Journal of Pharmaceutical and Biomedical Analysis Open最新文献

{"title":"Enantioseparation of new axially chiral carboxylic acids on polysaccharide-based chiral stationary phases under normal phase elution conditions","authors":"Barbara Sechi ,&nbsp;Victor Mamane ,&nbsp;Roberto Dallocchio ,&nbsp;Alessandro Dessì ,&nbsp;Sergio Cossu ,&nbsp;Giorgi Jibuti ,&nbsp;Paola Peluso","doi":"10.1016/j.jpbao.2023.100011","DOIUrl":"https://doi.org/10.1016/j.jpbao.2023.100011","url":null,"abstract":"<div><p>In the last decade, the availability of new and versatile synthetic strategies for the preparation of substituted 4,4’-bipyridyl derivatives based on chemo- and regioselective functionalization of the 4,4’-bipyridine core has encouraged studies for exploring the bioactivity of these compounds in the fields of drug discovery and medicinal chemistry. In substituted 4,4’-bipyridines, chirality may emerge from restricted rotation induced by sterically hindered atoms or functional groups located around the 4,4’-biaryl bond (chiral axis). The first atropisomeric substituted 4,4’-bipyridine was prepared in 2008, and no asymmetric synthesis to produce pure atropisomers of chiral 4,4’-bipyridine derivatives has been available so far. Thus, in the last few years, our groups developed methods to separate atropisomers of a wide series of 4,4’-derivatives by high-performance liquid chromatography (HPLC) using polysaccharide-based chiral stationary phases (CSPs). In the frame of our interest in this field, we reported herein the synthesis of two new chiral carboxylic acids containing an axially chiral 4,4’-bipyridyl unit as source of chirality, and their HPLC enantioseparation on polysaccharide-based CSPs. In particular, the impact of analyte and CSP structures on the enantioseparation outcomes as well as mechanisms and noncovalent interactions underlying the enantioseparation were explored by using electrostatic potential analysis and molecular dynamics (MD) simulations.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"1 ","pages":"Article 100011"},"PeriodicalIF":0.0,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49883946","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":"Analysis of perfluoroalkyl substances (PFAS) in conventional and unconventional matrices: Clinical outcomes","authors":"Alessandro Di Giorgi ,&nbsp;Nunzia La Maida ,&nbsp;Omayema Taoussi ,&nbsp;Simona Pichini ,&nbsp;Francesco Paolo Busardò ,&nbsp;Anastasio Tini ,&nbsp;Annagiulia Di Trana","doi":"10.1016/j.jpbao.2023.100002","DOIUrl":"https://doi.org/10.1016/j.jpbao.2023.100002","url":null,"abstract":"<div><p>Since 1950, the use of perfluoroalkyl substances (PFAS) increased due to their heat resistance, lipophobic and hydrophobic properties; therefore, these compounds are widely employed to make waterproof and heat resistant coatings, such as food packaging or work wear. However, these chemicals represent a risk to the environment due to their stability to degradation. Moreover, these compounds properties represent a risk also for humans; many studies correlated their concentrations in biological matrices to pathologies, such as hypertension, diabetes, and cancer. To this concern, the analytical detection in different biological matrices plays a crucial role to assess the presence of such analytes in different body districts. We performed a literature search in different scientific databases to review articles reporting the application of PFAS analysis for human exposure monitoring and for possible association with pathologies. The search resulted in 58 studies investigating PFAS presence in conventional matrices, such as blood and urine, and unconventional matrices. Although the solid-phase extraction was preferred for all the considered matrices, liquid-liquid extraction and dilute and shot demonstrated to be suitable extraction approach. The most used instrumental technique was the LC-MS/MS equipped with C18 chromatographic column, electrospray injection source operating in negative mode, and multiple reaction monitoring spectrometric acquisition. The untargeted detection of PFAS was attempted using an LC-HRMS method to elucidate possible new compound structures. Notably, the instruments and laboratory tools may represent an important contamination source due to the PFAS presence in their constituents. The development of an analytical method able to reach low limits of detection (LOD) and suitable for different biological matrices is crucial to study both PFAS health effects and a possible pharmacokinetics. For this purpose, current knowledge about PFAS analytical methods in biological matrices applied to human biomonitoring and pathology studies is reviewed to raise awareness of these chemicals’ activities.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"1 ","pages":"Article 100002"},"PeriodicalIF":0.0,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49883948","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":"Characterization and validation of a middle-down hydrophobic interaction chromatography method to monitor methionine oxidation in IgG1","authors":"Somar Khalil ,&nbsp;Nisha Patel ,&nbsp;Francoise Bevillard-Kumar ,&nbsp;Cyrille Chéry ,&nbsp;William Burkitt ,&nbsp;John O’Hara ,&nbsp;Annick Gervais","doi":"10.1016/j.jpbao.2023.100008","DOIUrl":"https://doi.org/10.1016/j.jpbao.2023.100008","url":null,"abstract":"<div><p>Post-translational modifications (PTMs) of therapeutic monoclonal antibodies (mAbs) can impact the efficacy of a drug. Methionine oxidation can alter the overall hydrophobicity of an antibody, thereby inducing conformational changes and affecting its biological activity. To ensure high quality, safety, and efficacy of mAbs, routine monitoring of PTMs such as methionine (Met) oxidation is essential. Met oxidation in the fragment crystallizable (Fc) region of immunoglobulin-G1 (IgG1) is a potential critical quality attribute because it impacts not only the interaction with the neonatal Fc receptor and protein A but also the half-life of mAbs in serum circulation. Although bottom-up mass spectrometry provides high site specificity, it may have limited application in quality control workflows, and its complicated sample preparation could result in procedure-induced oxidation. In this study, we describe the development and characterization of a rapid and robust middle-down hydrophobic interaction chromatography method for monitoring Met oxidation in the Fc region of IgG1. Additionally, we assessed a comprehensive method validation package and demonstrated the specificity, linearity, precision, and accuracy of the new method within a range of 3.8–37.7%. The relative quantitative data provided by this method may be used in a regulated workflow to support process and formulation development as well as in the later stages of drug development and batch release and stability studies.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"1 ","pages":"Article 100008"},"PeriodicalIF":0.0,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49883935","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 a three-dimensional HPLC system for acidic amino acid enantiomers and determination of their amounts in mice lacking D-aspartic acid oxidase activity","authors":"Chiharu Ishii ,&nbsp;Rin Morinaga ,&nbsp;Miho Takahashi ,&nbsp;Masashi Mita ,&nbsp;Takeyuki Akita ,&nbsp;Kenji Hamase","doi":"10.1016/j.jpbao.2023.100004","DOIUrl":"https://doi.org/10.1016/j.jpbao.2023.100004","url":null,"abstract":"<div><p>A highly-selective three-dimensional (3D) HPLC system has been designed/developed for the determination of acidic amino acid enantiomers, i.e., aspartic acid (Asp) and glutamic acid (Glu). The 3D-HPLC system consisted of a reversed-phase column (Singularity RP18, 1.0 ×250 mm) in the first dimension, a mixed-mode column (Singularity MX-001, 1.5 ×250 mm) in the second dimension and a Pirkle-type enantioselective column (Singularity CSP-011S, 1.5 ×250 mm) in the third dimension. By using this system, the amounts of Asp and Glu enantiomers in 6 tissues (cerebrum, heart, lung, liver, kidney and testis) and 2 physiological fluids (plasma and urine) were determined in the control C57BL/6J mice and B6DDO^-/- mice lacking <span>D</span>-aspartic acid oxidase activity. In the control C57BL/6J mice, a high amount of <span>D</span>-Asp (466.15 nmol/g) was observed in the testis, and relatively high amounts of <span>D</span>-Asp were observed in the cerebrum, lung, liver and kidney (21.40–92.87 nmol/g). In the heart and 2 physiological fluids, the amounts of <span>D</span>-Asp were low (trace–7.75 nmol/g or mL). In the B6DDO^-/- mice, the amounts of <span>D</span>-Asp drastically increased in all the tissues and physiological fluids. In contrast to the results of <span>D</span>-Asp, the amounts of <span>D</span>-Glu did not change depending on the alteration of the DDO activity, and the amounts were extremely low and not detectable in most of the tested tissues and physiological fluids. Although the amounts of <span>D</span>-Glu were low, it is noteworthy that clear localization in the testis (8.60–9.53 nmol/g) was demonstrated in both the C57BL/6J and B6DDO^-/- mice.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"1 ","pages":"Article 100004"},"PeriodicalIF":0.0,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49883904","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":"Efficient screening of anti-idiotype DNA aptamers that bind specifically to trastuzumab for bioanalytical applications","authors":"Kenichiro Todoroki ,&nbsp;Jiaxing Tong ,&nbsp;Moe Aoki ,&nbsp;Nao Kobayashi ,&nbsp;Ryota Isobe ,&nbsp;Hiroyuki Tasaki ,&nbsp;Tomohiro Yamada ,&nbsp;Aogu Furusho ,&nbsp;Eiji Sugiyama ,&nbsp;Hajime Mizuno ,&nbsp;Hideki Hayashi ,&nbsp;Toshimasa Toyo’oka","doi":"10.1016/j.jpbao.2023.100006","DOIUrl":"https://doi.org/10.1016/j.jpbao.2023.100006","url":null,"abstract":"<div><p>We have developed a novel aptamer discovery method that rapidly and efficiently yields anti-idiotypic DNA aptamers for trastuzumab using fast protein liquid chromatography (FPLC) separation and large amounts of DNA. The use of large amounts of oligo DNA allowed us to obtain more aptamer candidates without PCR amplification within only two days. Quartz crystal microbalance (QCM) measurements confirmed that the obtained anti-trastuzumab aptamer had a high affinity with a <em>K</em>_D of 120.0 nM and 97.7 nM at pH 6.0 and 7.4, respectively. Molecular docking simulations suggested that this sequence has high specificity and binding affinity to multiple sites in the complementarity-determining region of trastuzumab. The <em>K</em>_D increased to 11.4 nM due to avidity expression after dense immobilization in the QCM sensor cell, indicating that this anti-trastuzumab aptamer is applicable as a capture molecule in the ligand binding assay.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"1 ","pages":"Article 100006"},"PeriodicalIF":0.0,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49883934","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":"Combination quantitative 1H NMR and chemometric approaches for the assessment of quality control in commercially available products of red fruit (Pandanus conoidues, Lam.) oil","authors":"Liling Triyasmono ,&nbsp;Ulrike Holzgrabe","doi":"10.1016/j.jpbao.2023.100010","DOIUrl":"https://doi.org/10.1016/j.jpbao.2023.100010","url":null,"abstract":"<div><p>The assessment of fat acid parameters (acid value, saponification value, ester value, iodine value, composition of monounsaturated fatty acids, polyunsaturated fatty acids, and total unsaturated fatty acids) in edible oils, including red fruit oil, delivers essential indices to guarantee their quality. This index also holds true for excipients as well as for traditional medicines. NMR spectroscopy is an alternative tool to the conventional methods for the determination of these quality parameters, offering attractive advantages. Here, the approach reported in the literature based on the ¹H NMR quantitative method is illustrated, highlighting the application procedure strategy and suggested sample processing. Chemometric applications on ¹H NMR spectra are also discussed. Furthermore, this review can support the role of ¹H NMR and chemometrics in routine analysis for oil quality control.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"1 ","pages":"Article 100010"},"PeriodicalIF":0.0,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49883937","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":"Recent applications of the derivatization techniques in capillary electrophoresis","authors":"Roberto Gotti ,&nbsp;Benedetta Pasquini ,&nbsp;Serena Orlandini ,&nbsp;Sandra Furlanetto","doi":"10.1016/j.jpbao.2023.100003","DOIUrl":"https://doi.org/10.1016/j.jpbao.2023.100003","url":null,"abstract":"<div><p>The main reasons for performing derivatization in capillary electrophoresis are largely the same as for liquid chromatography, however there are specific aspects in electrokinetic separations where derivatization plays specific roles. The review is focused on the articles published in the past 5 years with the aim to highlight this unicity. Derivatization is mainly applied to improve the inherent low sensitivity of capillary electrophoresis when optical detection is used and the introduction of originally developed derivatization approaches have been addressed mainly to the detection by laser-induced fluorescence. A further peculiarity concerns the development of automatized as well as in-capillary derivatization that can be performed using the commercially available instrumentation. The majority of the methods considered deal with the derivatization of amine group in small molecules (in particular, amino acids) as well as in proteins and peptides. Applications are also addressed to chiral analysis and for trapping unstable and reactive small molecules and inorganic ions. The analysis of proteins and saccharides in glycomics, have been covered in dedicated sections.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"1 ","pages":"Article 100003"},"PeriodicalIF":0.0,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49883905","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":"Determination of carbamazepine and its main metabolite in human hair by capillary electrophoresis and liquid chromatography techniques, both coupled with mass spectrometry","authors":"Aneta Woźniakiewicz,&nbsp;Renata Wietecha-Posłuszny","doi":"10.1016/j.jpbao.2023.100009","DOIUrl":"https://doi.org/10.1016/j.jpbao.2023.100009","url":null,"abstract":"<div><p>The aim of the research was to determine carbamazepine (CBZ) and its main metabolite 10,11-epoxy-10,11-dihydro-carbamazepine (CBZ-E) in human hair using the capillary electrophoresis (CE) system coupled with mass spectrometry detection (MS) and to compare the obtained results with the liquid chromatography (LC) technique, also coupled with the MS detector. Hair samples were prepared using microwave-assisted extraction (MAE) at 60 °C for 10 min in an alkaline solution (pH = 10) with ethyl acetate as the extraction solvent. In the frame of this study, the procedure for the separation of CBZ and CBZ-E using the CE-MS technique was developed. The best results were achieved using 10 mM ammonium acetate (pH=6.8) as the background electrolyte (BGE), after filling the capillary with 1% highly sulfonated β-cyclodextrin (HSβCD) in 10 mM ammonium acetate. Then, the validation parameters of the MAE/CE-MS and MAE/LC-MS methods such as: limit of detection (for CBZ are: 0.36 and 0.22 ng/mg, respectively; for CBZ-E 0.38 and 0.17 ng/mg, respectively), limit of quantification (for CBZ are: 0.86 and 0.72 ng/mg, respectively; for CBZ-E 0.94 and 0.56 ng/mg, respectively), precision (6.91–14.5% and 2.16–15.6%, respectively), recovery (87.7–102.7% and 88.9–105.5%, respectively), and matrix effect (99.5–111.0% and 98.9–115.1%, respectively) were defined and compared. Finally, the validated methods were applied to identify and quantify carbamazepine and its metabolite in hair in patients who received CBZ for medical reasons.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"1 ","pages":"Article 100009"},"PeriodicalIF":0.0,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49883936","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":"Comparison of the use of 6-thioguanine riboside versus 6-thioguanine as calibration standard to monitor 6-thioguanine nucleotides in red blood cells","authors":"Roselyne Boulieu ,&nbsp;Antoine Tourlonias ,&nbsp;Magali Larger","doi":"10.1016/j.jpbao.2023.100007","DOIUrl":"https://doi.org/10.1016/j.jpbao.2023.100007","url":null,"abstract":"<div><p>The analytical methods reported to evaluate 6-Thioguanine nucleotides (6-TGNs) level in red blood cells (RBC) are based on the conversion of 6-TGNs to 6-Thioguanine (6-TG) using 6-thioguanine as calibration standard.</p><p>Using the LC-DAD method previously reported by Dervieux and Boulieu in 1998 to determine 6-TGNs, we evaluated the use of 6-Thioguanine Riboside (6-TGR) as standard instead of the base 6-TG for the monitoring of 6-TGNs in RBC from patients with IBD.</p><p>Our results show that 6-TGN values measured in RBC from 30 patients were significantly (p &lt; 0,00001) higher when 6-TGR was used as calibration standard compared to 6-TG. The difference observed may be explained by the presence of ribose in the chemical structure of 6-TGR contrary to 6-TG. This difference in 6-TGN values was also observed in external quality control assay using 6-TGR versus 6-TG calibration standard.</p><p>The use of the nucleoside 6-TGR as calibrator constitutes a better reflection of the chemical reaction which occurs in RBC compared to 6-TG. This preliminary observation suggests that the choice of calibration standard to monitor 6-TGNs may have a significant impact on the values measured in patients and laboratory should be aware of this potential pitfall.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"1 ","pages":"Article 100007"},"PeriodicalIF":0.0,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49885071","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}