Journal of Chromatography B最新文献

{"title":"Method development and validation on RP-HPLC method for estimation of xanthohumol in nanostructured lipid carriers drug delivery systems","authors":"Shubham Singh ,&nbsp;Himani Sharma ,&nbsp;Vijay Kumar ,&nbsp;Gaurav Gupta ,&nbsp;Samir Patel ,&nbsp;Archita Patel ,&nbsp;Kamal Dua ,&nbsp;Sachin Kumar Singh","doi":"10.1016/j.jchromb.2024.124437","DOIUrl":"10.1016/j.jchromb.2024.124437","url":null,"abstract":"<div><div>Xanthohumol(Xn) is isolated from female inflorescences of <em>Humulus lupulus</em>. It has been discovered that Xn and its formulation are useful in the treatment of cancer. As this bioactive compound has medicinal importance, hence, a novel, precise, and sensitive HPLC method should be developed. In the present study, an RP-HPLC method has been developed and validated as per ICH Q2(R1) guidelines using column C18 having particle size 5 µm and dimension 250 × 4.6 mm. The detection wavelength (λ) used was 370 nm. The mobile phase consisted of a combination of HPLC grade Methanol and HPLC grade water buffer at a ratio of 95:5 v/v, with a flow rate of 1.0 mL/min. The total run time was 10 min with Xn retention time (Rt) at 4.5 min. The calibration plot was found linear in the range 2–10 μg/mL. The recovery of 97.65 % indicated good accuracy of method. The method’s precision is within 2 % of acceptable limits. LOD and LOQ values of 0.85 and 2.6 μg/mL indicated good sensitivity of method. The uniqueness of the research work is relying on achieving peak of Xn at lesser retention time as compared to existing methods. Further the results of specificity studies revealed absence of any interference of Xn peak with the excipients used in the nanostructured lipid carriers (NLCs). Overall, the study provided an accurate, precise, sensitive and specific method to quantify Xn in bulk and NLCs.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124437"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142925895","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 validation of a RP-HPLC method for simultaneous determination of cimetidine, metoprolol tartrate and phenol red for intestinal perfusion studies","authors":"Meryem Ermis ,&nbsp;Fatma Kir ,&nbsp;Selma Sahin","doi":"10.1016/j.jchromb.2025.124449","DOIUrl":"10.1016/j.jchromb.2025.124449","url":null,"abstract":"<div><div>A new reversed phase high-performance liquid chromatography (RP-HPLC) method, with a short analysis time and easy to apply, was developed for the simultaneous detection of cimetidine (CIM), metoprolol tartrate (MT) and phenol red (PR) for use in intestinal perfusion studies. The analysis was performed with phosphate buffer (pH 5.0, 12.5 mM)-acetonitrile mixture as mobile phase and C₁₈ column (Inertsil ODS-3; 5 µm, 4.6 × 250 mm) as stationary phase. Gradient analysis conditions were used and the acetonitrile ratio in the mobile phase varied from 10 to 50% in 10 min. Total run time for analysis was 10 min and the injection volume was 20 µL. Detection of compounds was performed at 207 nm. Under optimum HPLC conditions, retention times were 4.03 min for CIM, 6.99 min for MT and 8.49 min for PR. The method was validated according to ICH Q2 (R1) guideline for specificity, linearity, sensitivity, precision, accuracy, stability and robustness. Developed method was linear and determination coefficients of the calibration curves were 0.9993, 0.9991 and 1.0 for CIM, MT and PR, respectively. The limits of quantification were 6.20, 2.78 and 0.45 μg/mL for CIM, MT and PR, respectively. The precision and accuracy values of the developed analytical method met the ICH Q2 (R1) limits. The applicability of the method was demonstrated by preliminary <em>in-situ</em> intestinal perfusion studies. In conclusion, samples obtained from <em>in-situ</em> intestinal perfusion studies performed to examine the absorption/permeability of CIM, MT, and PR can be analyzed with the developed HPLC method.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124449"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142942171","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 simple HPLC-UV method for monitoring therapeutic adherence in pulmonary arterial hypertension","authors":"Paweł K. Kunicki ,&nbsp;Maciej T. Grymm ,&nbsp;Tomasz Pawiński ,&nbsp;Daniel Szulczyk ,&nbsp;Marcin Waligóra ,&nbsp;Grzegorz Kopeć","doi":"10.1016/j.jchromb.2024.124443","DOIUrl":"10.1016/j.jchromb.2024.124443","url":null,"abstract":"<div><div>A considerable percentage of ineffective treatment in pulmonary arterial hypertension (PAH) may be related to subtherapeutic dosage or non-adherence. The aim of the study was to develop a simple analytical method suitable for plasma determination of selected drugs: riociguat (RIO), bosentan (BOS) and macitentan (MAC) administered to PAH patients. An isocratic HPLC-UV system (Spectra Physics – Shimadzu) with a manual injector (50 μL loop) was applied. Chromatographic analysis was performed using a Suplecosil LC-CN column (150 × 4.6 mm, 5 μm) protected with a Supelguard precolumn at room temperature. The separation was carried out using the mobile phase: CH₃CN:H₂O:0.5 M KH₂PO₄:85 % H₃PO₄ (172:324.2:3.7:0.1, v/v) at a flow rate of 1.8 mL/min. Ethyl acetate (4 mL) was used for 10-min liquid–liquid extraction from 0.4 mL alkalized plasma sample. Detection was performed at λ = 245 nm chosen as a compromise between signal intensity and matrix interference. The analytes were eluted at retention times of 4.4 min (RIO), 5.4 min (BOS), 8.9 min (MAC) and 7.8 min for gallopamil (internal standard, GAL). The method was found linear and calibrated in the ranges: 5–1000 ng/mL for RIO, 10–2000 ng/mL for BOS and 20–2000 ng/mL for MAC, with r² of 0.9991 for RIO, 0.9983 for BOS, and 0.9949 for MAC, respectively. Within the given ranges, the method ensured reliable results with the required precision and accuracy: ≤15 % (≤20 % for LLOQ). There was no significant carryover effect. The method has been successfully used in pilot study on adherence in patients treated for PAH, enabling monitoring of RIO, BOS and MAC. Drug concentrations were assessed in samples taken before (C0) and 3 h after drug administration (C3). For RIO, BOS and MAC, the developed method was suitable for both C0 and C3 samples, allowing steady-state drug determination if used. The presented method can be recommended to laboratories equipped with basic HPLC apparatus as an attractive analytical tool for both TDM and adherence studies.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124443"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142942014","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":"Determination of eldecalcitol in human plasma by SIL-IS UPLC-APCI-MS/MS method for pharmacokinetics study","authors":"Wanyu Wang ,&nbsp;Zhichao Yin ,&nbsp;Pengfei Du ,&nbsp;Jianbang Wu ,&nbsp;Minhui Wang ,&nbsp;Yaqin Wang ,&nbsp;Ping Wu ,&nbsp;Xiaocui Xia ,&nbsp;Lin Zhang ,&nbsp;Yamin Liu ,&nbsp;Zhenyue Gao ,&nbsp;Jie Shen ,&nbsp;Yuanwei Jia","doi":"10.1016/j.jchromb.2025.124468","DOIUrl":"10.1016/j.jchromb.2025.124468","url":null,"abstract":"<div><div>Eldecalcitol is a novel analog of 1α,25-dihydroxyvitamin D₃ [1,25(OH)₂D₃] for the treatment of patients with osteoporosis. A highly sensitive and specific ultra-performance liquid chromatography coupled to atmospheric pressure chemical ionization tandem mass spectrometry (UPLC-APCI-MS/MS) technique featuring a lower limit of quantitation (LLOQ) as low as 5 pg/ml, has been established and validated for the rapid and accurate quantification of eldecalcitol in human plasma samples. Plasma samples were extracted by solid phase extraction (SPE). Stable isotope-labeled compound eldecalcitol-d6 was used as an internal standard (SIL-IS). The detection process was carried out utilizing Multi-Reaction Monitoring (MRM) mode, employing an atmospheric pressure chemical ionization (APCI) source operating in the positive ion modality. The target fragment ion pairs for eldecalcitol and SIL-IS were identified as <em>m</em>/<em>z</em> 508.6 transitioning to 397.4, and <em>m</em>/<em>z</em> 514.6 transitioning to 403.3, respectively. This method was validated regarding selectivity, LLOQ, linearity, accuracy and precision, recovery, matrix effects, dilution reliability, stability, carryover test, and incurred sample reanalysis (ISR). This methodology had been successfully employed to assess the pharmacokinetics (PK) profile of eldecalcitol in a clinical investigation.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124468"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142997686","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":"High-throughput UPLC-ESI/MSMS method for simultaneous measurement of the urinary metabolites of volatile organic compounds and tobacco alkaloids","authors":"Shweta Srivastava ,&nbsp;Tatiana Krivokhizhina ,&nbsp;Rachel Keith ,&nbsp;Aruni Bhatnagar ,&nbsp;Sanjay Srivastava ,&nbsp;Zhengzhi Xie ,&nbsp;Pawel Lorkiewicz","doi":"10.1016/j.jchromb.2025.124463","DOIUrl":"10.1016/j.jchromb.2025.124463","url":null,"abstract":"<div><div>Human exposure to volatile organic compounds (VOCs) poses significant health risks, contributing to cardiovascular disease, pulmonary disease, and cancer. Measurement of VOC metabolites (VOCm) in urine by liquid chromatography-mass spectrometry (LC-MS) is a preferred method for VOCm analysis; however, existing methods encounter challenges related to sensitivity, throughput, and analyte coverage. In addition to VOCm, the measurement of tobacco alkaloids (TAm) is critical to account for tobacco use in population-based studies. A method is needed that is highly sensitive, offers higher throughput, and can analyze VOCm and TAm in a single run. Herein, we present a robust dilute-and-shoot method aimed at overcoming these analytical challenges and expanding the targeted analysis to include 35 urinary VOCm and TAm and their metabolites. By leveraging high-speed polarity switching and optimized chromatographic parameters, our method achieved comprehensive analyte coverage and enhanced sensitivity, enabling reliable individual level VOC exposure assessment. Validation demonstrates robust linearity, sensitivity, accuracy, and precision, with minimal matrix effects. This high-throughput UPLC-MS/MS method significantly enhances VOC exposure assessment by enabling simultaneous measurement of 35 urinary VOC and TAm with high sensitivity and efficiency. Multiple metabolites from single parent xenobiotics are included in one run, expanding biomarker specificity. Our data indicate the method effectively accounts for tobacco consumption as a confounder in population-based studies, ensuring accurate VOC exposure assessment.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124463"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142997758","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":"One-pot hydrothermal synthesis of polyethyleneimine-coated magnetic nanoparticles for high-efficient DNA extraction of pathogenic bacteria","authors":"Yan-Long Zhang ,&nbsp;Yu-Jun Shi ,&nbsp;Bao-Jian Duan ,&nbsp;Xian-Hua Wang","doi":"10.1016/j.jchromb.2024.124435","DOIUrl":"10.1016/j.jchromb.2024.124435","url":null,"abstract":"<div><div>For separation of deoxyribonucleic acid (DNA), positively charged amino-modified magnetic nanoparticles (MN) can effectively adsorb negatively charged DNA through electrostatic interaction. However, the reported preparation of amino-modified MN is usually tedious and time-consuming. Therefore, a simple synthesis method of amino-modified MN is necessary for DNA extraction. Herein, a novel polyethyleneimine-coated MN (PMN) was fabricated by one-pot hydrothermal synthesis for high-efficient DNA extraction. The fabricated PMN showed numerous exposed amino groups, which not only could effectively capture DNA through electrostatic interaction, but also limited the aggregation of PMN during application. Under optimized adsorption conditions, the maximum adsorption capacity of PMN for DNA could reach 192.4 μg m g⁻¹. <em>Shigella flexneri</em> (<em>S</em>. <em>flexneri</em>) has the highest mortality rate among <em>Shigella</em> species and has been selected as target model pathogenic bacteria. Based on the optimized extraction conditions, PMN-based magnetic solid-phase microextraction (MSPE) and quantitative real-time PCR (qPCR) were integrated for detection of <em>S</em>. <em>flexneri</em>. The limit of detection of the proposed strategy was 2.4 × 10² CFU mL⁻¹ and obviously lower than the commercial kit. To prove the practicability, the PMN-based MSPE combined qPCR strategy was successfully used in the determination of <em>S</em>. <em>flexneri</em> in spiked real sample, and the recovery values were in the range of 95.1 % to 102.1 % for apple juice, 60.4 % to 85.7 % for pickled vegetable, 97.8 % to 99.5 % for pig liver and 95.1 % to 102.1 % for pig colon, respectively. Therefore, we believe that the resultant PMN have great potential to become a universal magnetic adsorbent for high-efficient DNA extraction from complex biological samples.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124435"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142918941","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 validation of an LC-MS/MS method for quantifying total and unbound doravirine in human plasma","authors":"Rizqah Bernard,&nbsp;Sydwell P. Maputla,&nbsp;Phiwe Zuma,&nbsp;Anton Joubert,&nbsp;Sandra Castel,&nbsp;Marthinus van der Merwe,&nbsp;Edda Zangenberg,&nbsp;Lubbe Wiesner","doi":"10.1016/j.jchromb.2024.124439","DOIUrl":"10.1016/j.jchromb.2024.124439","url":null,"abstract":"<div><div>A robust LC-MS/MS method was developed to quantify total and unbound doravirine in plasma samples from patients receiving daily doses of 100 mg doravirine, in combination with lamivudine and tenofovir disoproxil fumarate, in a phase 3 clinical trial. The trial is ongoing, and sample analysis is planned to commence once all samples have been collected. The method was validated to quantify both total and unbound doravirine using a single calibration curve. Protein precipitation was used to obtain the total doravirine from plasma and ultrafiltration was used to obtain the unbound doravirine. A Kinetex 1.7 µm EVO C18 100 Å column was used for chromatography using a gradient mobile phase (0.1 % formic acid in water and 0.1 % formic acid acetonitrile) at a flow rate of 250 µL/min during a five minute runtime. The analyte was ionized by positive electrospray ionization and detection was by multiple reaction monitoring on a Sciex API3200 triple quadrupole mass spectrometer. Using calibration standards prepared in whole plasma, the calibration curve fitted a quadratic regression (weighted by 1/x) over a calibration range of 7.00–2000 ng/mL and was applied successfully for the measurement of both total and unbound doravirine. Validation experiments, conducted according to international guidelines, proved the accuracy and precision of the method over three consecutive days. The method demonstrated robustness in the presence of matrix components, different anticoagulants, hemolyzed blood (2 %), and concomitant medications, showing the necessary sensitivity and selectivity for the quantification of both total and unbound doravirine concentrations expected in the study samples.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124439"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142926115","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":"A novel LC-MS/MS assay for low concentrations of creatinine in sweat and saliva to validate biosensors for continuous monitoring of renal function","authors":"Sophie Adelaars ,&nbsp;Chyara S.M. Lapré ,&nbsp;Patricia Raaijmakers ,&nbsp;Constantijn J.A.M. Konings ,&nbsp;Massimo Mischi ,&nbsp;R. Arthur Bouwman ,&nbsp;Daan van de Kerkhof","doi":"10.1016/j.jchromb.2024.124444","DOIUrl":"10.1016/j.jchromb.2024.124444","url":null,"abstract":"<div><div>Monitoring of kidney function traditionally relies on plasma creatinine concentrations, necessitating invasive blood draws. Non-invasively obtainable biofluids, such as sweat and saliva, present a patient-friendly alternative with potential for continuous monitoring. This study focusses on developing and validating a novel Liquid Chromatography- tandem Mass Spectrometry (LC-MS/MS) assay as a reference test for measuring low creatinine concentrations in sweat and saliva. We explore the correlation between these biofluids and plasma creatinine concentrations during haemodialysis to support future biosensor applications. Creatinine concentrations were measured in sweat, saliva, and plasma obtained from forty patients undergoing haemodialysis. A novel LC-MS/MS assay was developed to quantify low creatinine concentrations in sweat and saliva. Correlation analyses were performed to compare the creatinine concentrations across biofluids. The novel LC-MS assay demonstrated high accuracy (93.9–97.8%) and low imprecision (3.4–8%) in measuring very low creatinine concentrations with a limit of quantitation of 1.26 µmol/L. Significant correlations ware found between creatinine concentrations in sweat and saliva with those in plasma (ρ: 0.68 and 0.80, respectively). During haemodialysis, creatinine concentrations decreased concurrently in all three biofluids. The strong correlations observed imply that these non-invasive biofluids could serve as reliable alternatives to traditional blood tests for kidney function assessment. This study enhances our understanding of creatinine excretion pathways of creatinine and provides a foundation for developing innovative, patient-friendly approaches for continuous kidney function monitoring, such as wearable biosensors.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124444"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143078301","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":"Evaluation of the effect of Ela tablets in the treatment of diabetic nephropathy based on rat experiments and screening strategy for quality markers of Ela tablets targeting aldose reductase","authors":"Shunan Guo ,&nbsp;Aizaiti Keremu ,&nbsp;Miao Hu ,&nbsp;Fei He ,&nbsp;Maitinuer Maiwulanjiang ,&nbsp;Haji Akber Aisa ,&nbsp;Xuelei Xin","doi":"10.1016/j.jchromb.2025.124450","DOIUrl":"10.1016/j.jchromb.2025.124450","url":null,"abstract":"<div><div>Ela tablets (ALP) is a traditional Uyghur medicinal formulation comprising 9 herbs. Clinical applications have demonstrated its potential in treating diabetic nephropathy (DN). However, its specific medicinal effects and pharmacodynamic components have not been elucidated. This research aims to investigate the efficacy of ALP in treating DN and to explore the quality markers (Q-markers) for its exertion of efficacy. Using the UHPLC-Q-Orbitrap HRMS technique, a total of 60 compounds were identified within ALP. Animal experiments were conducted to investigate the effect of ALP intervention at doses of 80, 160, and 320 mg/kg in Sprague-Dawley rats. Then, fingerprints of ten batches of ALP extracts were established using UPLC-DAD. Spectrum-effect relationship analysis of these fingerprints and aldose reductase (AR) activity was conducted by chemometric analysis methods. The results were further validated by molecular docking and cellular experiments. The animal experiments indicated that ALP had a therapeutic effect on DN. Specifically, ALP reduced biochemical indexes such as serum creatinine (SCr), 24-hour urinary total protein (24 h UTP), uric acid (UA), blood urea nitrogen (BUN), triglycerides (TG), and total cholesterol (TC). ALP stabilized body weight and fasting blood glucose, enhanced the antioxidant capacity of kidneys, and improved renal pathology. Comprehensive analysis indicated that crocin-I and gallic acid may be used as Q-markers for ALP. In summary, ALP has been identified as a treatment for DN, and gallic acid and crocin-I can be used as its Q-markers.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124450"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142963255","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":"Extraction and quantitation of fentanyl in exhaled breath condensate using a magnetic dispersive solid phase based on graphene oxide and covalent organic framework composite and LC-MS/MS analysis","authors":"Sedigeh Mohamadzadeh ,&nbsp;Ali Akbar Fathi ,&nbsp;Abolghasem Jouyban ,&nbsp;Afshin Gharekhani ,&nbsp;Mohamadbagher Hosseini ,&nbsp;Maryam Khoubnasabjafari ,&nbsp;Vahid Jouyban-Gharamaleki ,&nbsp;Mir Ali Farajzadeh ,&nbsp;Mohammad Reza Afshar Mogaddam","doi":"10.1016/j.jchromb.2024.124447","DOIUrl":"10.1016/j.jchromb.2024.124447","url":null,"abstract":"<div><div>Free fentanyl is responsible for its pharmacological effects, but its total concentration is typically determined for therapeutic drug monitoring purposes. Determination of fentanyl concentration can help reduce the prescribed doses, leading to fewer side effects and increased effectiveness. Therefore, predicting free drug concentration in pharmaceutical research is crucial. The aim of this study was to determine free fentanyl in exhaled breath condensate. These samples were extracted using a dispersive micro solid phase extraction method with a new adsorbent made of graphene oxide, magnetic iron oxide nanoparticles, and covalent organic framework. 10 mg of the adsorbent was added to the sample solution adjusted to pH 10. After sonication for 5 min, the sorbent was separated using an external magnet. The adsorbed analyte was then eluted from the sorbent surface using a mixture of acetonitrile, methanol, and deionized water in a ratio of 42.5:42.5:15 (v/v/v) and analyzed using liquid chromatography-tandem mass spectrometry system. The calibration curve showed high linearity in the range of 0.17–10000 μg L⁻¹ with a coefficient of determination of 0.9998 and good repeatability with a relative standard deviation of 4.1 %. Additionally, this method provided a low detection limit of 0.05 μg L⁻¹ and quantification limit of 0.17 μg L⁻¹.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"Article 124447"},"PeriodicalIF":2.8,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142997757","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}