Journal of Pharmaceutical and Biomedical Analysis Open最新文献

{"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":"2024-06-28","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":"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":"2024-06-18","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":"Ultrasound super resolution imaging for accurate uterus tumor detection and malignancy prediction","authors":"Ashwini Sawant ,&nbsp;Sujata Kulkarni ,&nbsp;Milind Sawant","doi":"10.1016/j.jpbao.2024.100029","DOIUrl":"https://doi.org/10.1016/j.jpbao.2024.100029","url":null,"abstract":"<div><p>The term ‘tumor’ describes an atypical development of cells that forms a mass inside an organ; depending on the organ's invasive nature and propensity for metastasis, the growth may be benign or malignant. Improving patient outcomes requires the early detection of malignant tumors. Despite its lower resolution and noise problems, ultrasound, which is frequently used to diagnose uterine tumors, is safer and more economical than magnetic resonance imaging (MRI) scans and biopsies. Ultrasound pictures can be processed using methods including denoising, enhancement, segmentation, and feature extraction to get around these restrictions and boost their quality. Enhanced ultrasound images can reach even higher accuracy, cementing them as plausible alternatives to MRI. A comparative analysis of copious relevant image de-speckling, image enhancement, segmentation, and feature extraction methods are carried out. Higher resolution and superior quality, strong segmented real-time ultrasound uterus tumour images are produced by using diffusion-based hybrid filters, Super Resolution Convolutional Neural Networks (SRCNN), and U-net segmentation technique. The Grey Level Co-occurrence Matrix (GLCM) and Discrete Wavelet Transform (DWT) are used to extract textural features. With the help of several machine learning approaches, such as Support Vector Machine (SVM), K-Nearest Neighbour (KNN), and Random Forest classifiers (RFC), the extracted characteristics are immediately sent to classifiers to classify uterus tumours from ultrasound images between benign and malignant. For the categorization of uterine tumors, the RFC classifier outperformed the other classifiers. The viability of cancer detection using ultrasound pictures is significantly strengthened by the suggested machine learning methodology. Multiple hospitals provided data on ultrasound pictures of uterine tumors, which were used to develop the model and obtain the prediction findings. A radiologist with 17 years of expertise in diagnostic radiology further assessed this dataset. We could produce high-quality ultrasonic real-time images of uterine tumor datasets with the suggested machine learning model at a 97.8 % accuracy rate utilizing RFC.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"3 ","pages":"Article 100029"},"PeriodicalIF":0.0,"publicationDate":"2024-05-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X24000057/pdfft?md5=b0ec160d7302bc75f048a1a6eb6c44b8&pid=1-s2.0-S2949771X24000057-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140918528","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":"Studies on the thermal behavior of sildenafil citrate","authors":"Francisco V.B. Nascimento,&nbsp;Ana P.G. Ferreira,&nbsp;Rafael T. Alarcon,&nbsp;Éder T.G. Cavalheiro","doi":"10.1016/j.jpbao.2024.100028","DOIUrl":"https://doi.org/10.1016/j.jpbao.2024.100028","url":null,"abstract":"<div><p>Thermal behavior of sildenafil citrate (SC), a vasodilator used in the treatment of both erectile dysfunction (ED) and pulmonary arterial hypertension (PAH) treatment was investigated by thermogravimetry-differential thermal analysis (TGA-DTA), differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD) and evolved gas analysis by thermogravimetry coupled to infrared spectroscopy (TGA-FTIR). Under N₂ and air atmospheres SC remained thermally stable until 180.0 °C, and then decomposed in three steps under N₂ and four steps under air. DSC curves showed two endothermic events at first heating, one related to the dehydration around 63.5 °C and the second event is a concomitant melting-decomposition process (T_{<em>peak</em>} = 199.6 °C). Cold recrystallization was observed during the second heating, with peaks at 119.8 °C and 129.7 °C and melting at 179.7 °C. XRD results for powder collected at 138 °C suggested that the phase formed is the sildenafil free base. TGA-FTIR revealed that the thermal decomposition of SC initiates with release of water, carbon dioxide, and itaconic anhydride, resulting from the decomposition of the citrate counter-ion. Above 303 °C, CO, SO₂, benzene, ethanol, 1-methylpiperazine, isocyanic acid, and methylamine were identified in the gas phase. Based on these results, a thermal behavior mechanism for sildenafil citrate was proposed.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"3 ","pages":"Article 100028"},"PeriodicalIF":0.0,"publicationDate":"2024-04-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X24000045/pdfft?md5=134e435dc2a8a6224a704fbdbde2b6aa&pid=1-s2.0-S2949771X24000045-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140539168","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":"Mitigating matrix effects for LC-MS/MS quantification of nitrosamine impurities in rifampin and rifapentine","authors":"Qiyao Li ,&nbsp;Qun Xu ,&nbsp;Nadine Lo ,&nbsp;Allan T. Leeks Jr. ,&nbsp;Mark Han ,&nbsp;Marcela Nefliu ,&nbsp;John T. Simpson ,&nbsp;Jennifer L. Belsky","doi":"10.1016/j.jpbao.2024.100027","DOIUrl":"https://doi.org/10.1016/j.jpbao.2024.100027","url":null,"abstract":"<div><p>Since the discovery of potentially mutagenic nitrosamine impurities in pharmaceuticals in 2018, liquid chromatography-mass spectrometry (LC-MS) methods have been widely applied for the trace level quantification of nitrosamines. As more nitrosamines and drug samples are analyzed, method accuracy is increasingly recognized as a major analytical challenge. Matrix effects can have a significant adverse impact on method accuracy but have not attracted much attention in nitrosamine quantification literature. In this study, we observed severe matrix effects when adapting LC-MS method conditions from a published and validated method for the analysis of nitrosamines in tuberculosis drugs. Several approaches were explored to mitigate these matrix effects, including using stable isotope-labeled internal standards, modifying LC conditions and sample concentration, and quantifying with standard addition instead of an external calibration method. The results underscore the importance of monitoring matrix effects and validating nitrosamine quantification procedures for specific sample matrices. Finally, two LC-MS/MS methods are presented with validation data for the quantification of 1-methyl-4-nitrosopiperazine (MNP) in rifampin and 1-cyclopentyl-4-nitrosopiperazine (CPNP) in rifapentine and revealed high nitrosamine levels in the tested samples that far exceeded recommended acceptable intake limits.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"3 ","pages":"Article 100027"},"PeriodicalIF":0.0,"publicationDate":"2024-02-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X24000033/pdfft?md5=943d4b0163ce944a7c98d3f4e92c1d2d&pid=1-s2.0-S2949771X24000033-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139987016","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":"Synthesis of biowaste-derived nanostructured material for the nanomolar detection of glucose: Biological sample analysis","authors":"Shweta J. Malode ,&nbsp;Shireesha Bilagi ,&nbsp;Nagaraj P. Shetti","doi":"10.1016/j.jpbao.2024.100026","DOIUrl":"https://doi.org/10.1016/j.jpbao.2024.100026","url":null,"abstract":"<div><p>Glucose electro-oxidation in an alkaline media was investigated using an electrode composed of carbon paste and sugarcane bagasse activated carbon (SBAC). The SBAC was prepared using an easy, affordable, and environmental friendly process. The porous activated carbon was produced using sugarcane bagasse through a pre-treatment process that involved carbonization at 650 °C and K₂CO₃. X-ray diffraction (XRD) was used to observe the formation of carbon crystallites during activation at higher temperatures. The Fourier-transform infrared (FTIR) spectrum shows functional groups that are present in the carbon material. The carbon sample's morphology was evaluated using scanning electron microscope (SEM). The surface roughness was studied using atomic force microscopy (AFM). Porous activated carbon derived from sugarcane bagasse was carefully mixed into electrode components such as graphite powder and mineral oil for glucose (GLS) detection. For precise GLS detection, the SBACs were employed as non-enzymatic electrochemical sensor probes in their as-prepared condition. According to the electrochemical experiments, the constructed sensor shows exceptional electrochemical performance towards glucose oxidation, including excellent selectivity, a low detection limit, good sensitivity, and a wide linear range. Investigation has been conducted on the oxidation of GLS in alkaline solutions with varying concentrations of halide ions such as iodide and chloride. The GLS oxidation peak current increased the performance of a SBAC modified electrode was compared to that of a bare carbon paste electrode (CPE). The role of sensitivity in minimizing halide poisoning is significant. The risk of poisoning is increased if iodide &gt; chloride. As the modified electrode's voltage changes in a chloride solution containing glucose, the peak current gradually reduces. The redesigned electrode that is currently in use as a consequence not only promotes glucose oxidation but also shows strong resistance to electrode poisoning caused by halides. The sensitive and targeted SBAC/CPE has also improved its reliability while evaluating samples of human serum, urine, and breast milk.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"3 ","pages":"Article 100026"},"PeriodicalIF":0.0,"publicationDate":"2024-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X24000021/pdfft?md5=5af6905d7f946aac73c3319cc9e20fb4&pid=1-s2.0-S2949771X24000021-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139987015","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":"Validation of a sensitive bioanalytical method for metronidazole extraction from human plasma","authors":"Krishna Kumar Patel ,&nbsp;Valeria Cota ,&nbsp;Nicole K. Brogden","doi":"10.1016/j.jpbao.2024.100025","DOIUrl":"https://doi.org/10.1016/j.jpbao.2024.100025","url":null,"abstract":"<div><p>Metronidazole (MTZ) is a broad-spectrum antibiotic with numerous routes of administration, including topical. Topical application of MTZ gel or cream results in very low systemic absorption, resulting in the need for a sensitive extraction method to quantify plasma concentrations. Currently published methods are not suitable for analysis of plasma concentrations after topical application, as undetectable MTZ concentrations commonly occur. We validated a simple extraction method for MTZ recovery from plasma and quantified it using an LC-MS/MS analytical method. Methods: Plasma samples were spiked with MTZ (0.5 – 5 ng/mL) and internal standard (tinidazole, 2 ng/mL). MTZ was extracted by liquid-liquid extraction using ethyl acetate and acetonitrile mixture (4:1) as the extraction solvent. A quadrupole mass spectrometer interfaced with an Acquity H-Class HPLC was used to quantify MTZ concentrations in positive ion mode. A Kinetix C18 analytical column (150 mm × 4.6 mm i.d., 5 µm particle size) was used for separation. The plasma extraction method was validated for various parameters, including % recovery, precision, accuracy, and stability. Results: The extraction method demonstrated high MTZ recovery, ranging from 93.7 – 97.5%. The calibration curve prepared using MTZ samples extracted from plasma (0.5 – 5 ng/mL) had excellent linearity with R² = 0.999. The extracted samples also showed higher autosampler and freeze-thaw stability over a 72-hr period. The mean intra- and inter-day accuracy and precision of the extraction assay ranged from 97 to 101.6% and 2.7 – 4.8% RSD, respectively. The assay was highly efficient, with a limit of quantification (0.53 ± 0.04 ng/mL) lower than previously published methods (≥5 ng/mL). The extraction method was successfully validated using LC-MS/MS and can be used to extract and detect trace amounts of MTZ in plasma after topical application.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"3 ","pages":"Article 100025"},"PeriodicalIF":0.0,"publicationDate":"2024-02-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X2400001X/pdfft?md5=9b688a9f3a812c65521b6f8b3ea5aeb2&pid=1-s2.0-S2949771X2400001X-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139714996","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":"Comparative physicochemical and biological characterization of the similar imiglucerase product Glurazyme® and the originator product Cerezyme®","authors":"Maksim Smolov,&nbsp;Serge Taran,&nbsp;Ivan Lyagoskin,&nbsp;Maria Neronova,&nbsp;Maksim Degterev,&nbsp;Rakhim Shukurov","doi":"10.1016/j.jpbao.2023.100024","DOIUrl":"10.1016/j.jpbao.2023.100024","url":null,"abstract":"<div><p>A biosimilar considered as a biomolecule medicinal product that is comparable to a reference medicinal product in terms of the structural, functional, biological, and clinical attributes. Glurazyme® was developed as a biosimilar to Cerezyme® (imiglucerase) and was approved in CIS countries (Russian Federation, Belarus, Kazakhstan) and recently Algeria for the treatment of type 1 and type 3 Gaucher disease. The quality assessment of Glurazyme® was performed in accordance with the Rules for the Study of Biological Medicines of the Eurasian Economic Union harmonized with the ICH comparability guideline and the biosimilar guidelines of the European Medicines Agency and Food and Drug Administration. Extensive side-by-side comparison was employed with state-of-the-art and orthogonal assays designed to interrogate all expected physicochemical and biological activities, including those known to affect the mechanisms of action for imiglucerase. Similarity evaluation was performed on the basis of tolerance intervals determined from about 10 lots of commercial Cerezyme®. Mainly three discrepancies of quality attributes were established concerning oxidized and deamidated forms as well as phosphorylated oligomannose N-glycans reflecting the difference between cultivation and down-stream processes of both medicinal products. Nevertheless, all of them possess a little or no influence on safety and efficacy.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"3 ","pages":"Article 100024"},"PeriodicalIF":0.0,"publicationDate":"2023-12-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X23000245/pdfft?md5=af72c4a69d296aaef6a235848c9bb9e1&pid=1-s2.0-S2949771X23000245-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139014105","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 novel approach to determine residual aldehyde content in conjugated polysaccharides with 3-methyl-2-benzothiazolinonehydrazon (MBTH) by colorimetric method, automation, and HP-SEC","authors":"Weidong Tong,&nbsp;Mingxiang Lin,&nbsp;Ping Zhuang,&nbsp;Bukuru Anaclet,&nbsp;Castle Cooper","doi":"10.1016/j.jpbao.2023.100022","DOIUrl":"https://doi.org/10.1016/j.jpbao.2023.100022","url":null,"abstract":"<div><p>Polysaccharide activation by periodate oxidation to form aldehydes, followed by conjugation with proteins via reductive amination is a general procedure to make polysaccharide-protein conjugate vaccines. Controlling the level of residue aldehyde content after conjugation is critical to ensure vaccine product stability. Herein, to support conjugation process optimization, we developed a 3-methyl-2-benzothiazolone hydrazone (MBTH) chemistry-based colorimetric method, which can measure low-level residual aldehyde polysaccharide-protein conjugate in high throughput 96-well plate format. This mechanism of detection works in two steps. First, MBTH reacts with the aldehyde group to form azine. Then the excess MBTH was oxidized by ferric ammonium sulfate in sulfamic acid to form a reactive cation, which reacts further with azine to form formazan, a characteristic blue chromophore at 610 nm, for colorimetric detection. The method performance, including detection limit, linearity range, matrix effect, kinetics, and color stability was systematically studied. For samples with severe matrix interference, a supplemental size exclusion chromatography (SEC) method was also developed as an alternative method.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"2 ","pages":"Article 100022"},"PeriodicalIF":0.0,"publicationDate":"2023-11-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X23000221/pdfft?md5=eafa9469ba2f3683e089c099514af195&pid=1-s2.0-S2949771X23000221-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"136968400","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 of a LC–MS/MS analytical method of 15 compounds related to renal function for a prognostic method of progression risk in patients with diabetic kidney disease","authors":"Ryota Kujirai ,&nbsp;Yotaro Matsumoto ,&nbsp;Mizuki Abe ,&nbsp;Kodai Hiramoto ,&nbsp;Takumi Watanabe ,&nbsp;Chitose Suzuki ,&nbsp;Takafumi Toyohara ,&nbsp;Takaaki Abe ,&nbsp;Yoshihisa Tomioka","doi":"10.1016/j.jpbao.2023.100021","DOIUrl":"10.1016/j.jpbao.2023.100021","url":null,"abstract":"<div><p>Diabetic kidney disease (DKD) onset and progression is a major cause of end-stage renal failure in diabetic patients, however, no practical method has been reported to predict the progression rate of renal function decline. Nine serum compounds are reported to associate with prognosis in type 1 diabetes patients; however, quantitative analytical methods for these compounds lacks. Herein, we developed a simultaneous quantitative method for 15 compounds, including Niewczas’s nine biomarker candidates, associated with renal function and its prognosis in kidney disease patients to achieve a prognostic method of renal function decline in DKD patients. This report describes the development and validation of a LC–MS/MS analytical method for 15 compounds of biomarker candidates using human plasma, serum, and urine as sample matrices. The analytes are N-acetyl-L-alanine, N6-acetyl-L-lysine, N-acetyl-L-serine, N-acetyl-L-threonine, phenyl sulfate, pseudouridine, N6-threonylcarbamoyladenosine, tryptophan 2-C-mannoside, tyrosine O-sulfate, creatinine, p-cresol sulfate, 4-ethylphenyl sulfate, indoxyl sulfate, N1-methyladenosine, and trimethylamine N-oxide. The Capcell Pak ADME-HR column was compared to several general columns and selected as the most suitable column for the simultaneous analysis of all 15 compounds. The proposed method was validated for selectivity, accuracy, precision, stability, dilution integrity, and parallelism. This report describes the suitability of the calibration ranges established and the actual sample concentrations of serum and urine from type 2 diabetic patients, as well as new findings on the unknown analyte levels of several compounds in these samples. The proposed method can be used to aid the development of prognostic methods for renal function decline in patients with DKD.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"2 ","pages":"Article 100021"},"PeriodicalIF":0.0,"publicationDate":"2023-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X2300021X/pdfft?md5=f0b7f3218761bed3d45465c43370fd8d&pid=1-s2.0-S2949771X2300021X-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135371227","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}