic drug monitoring.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124465"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142997692","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":"Unraveling the in vivo pharmacokinetic behavior of mPEG5-NH2 polymer in rats by UHPLC-MS/MS assay","authors":"Yingxia Guo ,&nbsp;Meichen Liu ,&nbsp;Jiye Tian ,&nbsp;Chunpeng Feng ,&nbsp;Qingbin Wang ,&nbsp;Xuan Zhao ,&nbsp;Lei Yin","doi":"10.1016/j.jchromb.2025.124460","DOIUrl":"10.1016/j.jchromb.2025.124460","url":null,"abstract":"<div><div>As an important chemical reagent, methoxy polyethylene glycol amine (mPEG-NH₂) is widely used in biomedical field. Unraveling the pharmacokinetic behavior of mPEG-NH₂ polymers is essential for revealing the toxicity and efficiency of mPEG-NH₂ related drug delivery systems. In this study, a simple analytical assay based on mass spectrometry (MS) was first established and validated for quantification of mPEG₅-NH₂ in biological matrix. The multiple reaction monitoring (MRM) transitions at <em>m</em>/<em>z</em> 252.2 (precursor ions) → 87.7 (fragment ions) and <em>m</em>/<em>z</em> 371.2 (precursor ions) → 89.2 (fragment ions) were chosen to determine mPEG₅-NH₂ and OH-PEG₈-OH, respectively. The UHPLC-MS/MS assay showed excellent linearity over the range of 0.01–10 μg/mL. Intra-day and inter-day accuracies and precisions of the assay were all within ± 6.44 %. The analytical assay was successfully applied to reveal the <em>in vivo</em> pharmacokinetic behavior of mPEG₅-NH₂ in rats.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124460"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142997760","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}