Journal of Pharmaceutical and Biomedical Analysis Open最新文献

{"title":"Recent advances in molecular imprinting techniques for the electrochemical analysis of chiral compounds","authors":"Sevda Hasanova ,&nbsp;Abdellatif Ait Lahcen ,&nbsp;Erhan Zor","doi":"10.1016/j.jpbao.2024.100046","DOIUrl":"10.1016/j.jpbao.2024.100046","url":null,"abstract":"<div><div>Molecular imprinting technology has emerged as a powerful tool for creating highly selective recognition elements, known as molecularly imprinted polymers (MIPs). These synthetic polymers possess tailor-made binding sites with high affinity and specificity for target molecules, making them ideal for various analytical applications, including detecting and separating chiral compounds. This review provides a comprehensive overview of recent advances in the design, synthesis, and application of MIPs for chiral analysis. Key developments in using novel monomers, innovative polymerization techniques, and advanced characterization methods are discussed. Additionally, integrating MIPs with cutting-edge materials such as metal-organic frameworks (MOFs) and nanomaterials is explored, highlighting their impact on improving sensor performance. The novelty of our review lies in its profound discussion of the recent advancement of electrochemical sensors-based MIPs that exhibit significant improvements in sensor miniaturization, rapid response times, and portability. The progress made in this fieldmarks a significant leap forward in the development of cost-effective, sustainable sensing devices for chiral analysis in complex matrices. Additionally, this review critically evaluates the pros and cons of various approaches, providing a comprehensive guide to future research in the field. The discussed techniques have strong potential for application in pharmaceutical quality control, clinical diagnosis, and environmental monitoring. This review aims to provide researchers and practitioners in MIPs with valuable insights into the current state and future directions of this technology for chiral compound analysis.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"4 ","pages":"Article 100046"},"PeriodicalIF":0.0,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142660805","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":"Isolation and structural elucidation of novel degradant during degradation study of Azilsartan kamedoxomil","authors":"Anil Kumar Guduri ,&nbsp;Vundavilli Jagadeesh Kumar ,&nbsp;P.Badarinadh Gupta ,&nbsp;Julakanti Shashidar Reddy ,&nbsp;Kishore Babu Bonige ,&nbsp;Hemant Kumar Sharma","doi":"10.1016/j.jpbao.2024.100032","DOIUrl":"https://doi.org/10.1016/j.jpbao.2024.100032","url":null,"abstract":"<div><p>To investigate the stability of Azilsartan kamedoxomil (AKM) under stress conditions and to identify the degradation products, it was subjected to force degradation/stress under basic, acidic, oxidative, thermal, humidity, and photolytic conditions as per international council for harmonisation (ICH) guidelines. AKM degradation was found under basic, acidic, oxidative, thermal, photolytic, and humidity stress. Separation of the four degradation products of AKM was carried out utilizing a C-18 column, employing preparative High-performance liquid chromatography (HPLC) and gradient mode elution. The structures were elucidated with spectroscopic HRMS, 1D, and 2D NMR and the products were identified as <em>2-hydroxy-1-[[2′-(5-oxo-4,5-dihydro-1,2,4-oxadiazol −3-yl)[1,1′-biphenyl]-4-yl]-methyl]-1 H-benzimidazole-7-carboxylic acid</em> (AKMDP-1), 2<em>-ethoxy-1-[[2′-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl]-1 H-benzimidazole-7-carboxylic acid</em> (AKMDP-2), <em>(5-methyl-2-oxo-1,3-dioxol-4-yl)methyl 2-hydroxy-1-[[2′-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)[1,1′-biphenyl]-4-yl]methyl]-1 H-benzimidazole-7-carboxylate</em> (AKMDP-3) and <em>2-hydroxy-3-oxobutyl 2-ethoxy-1-((2′-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)-[1,1′-biphenyl]-4-yl)methyl)-1 H-benzo[d]imidazole-7-carboxylate</em> (AKMDP-4). Out of them, two degradants AKMDP-1 and AKMDP-3 were reported earlier, AKMDP-2 was one of the process intermediate (Azilsartan) used in the preparation of Azilsartan kamedoxomil.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"4 ","pages":"Article 100032"},"PeriodicalIF":0.0,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X24000082/pdfft?md5=9383b0112254ebad0cd5103d8732f5df&pid=1-s2.0-S2949771X24000082-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141486207","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":"Preparation of novel semi-covalent molecularly imprinted polymer for highly improved adsorption performance of tetracycline in aqueous medium","authors":"Luana Rianne da Rocha ,&nbsp;Mariana Gava Segatelli ,&nbsp;César Ricardo Teixeira Tarley","doi":"10.1016/j.jpbao.2024.100044","DOIUrl":"10.1016/j.jpbao.2024.100044","url":null,"abstract":"<div><div>In the present study, a novel tetracycline-imprinted polymer for tetracycline (TC) adsorption in an aqueous medium was synthesized using a semi-covalent imprinting method for the first time. In this approach, the template-monomer complex was synthesized by the reaction of 3-isopropenyl-α,α-dimethylbenzyl isocyanate (IPDMBI) as the functional monomer and TC as a template, forming a thermally reversible urethane bond (covalent bond). The polymer was characterized by Fourier transform infrared (FT-IR) spectroscopy, thermogravimetric analysis (TGA), nitrogen adsorption/desorption measurements, and determination of point zero charge (PCZ). The equilibrium time of TC onto MIP was reached in 15 min, which was described by the non-linear pseud second-order kinetic model. Adsorption isotherm was described as a dual-site Langmuir-Freundlich model and the maximum adsorption capacity, determined at pH 5.0, was found to be 76.74 mg g⁻¹ for MIP, exhibiting higher adsorption capacity when compared with other adsorbent materials previously reported in the literature for TC. Based on the increment relative selectivity coefficient the MIP showed higher selectivity towards TC and some structurally similar compounds belonging to the tetracyclines family (oxytetracycline and chlorotetracycline), when compared with NIP (non-imprinted polymer). The obtained outcomes in terms of selectivity, maximum adsorption capacity, and fast kinetic make this imprinted polymer an outstanding material for future application in molecularly imprinted solid phase extraction for analytical purposes.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"4 ","pages":"Article 100044"},"PeriodicalIF":0.0,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142539996","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":"Development and validation of LC/MS/MS quantification method for plantaricins in culture supernatant","authors":"Yumi Komori,&nbsp;Hiroshi Kuwahara,&nbsp;Mikio Aoki","doi":"10.1016/j.jpbao.2024.100043","DOIUrl":"10.1016/j.jpbao.2024.100043","url":null,"abstract":"<div><div>Bacteriocins are a group of small antimicrobial peptides that are ribosomally synthesized and secreted by lactic acid bacteria (LAB). These peptides exhibit high inhibitory activity at low concentrations in the nanomolar range and possess relatively narrow-spectrum antimicrobial activity, making them attractive for various applications, especially as natural food preservatives. Here, we report a novel nanoflow LC/MS/MS-based analysis method for the simultaneous quantification of plantaricin E, F, J, and K in the culture supernatants of their producer LAB strain ABG0035. This method enables accurate quantification of the bacteriocins of interest, even in the presence of high concentrations of sample matrices commonly found in the culture medium. Furthermore, this approach is promising for the analysis of bacteriocins in diverse environments, including cultured bacteria and food matrices.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"4 ","pages":"Article 100043"},"PeriodicalIF":0.0,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142433951","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":"A review for cortisol sensing in medical applications","authors":"Gaye Ezgi Yılmaz,&nbsp;Yeşeren Saylan,&nbsp;Adil Denizli","doi":"10.1016/j.jpbao.2024.100045","DOIUrl":"10.1016/j.jpbao.2024.100045","url":null,"abstract":"<div><div>Cortisol, one of the most important glucocorticoids, plays a critical role in various physiological processes. Elevated cortisol levels have been associated with chronic stress, increased vulnerability to anxiety, depression, cardiovascular disease, and weakened immune responses. Consequently, the development of reliable, effective, and rapid cortisol detection methods is invaluable for understanding the dynamic stress-response profile of individuals, enabling comprehensive self-monitoring, personalized healthcare, and effective health management. Cortisol sensors offer limitless possibilities in terms of their applications, featuring straightforward sensor preparation and wide detection limits. To sum, the future of cortisol sensing in medical applications holds immense assure for transforming stress management, mental health care, chronic disease management, athletic performance optimization, and personalized medicine, with significant benefits for individuals and healthcare providers alike. This review gives a wide overview of current state of cortisol hormone sensors, encompassing their working mechanisms and diverse applications. By examining the advancements in cortisol sensing technology, this review aims to provide insights into the potential of cortisol sensing in healthcare and its implications for improved patient outcomes.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"4 ","pages":"Article 100045"},"PeriodicalIF":0.0,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142660804","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":"Fabrication of ultra-sensitive and disposable electrochemical biosensor: Detection of kidney injury molecule-1 protein in urine for diagnosis of kidney injury","authors":"Elif Ceren Ankara,&nbsp;Sude Aras,&nbsp;Burçak Demirbakan,&nbsp;Mustafa Kemal Sezgintürk","doi":"10.1016/j.jpbao.2024.100042","DOIUrl":"10.1016/j.jpbao.2024.100042","url":null,"abstract":"<div><div>This research study indicates the development of the indium tin oxide-polyethylene terephthalate (ITO-PET) coated electrode-based electrochemical biosensor system to sensitively and specifically detect kidney injury molecule-1 (KIM-1), an acute kidney injury (AKI) biomarker. The ITO-PET electrode surface was modified with 3-(Trimethoxysilyl)-1-propanethiol (3-TMESP) silane agent. Electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), and single frequency impedance (SFI) techniques were utilized to examine the interactions between anti-KIM-1 antibody and KIM-1 antigen. The ITO-PET electrode surface was observed by scanning electron microscopy (SEM) and atomic force microscopy (AFM) to analyze the morphological characterization at each electrode development stage. Optimization studies have been conducted to determine the optimal concentrations for detecting the 3-TMESP silane agent, the NHS crosslinker, the anti-KIM-1 antibody, and the optimum incubation period for the anti-KIM-1 antibody and the KIM-1 antigen. Analytical characteristic properties of the developed biosensor, including linear determination range, and the studies of reproducibility, regeneration, repeatability, storage life, and selectivity were investigated. The KIM-1 biosensor system, based on 3-TMESP, has a broad linear range and is capable of providing sensitive measurements between 0.1 fg/mL and 1000 fg/mL. The values of low limits of detection (0.26 fg/mL) and of quantification (0.87 fg/mL) were calculated, highlighting its high sensitivity and precision in detecting KIM-1. In addition, five different commercially purchased human urine samples were tested to validate the practicability of the developed biosensor.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"4 ","pages":"Article 100042"},"PeriodicalIF":0.0,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142433952","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":"Nitrosamine contamination of pharmaceuticals: Cases in Japan, formation mechanisms, detection methods, regulatory perspectives, and insights","authors":"Genichiro Tsuji ,&nbsp;Hidetomo Yokoo ,&nbsp;Yosuke Demizu ,&nbsp;Yasuhiro Abe ,&nbsp;Sayaka Masada ,&nbsp;Nahoko Uchiyama ,&nbsp;Tomoaki Tsutsumi ,&nbsp;Eiichi Yamamoto","doi":"10.1016/j.jpbao.2024.100034","DOIUrl":"10.1016/j.jpbao.2024.100034","url":null,"abstract":"<div><p>In recent years, mutagenic nitrosamines, such as <em>N</em>-nitrosodimethylamine, have been detected in medicine. This has led to global product recalls and long-term supply suspensions by pharmaceutical companies and consequent clinical impacts. Measures to control nitrosamines in medicine, including detection methods and clarification of contamination routes, are being implemented worldwide. In this review, we focus on case reports of nitrosamine contamination of drug products in Japan, nitrosamine formation mechanisms during manufacturing and storage, as well as detection methods. We also discuss the acceptable nitrosamine intake (ng/day) in chemically synthesized drug substances in human drugs (including drug products) in the US, EU, and Japan. Overall, nitrosamine contamination of medicines is expected to remain a global public health issue. Therefore, detection methods using new technologies and detailed analysis of the formation mechanisms are necessary. However, excessive regulation may cause essential drug shortages owing to product recall; therefore, a realistic and prudent response based on regulatory science is needed.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"4 ","pages":"Article 100034"},"PeriodicalIF":0.0,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X24000100/pdfft?md5=8fa219998320e21f083d68540fd3baf6&pid=1-s2.0-S2949771X24000100-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141839356","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":"An intriguing future is approaching: Artificial intelligence meets molecularly imprinted polymers","authors":"Tunca Karasu ,&nbsp;Fatih Çalışır ,&nbsp;Sena Pişkin ,&nbsp;Erdoğan Özgür ,&nbsp;Canan Armutcu ,&nbsp;Mehmet Emin Çorman ,&nbsp;Lokman Uzun","doi":"10.1016/j.jpbao.2024.100041","DOIUrl":"10.1016/j.jpbao.2024.100041","url":null,"abstract":"<div><p>Artificial intelligence (AI) is developing and expanding rapidly beyond the expectations of engineers who develop it as well. It is evaluated that it has/will have great potential not only in terms of software but also in terms of material science, data analysis, and decision-making. On the other hand; molecularly imprinted polymers (MIPs) still attract researchers’ attention with their superior features in terms of wide range of design options and application fields. In this review, the combination of AI and MIP applications and their potential contributions to the future were compiled. In this context, firstly, a brief introduction to MIPs were given in a combination with recent sensor design approaches. Subsequently, the subject of artificial intelligence, in other commonly used words, machine learning, was discussed while summarizing the commonly used algorithms. In the last section, pioneering studies involving the combination of AI and MIPs are highlighted. This review will be the first article compiling AI and MIPs as well as it is thought to be an important main resource for researchers and enthusiasts.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"4 ","pages":"Article 100041"},"PeriodicalIF":0.0,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X24000173/pdfft?md5=167be38a8a1ccf3d8345fa82ed16be9d&pid=1-s2.0-S2949771X24000173-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142232742","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":"USP’s characterization of commercial poly(lactic-co-glycolic acid) utilizing SEC-Multi-Angle Light Scattering and Refractive Index techniques via Absolute Method approach","authors":"Yixin Ren ,&nbsp;Leo Liu ,&nbsp;Yang Liu ,&nbsp;Weidong Zhao ,&nbsp;Peng Zhang ,&nbsp;Hong Wang ,&nbsp;Catherine Sheehan ,&nbsp;Michael Ambrose","doi":"10.1016/j.jpbao.2024.100031","DOIUrl":"https://doi.org/10.1016/j.jpbao.2024.100031","url":null,"abstract":"<div><p>This research focuses on evaluating the data quality and reliability of Size Exclusion Chromatography with Multi-Angle Light Scattering and Refractive Index (SEC-MALS/RI) chromatography in determining molecular weight-related parameters in poly(lactic-co-glycolic) acid (PLGA) polymers. The study utilizes key metrics, particularly percent relative standard deviation (%RSD), to evaluate the precision across different data processing conditions. Exploring baseline selection of the chromatograms reveals that selection of the baseline based on the intrinsic shape of the chromatogram, rather than relying on elution peaks, improves consistency. The study emphasizes the critical role of result fitting in addressing systematic errors and sample heterogeneity, recommending the minima of the elution peak selection range for realistic molecular weight distribution representation. Analysis of light-scattering (LS) detector chromatograms highlights varying effects on different PLGA polymers, emphasizing the need for careful assessment and potential exclusion for precision improvement, especially in the presence of experimental artifacts. Across diverse PLGA polymers, the utilization of different column types, along with considerations such as baseline determination and peak selection, shows minimal variations in <em>M</em>n, <em>M</em>w, and polydispersity index (PDI), affirming the consistency of the methodology. The %RSD analysis further supports the methodology's precision, with values well within acceptable limits. In summary, this comprehensive evaluation of methodological conditions, including baseline selection, result fitting, LS detector data management, and column types, establishes a reliable SEC-MALS/RI chromatographic approach by Absolute Method for determining molecular weight parameters in PLGA polymers.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"4 ","pages":"Article 100031"},"PeriodicalIF":0.0,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X24000070/pdfft?md5=bbe1e901af41b24ff4f3540bad739844&pid=1-s2.0-S2949771X24000070-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141438564","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":"Absolute purity determination of an organic fluorine pharmaceutical voriconazole via quantitative 19F NMR and method validation","authors":"Nahoko Uchiyama ,&nbsp;Junko Hosoe ,&nbsp;Kohei Kiyota ,&nbsp;Takanori Komatsu ,&nbsp;Naoki Sugimoto ,&nbsp;Kyoko Ishizuki ,&nbsp;Tatsuo Koide ,&nbsp;Mika Murabayashi ,&nbsp;Taeko Shinozaki ,&nbsp;Yoshinori Fujimine ,&nbsp;Katsuya Ofuji ,&nbsp;Hitoshi Shimizu ,&nbsp;Kazuhiro Fujita ,&nbsp;Takashi Hasebe ,&nbsp;Yumi Asai ,&nbsp;Eri Ena ,&nbsp;Yoshinobu Makino ,&nbsp;Toru Miura ,&nbsp;Yasuhiro Muto ,&nbsp;Katsuo Asakura ,&nbsp;Yukihiro Goda","doi":"10.1016/j.jpbao.2024.100039","DOIUrl":"10.1016/j.jpbao.2024.100039","url":null,"abstract":"<div><p>The ¹⁹F NMR spectrum has a smaller number of signals than ¹H NMR, therefore, quantitative ¹⁹F NMR (¹⁹F-qNMR) can replace quantitative ¹H NMR (¹H-qNMR) for the absolute quantitation of organic fluorine-bearing compounds. In this study, we determined the purity of voriconazole (VCZ), an organic fluorine pharmaceutical, using ¹⁹F-qNMR, validated the results in multiple laboratories, and compared them with those obtained using an established ¹H-qNMR method. 3,5-Bis(trifluoromethyl)benzoic acid (3,5-BTFMBA) was selected as the reference standard for both ¹⁹F-qNMR and ¹H-qNMR owing to its solubility characteristics and ¹⁹F-qNMR and ¹H-qNMR chemical shifts.</p><p>Since VCZ contains three fluorines, the ¹⁹F-qNMR spectrum of VCZ showed three major fluorine signals (FA, FB, and FC). ¹⁹F-qNMR measurements were performed under three conditions with each ¹⁹F signal of VCZ (FA, FB, and FC) and the ¹⁹F signal of RS as the center (offset) of each observation. The quantitative values of the three target signals FA, FB, and FC were calculated and were comparable; 99.40 %, 99.66 %, and 99.49 %, respectively.</p><p>Owing to a difference of up to 8.8 % between the quantitative values of the two signals other than the targeted quantitative signal, the average FA, FB, and FC quantitative values were considered for purity (%). The purity of VCZ determined by ¹H- and ¹⁹F-qNMR was comparable (99.65±0.29 % and 99.52±0.44 %, respectively), exhibiting variations within an acceptable range. Compared to conventional ¹H-qNMR methods, the developed ¹⁹F-qNMR method has been proven efficient and highly promising for determining the accurate purity of organic fluorine pharmaceuticals.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"4 ","pages":"Article 100039"},"PeriodicalIF":0.0,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X2400015X/pdfft?md5=f5acbec6128e8e151c576b31ad103517&pid=1-s2.0-S2949771X2400015X-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142149674","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}