Journal of pharmaceutical and biomedical analysis最新文献

{"title":"Development and validation of a liquid chromatography-tandem mass spectrometry method for the determination of polymixin B1, B2, ile-B1, E1, and E2 in human plasma and its clinical pharmacokinetic application","authors":"","doi":"10.1016/j.jpba.2024.116403","DOIUrl":"10.1016/j.jpba.2024.116403","url":null,"abstract":"<div><p>Polymyxin B (PB) and Polymyxin E (PE, also called colistin) are used as the last treatment resort for multidrug-resistant Gram-negative bacterial infections. The nephrotoxicity and neurotoxicity of polymyxins limit their clinical use, and guidelines recommend therapeutic drug monitoring (TDM) to optimize efficacy and reduce toxicity. However, there are limited analytical methods available for the determination of PB and PE. This study aimed to develop a simple and robust liquid chromatography with tandem mass spectrometry (LC-MS/MS) analytical method for determining the main compounds of PB and PE, namely PB1, PB2, ile-PB1, PE1, and PE2, in human plasma and to investigate of their pharmacokinetics in critically ill patients with the use of PB and PE, respectively. Plasma PB1, PB2, ile-PB1, PE1, and PE2 were chromatographically separated on a Welch LP-C18 column and detected using electrospray ionization mode coupled with multiple reaction monitoring. The calibration curve showed acceptable linearity over 20–10,000 ng/mL for PB1, PE1, and PE2 and 10–5000 ng/mL for PB2 and ile-PB1 in the plasma, respectively. After validation following approved guidelines, this method was successfully applied for PB and PE pharmacokinetic analysis and TDM in critically ill patients. Additionally, the composition of PB1, PB2, ile-PB1, PE1, and PE2 remains unchanged from 0 to 12 h after entering the patient’s body.</p></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":null,"pages":null},"PeriodicalIF":3.1,"publicationDate":"2024-08-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141906899","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":"Proteomic analysis reveals the mechanism that low molecular weight hyaluronic acid enhances cell migration in keratinocyte","authors":"","doi":"10.1016/j.jpba.2024.116402","DOIUrl":"10.1016/j.jpba.2024.116402","url":null,"abstract":"<div><p>Hyaluronic acid (HA), as an extracellular matrix, is known to promote wound healing, and its bioactivity is affected by molecular weight. However, the mechanism of LMW-HA on cells migration remains unclear. In this study, we investigated the effect of LMW-HA on cells migration and the underlying mechanism by employing proteomics. The scratch assay showed that LMW-HA can significantly enhance the migration of keratinocytes in vitro, and ten differentially expressed proteins (DEPs) were found to be associated with wound healing through proteomics and network pharmacology. The result of bioinformatic analysis indicated that these DEPs are involved in positive regulation of cell motility and cellular component movement. Moreover, protein targets of key pathways were further validated. The findings suggest that LMW-HA can promote wound healing by accelerating epithelization via the HIF-1α/VEGF pathway, which provides new insight and reference for HA to enhance cells migration.</p></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":null,"pages":null},"PeriodicalIF":3.1,"publicationDate":"2024-08-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141990769","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 simplified non-reduced peptide mapping method with faster and efficient enzymatic digestion for characterization of native disulfide bonds in monoclonal and bispecific antibodies","authors":"","doi":"10.1016/j.jpba.2024.116400","DOIUrl":"10.1016/j.jpba.2024.116400","url":null,"abstract":"<div><p>Development of monoclonal and bispecific antibody-based protein therapeutics requires detailed characterization of native disulfide linkages, which is commonly achieved through peptide mapping under non-reducing conditions followed by liquid chromatography-mass spectrometry (LC-MS) analysis. One major challenge of this method is incomplete protein digestion due to insufficient denaturation of antibodies under non-reducing conditions. For a long time, researchers have explored various strategies with the aim of efficiently digesting antibody drugs when the disulfide bonds remain intact, but few could achieve this by using a simple and generic approach with well controlled disulfide scrambling artifacts. Here, we report a simple method for fast and efficient mapping of native disulfides of monoclonal and bispecific antibody-based protein therapeutics. The method was optimized to achieve optimal digestion efficiency by denaturing proteins with 8 M urea plus 0–1.25 M guanidine-HCl at elevated temperature (50 °C), followed by two-step digestion with trypsin/Lys-C mix using a one-pot reaction. The only parameter that needs to be optimized for different proteins is the concentration of guanidine-HCl present. This simplified sample preparation eliminated buffer exchange and can be completed within three hours. By using this new method, all native disulfide bonds were confirmed for these monoclonal and bispecific antibodies with high confidence. When compared with a commercial kit utilizing low-pH digestion condition, the new method demonstrated higher digestion efficiency and shorter sample preparation time. These results suggest this new one-pot-two-step digestion method is suitable for the characterization of antibody disulfide bonds, particularly for those antibodies with digestion-resistant domains under typical digestion conditions.</p></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":null,"pages":null},"PeriodicalIF":3.1,"publicationDate":"2024-08-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S0731708524004400/pdfft?md5=e543da510c0f8d10a77ffb4ffa5daaa4&pid=1-s2.0-S0731708524004400-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141913045","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":"Tyrosine and tryptophan in urine as biomarkers for prostate cancer: A validation study","authors":"","doi":"10.1016/j.jpba.2024.116398","DOIUrl":"10.1016/j.jpba.2024.116398","url":null,"abstract":"<div><p>Prostate cancer (PCa) is a common male malignancy and early diagnosis is crucial for successful treatment. The current study aims to validate results from a pilot study that demonstrated an inverse association between urine tyrosine and tryptophan levels and the severity of PCa. This study comprised a cohort of 97 patients with benign prostatic hyperplasia, 93 patients diagnosed with localized PCa, 75 patients diagnosed with locally advanced PCa, and 68 patients diagnosed with metastatic PCa. The tyrosine and tryptophan levels in the samples were analyzed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and electrochemical sensors in accordance with the pilot to maintain uniformity for accurately evaluating the data. One-way ANOVA with post Tukey test as well as the Wilcoxon Rank Sum Test were performed. Analyzing 333 patients across PCa stages with consistent methods, we observed no significant differences in tyrosine and tryptophan levels between PCa patients and controls, finally rejecting the use of tyrosine and tryptophan as PCa biomarkers. We did, however, verify the strong correlation between the urinary concentrations of tyrosine and tryptophan found in the pilot study.</p></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":null,"pages":null},"PeriodicalIF":3.1,"publicationDate":"2024-08-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S0731708524004382/pdfft?md5=a7b5c79c960816853ccbd9748ee49f61&pid=1-s2.0-S0731708524004382-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141913059","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Development of a UHPLC-MS/MS method for the quantification of Pristinamycin ⅠA and ⅡA in beagle dog plasma and its pharmacokinetic application","authors":"","doi":"10.1016/j.jpba.2024.116401","DOIUrl":"10.1016/j.jpba.2024.116401","url":null,"abstract":"<div><p>The aim of this study was to develop and fully validate a sensitive and rapid ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for simultaneous quantification of pristinamycin ⅠA (PⅠA) and pristinamycin ⅡA (PⅡA) in plasma of beagle dogs after oral administration of pristinamycin tablets. PⅠA, PⅡA and quinupristin (internal standard, IS) were separated on an Agilent Eclipse Plus C₁₈ column (2.1 mm × 100 mm, 3.5 μm particle size) by using gradient elution consisting of methanol and water (0.1 % formic acid) at a flow rate of 0.4 mL/min in 4.0 min. Multiple reaction monitoring (MRM) mode was performed to quantify data under monitoring precursor-product ion transitions of <em>m/z</em> 867.6→134.1, 548.4→287.1 and 1022.7→133.9 for PⅠA, PⅡA and IS at positive ion mode, respectively. The method was developed at linearity ranging from 1.0 to 1000 ng/mL for all analytes.The accuracy of PⅠA and PⅡA was observed to range between −10.6 % and 7.1 %, while the precision was found to be within 8.9 %. No significant matrix effect was observed. PⅠA and PⅡA demonstrated stability during sample storage, preparation and analytic procedures. Furthermore, this method was successfully applied in the investigation of the pharmacokinetic profile of PⅠA and PⅡA in beagle dogs after oral administration of pristinamycin tablets (75 mg for PⅠA and 175 mg for PⅡA). The biological half-life (t_1/2) was determined to be 1.75 ± 0.07 h and 1.44 ± 0.31 h for PⅠA and PⅡA, respectively. The areas under curves (AUC_0-t) of PⅠA and PⅡA were 80.7 ± 24.6 and 230 ± 94.8 μg/L·h, respectively.</p></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":null,"pages":null},"PeriodicalIF":3.1,"publicationDate":"2024-08-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141990802","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":"Corrigendum to “Dissecting the antitumor effects of Scutellaria barbata: Initial insights into the metabolism of scutellarin and luteolin by gut microbiota” [J. Pharm. Biomed. Anal. 248 (2024) 116325]","authors":"","doi":"10.1016/j.jpba.2024.116393","DOIUrl":"10.1016/j.jpba.2024.116393","url":null,"abstract":"","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":null,"pages":null},"PeriodicalIF":3.1,"publicationDate":"2024-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S0731708524004333/pdfft?md5=e4e82bb61977991864a26d26c492860f&pid=1-s2.0-S0731708524004333-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141897648","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":"Highly accurate single-color fluorogenic DNA decoding sequencing for mutational genotyping","authors":"","doi":"10.1016/j.jpba.2024.116397","DOIUrl":"10.1016/j.jpba.2024.116397","url":null,"abstract":"<div><p>We proposed a single-color fluorogenic DNA decoding sequencing method designed to improve sequencing accuracy, increase read length and throughput, as well as decrease scanning time. This method involves the incorporation of a mixture of four types of 3’-O-modified nucleotide reversible terminators into each reaction. Among them, two nucleotides are labeled with the same fluorophore, while the remaining two are unlabeled. Only one nucleotide can be extended in each reaction, and an encoding that partially defines base composition can be obtained. Through cyclic interrogation of a template twice with different nucleotide combinations, two sets of encodings are sequentially obtained, enabling the determination of the sequence. We demonstrate the feasibility of this method using established sequencing chemistry, achieving a cycle efficiency of approximately 99.5 %. Notably, this strategy exhibits remarkable efficacy in the detection and correction of sequencing errors, achieving a theoretical error rate of 0.00016 % at a sequencing depth of ×2, which is lower than Sanger sequencing. This method is theoretically compatible with the existing sequencing-by-synthesis (SBS) platforms, and the instrument is simpler, which may facilitate further reductions in sequencing costs, thereby broadening its applications in biology and medicine. Moreover, we demonstrate the capability to detect known mutation sites using information from only a single sequencing run. We validate this approach by accurately identifying a mutation site in the human mitochondrial DNA.</p></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":null,"pages":null},"PeriodicalIF":3.1,"publicationDate":"2024-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141902072","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":"Comprehensive two-dimensional gas chromatography using a miniaturized multiloop splitter-based non-cryogenic artificial trapping (M-SNAT) modulation device for analysis of cannabis samples","authors":"","doi":"10.1016/j.jpba.2024.116395","DOIUrl":"10.1016/j.jpba.2024.116395","url":null,"abstract":"<div><p>Multiloop splitter-based non-cryogenic artificial trapping (M-SNAT) modulation technique was developed, miniaturized and applied in comprehensive two-dimensional gas chromatography (GC×GC) for analysis of cannabis samples. The approach employed deactivated fuse silica (DFS) columns configured into multiple loop splitter system halving the perimeters of the progressively upstream loops. This splitter device was located between the first (¹D) semi-nonpolar column outlet and a microfluidic Deans switch (DS). Each splitter loop splits a peak into two subpeaks having the same area with different void times. Three loops were then applied resulting in the number of the split subpeaks (<em>n</em>_split) of 8 for each peak, and retention time differences between any two adjacent subpeaks (∆<em>t</em>_R,split) were the same. By applying periodic heartcut event (H/C) within every artificial modulation period (<em>P</em>_AM) of <em>n</em>_split×∆<em>t</em>_R,split, comprehensive split-and-trapped modulation profiles of analytes could be selectively transferred onto the second (²D) polar column (30 m) without cryogen consumption. This artificial modulation system was applied for analysis of cannabis samples with enhanced ²D peak capacity (²<em>n</em>_c∼15). The established method was applied to analyse cannabis extracts using vegetable oils with or without frying process. This reveals 454 different peaks with 76, 92, 35 and 70 specific components specifically observed by using olive oil extraction (OE), fried OE, coconut oil extraction (CE) and fried CE, respectively.</p></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":null,"pages":null},"PeriodicalIF":3.1,"publicationDate":"2024-08-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141906836","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 of an integrated strategy for comprehensive characterization of Sinomenii Caulis extract and metabolites in rats based on UPLC/Q-TOF-MS","authors":"","doi":"10.1016/j.jpba.2024.116391","DOIUrl":"10.1016/j.jpba.2024.116391","url":null,"abstract":"<div><p>Sinomenii Caulis (SC), a commonly used traditional Chinese medicine for its therapeutic effects on rheumatoid arthritis, contains rich chemical components. At present, most studies mainly focus on sinomenine, with little research on other alkaloids. In this study, a comprehensive profile of compounds in SC extract, and biological samples of rats (including bile, urine, feces, and plasma) after oral administration of SC extract was conducted via ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UPLC/Q-TOF-MS). The fragmentation patterns and potential biotransformation pathways of six main types of alkaloids in SC were summarized, and the corresponding characteristic product ions, relative ion intensity, and neutral losses were obtained to achieve rapid classification and identification of complex components of SC from <em>in vitro</em> to <em>in vivo</em>. As a result, a total of 114 alkaloid compounds were identified, including 12 benzyl alkaloids, 4 isoquinolone alkaloids, 32 aporphine alkaloids, 28 protoberberine alkaloids, 34 morphinan alkaloids and 4 organic amine alkaloids. After administration of SC extract to rats, a total of 324 prototypes and metabolites were identified from rat plasma, urine, feces and bile, including 81 aporphines, 95 protoberberines, 117 morphinans and 31 benzylisoquinolines. The main types of metabolites were demethylation, hydrogenation, dehydrogenation, aldehydation, oxidation, methylation, sulfate esterification, glucuronidation, glucose conjugation, glycine conjugation, acetylation, and dihydroxylation. In summary, this integrated strategy provides an additional approach for the incomplete identification caused by compound diversity and low abundance, laying the foundation for the discovery of new bioactive compounds of SC against rheumatoid arthritis.</p></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":null,"pages":null},"PeriodicalIF":3.1,"publicationDate":"2024-08-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141906897","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":"Metabolic profiling of different parts of Physalis alkekengi L. var. franchetii (Mast.) Makino based on UPLC-Q-Orbitrap-HRMS coupled with bioactivity assays","authors":"","doi":"10.1016/j.jpba.2024.116388","DOIUrl":"10.1016/j.jpba.2024.116388","url":null,"abstract":"<div><p><em>Physalis alkekengi</em> L.var. <em>franchetii</em> (Mast.) Makino (PAF) is an important edible and medicinal plant resource in China. Historically, phytochemical studies have primarily examined the calyx and fruit due to their long-standing use in traditional Chinese medicine for their ability to clear heat and detoxify. Metabolites and bioactivities of other parts such as the leaves, stems and roots, are rarely studied. The study involved conducting metabolic profiling of five plant parts of PAF using UPLC-Q-Orbitrap-HRMS analysis, in conjunction with two bioactivity assays. A total of 95 compounds were identified, including physalins, flavonoids, sucrose esters, phenylpropanoids, nitrogenous compounds and fatty acids. Notably, 14 aliphatic sucrose esters, which are potentially novel compounds, were initially identified. Furthermore, one new aliphatic sucrose ester was purified and its structure was elucidated by 1D and 2D NMR analysis. The hierarchical clustering analysis and principal component analysis showed the close clustering of the root and stem, suggesting similarities in their chemical composition, whereas the leaf, calyx and fruit clustered more distantly. Orthogonal partial least-squares discriminant analysis results showed that 41 compounds potentially serve as marker compounds for distinguishing among plant parts. Variations in activity were observed among the plant parts during the comparative evaluation with biological assays. The calyx, leaf and fruit extracts showed stronger antibacterial and anti-inflammatory activities than the stem and root extracts, and 19 potential biomarkers were identified by S-plot analysis for the observed activities, including chlorogenic acid, luteolin, cynaroside, physalin A, physalin F, physalin J, apigetrin, quercetin-3<em>β</em>-D-glucoside and five ASEs, which likely explain the observed potent bioactivity.</p></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":null,"pages":null},"PeriodicalIF":3.1,"publicationDate":"2024-07-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141875155","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}