Journal of Pharmaceutical and Biomedical Analysis Open最新文献

{"title":"Formic acid-aided sample preparation method for sensitive and simultaneous analysis of eight nitrosamines in poorly-water soluble pharmaceutical drugs using liquid chromatography–ultraviolet detection","authors":"Eiichi Yamamoto,&nbsp;Hitomi Kan-no,&nbsp;Daisuke Ando,&nbsp;Tamaki Miyazaki,&nbsp;Tatsuo Koide,&nbsp;Ken-ichi Izutsu,&nbsp;Yoji Sato","doi":"10.1016/j.jpbao.2023.100020","DOIUrl":"10.1016/j.jpbao.2023.100020","url":null,"abstract":"<div><p>There has been a growing concern over the contamination of pharmaceutical products with nitrosamines (NAs) such as <em>N</em>-nitrosodimethylamine (NDMA). To quantify NA levels in drugs using reversed-phase liquid chromatography (LC), the sample solution should achieve a high drug concentration to detect trace NAs, and an appropriate amount of hydrophilic NAs should be retained. However, these are difficult to achieve, and no suitable method has yet been developed. The present study was the first to develop a sample preparation method to achieve this by combining drugs with formic acid (FA), followed by the removal of active pharmaceutical ingredients (APIs) from samples via crystallization. This method was successfully applied for the sensitive quantification of eight NAs in poorly water-soluble acidic atorvastatin (ATS) and basic itraconazole (ITC) via LC–ultraviolet (LC-UV) detection. The removal rate of ITC via recrystallization exceeded 99.96 %, whereas most NAs remained as solutes. Assuming that the enhancement in ITC solubility directly translates to heightened analytical sensitivity, a &gt; 100-fold increase in sensitivity was attained compared to conventional methodologies. This sample preparation method would be applicable to other poorly water-soluble drugs, contributing to the control of NA content in various formulations to realize the safe delivery of pharmaceuticals to patients.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"2 ","pages":"Article 100020"},"PeriodicalIF":0.0,"publicationDate":"2023-10-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X23000208/pdfft?md5=7d42ede05957e2e87dab21117535373b&pid=1-s2.0-S2949771X23000208-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135965851","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Advances in surface plasmon resonance biosensors for medical diagnostics: An overview of recent developments and techniques","authors":"G.I. Janith ,&nbsp;H.S. Herath ,&nbsp;N. Hendeniya ,&nbsp;D. Attygalle ,&nbsp;D.A.S. Amarasinghe ,&nbsp;V. Logeeshan ,&nbsp;P.M.T.B. Wickramasinghe ,&nbsp;Y.S. Wijayasinghe","doi":"10.1016/j.jpbao.2023.100019","DOIUrl":"https://doi.org/10.1016/j.jpbao.2023.100019","url":null,"abstract":"<div><p>Over the last two decades, surface plasmon resonance (SPR) sensors have advanced significantly, becoming an important tool in disciplines such as biosensing, chemical sensing, and material characterization. SPR has gained popularity in biosensing because of its great sensitivity and specificity in detecting biomolecular interactions. This review provides an overview of the recent developments of the SPR biosensor technology and its applications in medical diagnostics. To provide an up-to-date overview of the area, the review includes the most recent works from the last decade. Furthermore, it explores various configurations (prism, grating, fiber optic, waveguide modulated) and wave properties (angle, wavelength, phase) being tracked for sensing together with strategies for enhancing sensitivity and selectivity through mechanisms such as surface coatings, sensing mediums, and immobilization techniques.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"2 ","pages":"Article 100019"},"PeriodicalIF":0.0,"publicationDate":"2023-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49879898","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Development and validation of UHPLC-ESI-MS/MS bioanalytical method, ADMET profiling, and pharmacokinetic study of bioactive phytoconstituents from Ayurvedic botanical Guduchi (Tinospora cordifolia)","authors":"Aboli Girme,&nbsp;Vijay Parmar,&nbsp;Shubham Jagtap,&nbsp;Ganesh Saste,&nbsp;Siddharth J. Modi,&nbsp;Lal Hingorani","doi":"10.1016/j.jpbao.2023.100018","DOIUrl":"https://doi.org/10.1016/j.jpbao.2023.100018","url":null,"abstract":"<div><p><em>Tinospora cordifolia</em> (TC) is known for its immense therapeutic applications in 'Ayurveda', which has created considerable scientific interest in pharmacology. Thus, a targeted and rapid bioanalytical UHPLC-ESI-MS/MS method was developed and validated for the extraction of its bioactive markers from diverse classes of diterpenes as tinosporide (TC1) and phytosterol-20-β-hydroxyecdysone (TC2) and isoquinoline alkaloids-jatrorrhizine (TC3), tetrahydropalmatine (TC4) from the TC stem extract (TCE) in rat plasma by solid phase extraction technique (SPE). The optimum recovery (≥ 90 %) was achieved for TC1–4 and internal standard fluoxymesterone (IS) with the SPE method on the C18 phase. The analytes were subjected to chromatographic analysis on the Agilent C18 Zorbax Eclipse Plus column (4.6 × 100 mm, 3.5 µ) with a gradient program using 0.1 % acetic acid in water (% <em>v/v</em>) and acetonitrile as mobile phase at a flow rate of 0.500 mL/min. The MS/MS quantification and validation were performed on the Shimadzu 8045 tandem mass spectrometer associated with the heated-ESI probe in SRM mode. The precursor to product ion transitions <em>m/z</em> 416.20→375.10 (TC1), 481.40→445.20 (TC2), 339.15→323.05 (TC3), 356.25→192.10 (TC4) and 337.20→91.00 (IS) were used for quantification. Also, <em>in silico</em> ADMET prediction and <em>in vivo</em> pharmacokinetics revealed that TC1–4 was well absorbed from the GI tract and could act as a P-GP substrate. In the pharmacokinetic study<em>,</em> TC1–4 could be detected by this validated bioanalytical method. The TC1 was found bioavailable, having an optimum half-life of &gt; 9.0 h to exhibit therapeutic activity with other TC bioactive markers <em>in vivo</em>. This research is the first comprehensive study on <em>in silico</em> and <em>in vivo</em> pharmacokinetics of TC biomarkers, which may aid in further pre-clinical and clinical trial investigations.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"2 ","pages":"Article 100018"},"PeriodicalIF":0.0,"publicationDate":"2023-09-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49879899","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Expression analysis of p50-associated COX-2 extragenic RNA and NF-Kappa B Interacting long non-coding RNA in multiple sclerosis patients","authors":"Zeinab Shirvani-Farsani ,&nbsp;Mina Rezaei ,&nbsp;Zahra Abedi Kichi ,&nbsp;Mehrdad Behmanesh ,&nbsp;Shirin Farivar","doi":"10.1016/j.jpbao.2023.100017","DOIUrl":"https://doi.org/10.1016/j.jpbao.2023.100017","url":null,"abstract":"<div><p>Inflammatory long non-coding RNAs (lncRNAs) including PACER (p50-associated COX-2 extragenic RNA) and NKILA (NF-Kappa B Interacting long non-coding RNA) and have recently emerged as essential regulators in immune and inflammation pathways in patients with multiple sclerosis (MS), which have possible worthiness as diagnostic, prognostic, and therapeutic targets. In the current study, we aimed to evaluate the expressions of PACER, NKILA lncRNAs, CTCF (CCCTC-binding factor), and NF-κB in the PBMC (peripheral blood mononuclear cells) from MS patients and control subjects. We detected the expression levels of PACER, CTCF, NKILA, and NF-kB using real-time PCR in 39 MS patients and 37 healthy controls. The findings show that the expression levels of PACER lncRNA and CTCF, but not NKILA lncRNA and NF-κB, have significantly decreased in MS patients compared to the controls, so they are probably involved in MS pathogenesis. Notably, the area under the ROC curve for PACER and CTCF was up to 0.80 and 0.68, respectively. Based on these observations, the PACER and CTCF had been shown to have the best efficiency in the discrimination of disease status between MS patients and healthy controls. A low expression level of CTCF was correlated with PACER lncRNA and NF-KB expression levels as well as some factors including disease duration, age, and EDSS. Altogether, these results demonstrate that PACER lncRNA and CTCF were potentially related to the MS risk. However, further functional investigations are required to confirm the roles of these genes in the etiology of MS.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"2 ","pages":"Article 100017"},"PeriodicalIF":0.0,"publicationDate":"2023-08-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49879897","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Development and application of a supercritical fluid chromatography-tandem mass spectrometry method for the simultaneous determination of pantoprazole enantiomers in rat plasma","authors":"Junli Lin ,&nbsp;Youchen Liu ,&nbsp;Jiawei Zhang ,&nbsp;Ziqi Lu ,&nbsp;Jianmin Guo ,&nbsp;Yuankeng Huang ,&nbsp;Baoqin Lin ,&nbsp;Wei Yang","doi":"10.1016/j.jpbao.2023.100016","DOIUrl":"https://doi.org/10.1016/j.jpbao.2023.100016","url":null,"abstract":"<div><p>The study aimed to develop a supercritical fluid chromatography-tandem mass spectrometry (SFC-MS/MS) method for the enantioselective separation and quantification of pantoprazole in rat plasma. The method utilized protein precipitation with acetonitrile to prepare plasma samples. SFC was performed on an Acquity ultra-performance convergence chromatography (UPCC) system. An Acquity UPCC Trefoil™ CEL2 column was employed for enantioseparation, and isocratic elution was achieved using a mobile phase consisting of CO₂-methanol (81:19, v/v). The detection of pantoprazole enantiomers and the internal standard phenacetin was carried out using a Xevo TQD triple quadrupole mass spectrometer in selected reaction monitoring mode with positive electrospray ionization. The developed method successfully achieved full separation of <em>S</em>- and <em>R</em>-pantoprazole enantiomers. Calibration curves were linear in the concentration range of 10–5000 ng/mL for both <em>S</em>- and <em>R</em>-pantoprazole. The method met the acceptance criteria for carry-over, accuracy, precision, extraction recovery, matrix effect, stability, and dilution integrity, demonstrating its stereoselectivity, sensitivity, accuracy, precision, and reliability. The validated method was then applied to investigate the toxicokinetics of racemic pantoprazole and evaluate the potential of chiral inversion between <em>S</em>- and <em>R</em>-pantoprazole in rats. Following oral administration of 200 mg/kg racemic pantoprazole once daily for 90 consecutive days, there was no significant difference in toxicokinetic parameters between the two enantiomers on both day 1 (single-dose experiment) and day 90 (multiple-dose experiment). This suggests that there is no enantioselectivity in the toxicokinetic behaviors of racemic pantoprazole in rat plasma. Additionally, bidirectional chiral inversion between <em>S</em>- and <em>R</em>-pantoprazole in plasma was observed after single-dose and multiple-dose oral administrations of <em>S</em>-pantoprazole (20, 100, and 200 mg/kg) or <em>R</em>-pantoprazole (200 mg/kg) to rats. Compared to single and low doses, there was no accumulation of each enantiomer in rat plasma following repeated and escalated dosing. Overall, this study provided the first report on the toxicokinetics of pantoprazole in rat plasma and presented the first SFC-MS/MS method for the simultaneous quantification of pantoprazole enantiomers in rat plasma.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"2 ","pages":"Article 100016"},"PeriodicalIF":0.0,"publicationDate":"2023-07-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49879895","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Prediction of impurities in cocoa shell powder using NIR spectroscopy","authors":"Marciano M. Oliveira ,&nbsp;Marcus V.S. Ferreira ,&nbsp;Mohammed Kamruzzaman ,&nbsp;Douglas F. Barbin","doi":"10.1016/j.jpbao.2023.100015","DOIUrl":"https://doi.org/10.1016/j.jpbao.2023.100015","url":null,"abstract":"<div><p>Cocoa shell is a by-product from cocoa industry which contains bioactive compounds of high and attractive value for food, pharmaceutical and cosmetics industry. However, cocoa shell can be contaminated by undesirable materials that, even in small amounts, would not change the color, aroma, and taste characteristics of the final product. Identification and prediction of this impurity are performed using expensive methods that require chemicals and produce residues. Thus, this work aims to investigate the performances of benchtop (867–2535 nm) and portable (900–1700 nm) near-infrared (NIR) spectrometer for fast prediction of cocoa shell powder impurities. Mixtures (n = 432) of cocoa shell powders with leaves, pods, stem fragments and nibs at several proportions (0–20 % w/w), were analyzed. Multivariate calibration models were developed using partial least-squares regression (PLSR) with raw spectra and various preprocessing approaches applied to the spectra. The most informative spectral variables were selected by variable importance in projection (VIP) method. Results obtained for the benchtop (R²_P&gt; 0.99 and RMSEP&lt;0.71) and low-cost portable (R²_P&gt; 0.92 and RMSEP&lt;1.70) devices are promising, and portable spectrometer could be used to certify cocoa shell purity.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"2 ","pages":"Article 100015"},"PeriodicalIF":0.0,"publicationDate":"2023-06-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49879894","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Development of an enantioselective three-dimensional HPLC system for the determination of alanine, valine, isoleucine, allo-isoleucine and leucine in human plasma and urine","authors":"Yuri Nagata ,&nbsp;Takeyuki Akita ,&nbsp;Chiharu Ishii ,&nbsp;Mai Oyaide ,&nbsp;Masashi Mita ,&nbsp;Tomomi Ide ,&nbsp;Kenji Hamase","doi":"10.1016/j.jpbao.2023.100013","DOIUrl":"https://doi.org/10.1016/j.jpbao.2023.100013","url":null,"abstract":"<div><p>A three-dimensional (3D) HPLC system was designed/developed for the discriminative determination of aliphatic chiral amino acids, namely, alanine (Ala), valine (Val), isoleucine (Ile), <em>allo</em>-Ile (aIle) and leucine (Leu), in human physiological fluids. These aliphatic amino acid enantiomers are expected to be new physiologically active molecules and/or biomarkers in mammals. Among these aliphatic amino acids, the structural chain isomers of Leu (Ile/aIle/Leu) have similar chemical-physical properties, and the analytical method for these aliphatic amino acids is required to be highly enantio- and chemo-selective. In the present study, a reversed-phase column (Singularity RP18, first dimension) and a mixed-mode column (Singularity MX-103, second dimension) were utilized to separate these aliphatic amino acids as their scalemic mixtures, then chiral separations were performed using a Pirkle-type enantioselective column (Singularity CSP-001S) in the third dimension. By using the 3D-HPLC system, these aliphatic amino acid enantiomers were completely discriminated, and the analysis of these aliphatic chiral amino acids in the human plasma and urine was successfully carried out. The obtained amounts of the aliphatic amino acids (and %D value, the percentage of <span>D</span>-form to D + L forms) in the human plasma were 2.1 µM (0.5%) for <span>D</span>-Ala, and trace/not-detected for the other <span>D</span>-forms. In human urine, the values were 102.0 µM (24.7%) for D-Ala, 2.0 µM (3.4%) for D-Val, 2.3 µM (10.8%) for D-aIle (%D value of D-aIle was calculated using D-aIle and <span>L</span>-Ile) and 3.3 µM (5.5%) for D-Leu. The present 3D-HPLC system is a powerful and well validated tool for the simultaneous determination of aliphatic amino acid enantiomers, and further biological and clinical studies are expected.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"2 ","pages":"Article 100013"},"PeriodicalIF":0.0,"publicationDate":"2023-06-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49879896","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Fluorescent nanoprobe prepared from hyaluronic acid modified iron selenide nanoparticles for real-time detection of hyaluronidase as tumor marker","authors":"Chaoqun Zhang ,&nbsp;Jie Song ,&nbsp;Xin Shen ,&nbsp;Qian Li ,&nbsp;Feng Su ,&nbsp;Suming Li","doi":"10.1016/j.jpbao.2023.100001","DOIUrl":"https://doi.org/10.1016/j.jpbao.2023.100001","url":null,"abstract":"<div><p>A highly sensitive nanoprobe HAPPF@FeSe₂NPs was developed for real-time detection of hyaluronidase (HAase) as tumor marker. Hyaluronic acid (HA) was first functionalized with adipic acid dihydrazide (ADH) via amide formation. Carboxyl-terminated polylactide (PLA) was then grafted to HA-ADH using EDC/NHS as coupling agents, yielding an HA-ADH-PLA (HAP) graft copolymer. Iron selenide nanoparticles (FeSe₂NPs) were surface coated with HAP by ultrasonic assisted self-assembly. Finally, the resulted HAP@FeSe₂NPs were surface-modified with fluorescein isothiocyanate (FITC) and polyethyleneimine (PEI) to obtain HAPPF@FeSe₂NPs fluorescent nanoprobe. Analyses by FTIR, XRD, XPS, EDX, TEM, DLS, ¹H NMR and TGA confirmed the successful synthesis of the nanoprobe, and fluorescence spectroscopy proved its good detection performance. Moreover, cell imaging results demonstrated the ability of the nanoprobe to target tumor cells. MTT assay and hemolysis tests confirmed its good cyto- and hemo-compatibility. Therefore, it is concluded that HAPPF@FeSe₂NPs nanoprobe could be used in targeted tumor cell imaging for early diagnosis of cancers.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"1 ","pages":"Article 100001"},"PeriodicalIF":0.0,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49883947","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Label-free shotgun proteomics: Exploiting a reliable and sensitive method to monitor residual host-cell proteins in monoclonal antibody products","authors":"Somar Khalil,&nbsp;Adeline Wychowski,&nbsp;Cyrille Chéry,&nbsp;Annick Gervais","doi":"10.1016/j.jpbao.2023.100012","DOIUrl":"https://doi.org/10.1016/j.jpbao.2023.100012","url":null,"abstract":"<div><p>The removal of host cell proteins (HCPs) remains a challenge in the downstream processing of monoclonal antibodies (mAbs). It is critical to monitor residual HCPs since they can have an impact on product stability and safety. The enzyme-linked immunosorbent assay (ELISA) only quantifies the total amount of HCPs and does not indicate the identity or quantity of any specific HCP. Mass spectrometry-based proteomics applications demonstrate an advantage in quantitatively profiling individual HCPs. However, technical reproducibility, dynamic range, and ensuring an acceptable statistical significance of scoring measurements are critical hurdles that ought to be overcome. In this paper, we describe a sensitive and reproducible shotgun proteomics approach that includes an efficient mAb depletion strategy and addresses the shortcomings of such workflows. Our methodology is potentially a valuable complement or alternative to ELISA. Additionally, it can facilitate the purification process development and the evaluation of ELISA kits upon process changes.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"1 ","pages":"Article 100012"},"PeriodicalIF":0.0,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49883945","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"MIP-based electrochemical sensor for highly selective and sensitive determination of entacapone from the triple mixture in tablet dosage form","authors":"Fatma Budak ,&nbsp;Ahmet Cetinkaya ,&nbsp;S. Irem Kaya ,&nbsp;Sibel A. Ozkan","doi":"10.1016/j.jpbao.2023.100005","DOIUrl":"https://doi.org/10.1016/j.jpbao.2023.100005","url":null,"abstract":"<div><p>The aim of this study is to develop a molecularly imprinted polymer (MIP) sensor via photopolymerization for selective and sensitive analysis of entacapone (ENT), a catecholamine-o-methyl transferase (COMT) inhibitor. ENT is used for Parkinson’s disease treatment with levodopa (LEV) and carbidopa (CAR), and it is available in a triple combination tablet dosage form. For the MIP-based electrochemical sensor (4-AP@MIP/GCE) design, 4-aminophenol (4-AP) was selected as the functional monomer. Surface characterization of the 4-AP@MIP/GCE sensor was performed by scanning electron microscopy, electrochemical characterization by CV, and electrochemical impedance spectroscopy (EIS). The linear concentration range was between 1.0 pM and 10.0 pM under optimum conditions for ENT determination. The limit of detection (LOD) of 0.24 pM and the limit of quantification (LOQ) of 0.80 pM were calculated for ENT analysis using 4-AP@MIP/GCE. The accuracy was proven by performing a recovery study on the tablet sample that contains ENT, LEV, and CAR, and the recovery was found to be 99.32%. The selectivity of the 4-AP@MIP/GCE sensor for ENT has been proven by interference studies on LEV, CAR, and their binary mixtures. Looking at the results of the study, it has been proven that the 4-AP@MIP/GCE sensor is a highly selective, sensitive, and specific quantitative option for the analysis of ENT.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"1 ","pages":"Article 100005"},"PeriodicalIF":0.0,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49883903","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}