The isotope-coded derivatization method was developed for the accurate quantification of D/L-serine and D/L-proline in serum by liquid chromatography-single quadrupole mass spectrometry (LC–MS), using our original chiral resolution labeling reagent labeled with the stable isotope 1-fluoro-2,4-dinitrophenyl-5-D-leucine-13C6-N,N-dimethylethylenediamineamide (13C6-D-FDLDA). These D-amino acids are potential biomarkers for Alzheimer’s disease (AD). The method enables straightforward separation and detection of D/L-serine and D/L-proline using an octadecyl (C18) column after liquid–liquid extraction and derivatization. Moreover, the labeled samples remained stable for at least 1 month when stored at 4°C. The concentrations of D-serine (2.07 ± 0.07 μmol/L) and D-proline (1.50 ± 0.04 μmol/L) in the serum of AD patients were higher than those in non-AD (D-serine: 1.80 ± 0.06 μmol/L; D-proline: 0.43 ± 0.03 μmol/L), consistent with findings from previous studies. Extraction recovery rates for each amino acid were within ±15 %, and no carryover was detected immediately after serum sample analysis. Furthermore, this method enables accurate analysis of D/L-serine and D/L-proline in serum with RSD values below 10 % for intra-day and inter-day reproducibility. This method is promising for enabling early and minimally invasive diagnosis of patients with AD.
采用本公司独创的稳定同位素1-氟-2,4-二硝基苯-5-D-亮氨酸- 13c6 - n， n -二甲基乙二胺（13C6-D-FDLDA）手性拆分标记试剂，建立了液相色谱-单四极杆质谱（LC-MS）对血清中D/ l-丝氨酸和D/ l-脯氨酸进行精确定量的同位素编码衍生化方法。这些d -氨基酸是阿尔茨海默病（AD）的潜在生物标志物。该方法采用十八烷基（C18）柱，经液-液萃取衍生化后，可直接分离和检测D/ l -丝氨酸和D/ l -脯氨酸。此外，标记的样品在4°C下保存至少1个月。AD患者血清中d -丝氨酸（2.07 ± 0.07 μmol/L）和d -脯氨酸（1.50 ± 0.04 μmol/L）浓度高于非AD患者（d -丝氨酸：1.80 ± 0.06 μmol/L； d -脯氨酸：0.43 ± 0.03 μmol/L），与既往研究结果一致。每种氨基酸的提取回收率在±15 %以内，血清样品分析后未立即检测到残留。此外，该方法能够准确分析血清中D/ l -丝氨酸和D/ l -脯氨酸，RSD值低于10 %，日间和日间重复性好。该方法有望实现AD患者的早期和微创诊断。
{"title":"Quantitative analysis of D/L-serine and D/L-proline in serum by isotope-coded derivatization using an original chiral resolution labeling reagent","authors":"Makoto Ozaki , Yasunari Yamada , Tsunehisa Hirose , Motoshi Shimotsuma , Akari Ikeda , Takahiro Kawase , Ai Tsuji , Shozo Tomonaga , Miyuki Matsui , Takefumi Kuranaga , Hideaki Kakeya","doi":"10.1016/j.jpbao.2025.100099","DOIUrl":"10.1016/j.jpbao.2025.100099","url":null,"abstract":"<div><div>The isotope-coded derivatization method was developed for the accurate quantification of D/<span>L</span>-serine and D/<span>L</span>-proline in serum by liquid chromatography-single quadrupole mass spectrometry (LC<strong>–</strong>MS), using our original chiral resolution labeling reagent labeled with the stable isotope 1-fluoro-2,4-dinitrophenyl-5-<span>D</span>-leucine-<sup>13</sup>C<sub>6</sub>-<em>N</em>,<em>N</em>-dimethylethylenediamineamide (<sup>13</sup>C<sub>6</sub>-<span>D</span>-FDLDA). These <span>D</span>-amino acids are potential biomarkers for Alzheimer’s disease (AD). The method enables straightforward separation and detection of D/<span>L</span>-serine and D/<span>L</span>-proline using an octadecyl (C<sub>18</sub>) column after liquid–liquid extraction and derivatization. Moreover, the labeled samples remained stable for at least 1 month when stored at 4°C. The concentrations of <span>D</span>-serine (2.07 ± 0.07 μmol/L) and <span>D</span>-proline (1.50 ± 0.04 μmol/L) in the serum of AD patients were higher than those in non-AD (<span>D</span>-serine: 1.80 ± 0.06 μmol/L; <span>D</span>-proline: 0.43 ± 0.03 μmol/L), consistent with findings from previous studies. Extraction recovery rates for each amino acid were within ±15 %, and no carryover was detected immediately after serum sample analysis. Furthermore, this method enables accurate analysis of D/<span>L</span>-serine and D/<span>L</span>-proline in serum with RSD values below 10 % for intra-day and inter-day reproducibility. This method is promising for enabling early and minimally invasive diagnosis of patients with AD.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"7 ","pages":"Article 100099"},"PeriodicalIF":0.0,"publicationDate":"2025-12-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145685287","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}
To investigate the physiological role of Arabidopsis thalianaD-amino acid aminotransferase (AtDAAT), which catalyzes the transformation of D-aspartate (D-Asp) to D-glutamate (D-Glu) and D-alanine (D-Ala), we analyzed the amounts of various D-amino acids in AtDAAT-deficient and wild-type A. thaliana grown in a medium containing D-Asp. The amounts of Asp, Glu, Ala, valine (Val), and leucine (Leu) enantiomers in AtDAAT-deficient and wild-type A. thaliana were determined using a highly selective two-dimensional high-performance liquid chromatography (2D-HPLC) system. The 2D-HPLC system comprised reversed-phase and chiral separation columns, and amino acids were derivatized with 4-fluoro-7-nitro-2,1,3-benzoxadiazole for detection. To analyze the various d- and l-amino acids in A. thaliana, the separation conditions reported in our previous study were applied with modifications, and the method was validated. Enantioseparation, linearity, and accuracy were satisfactory for all the amino acid enantiomers studied. The amount of D-Asp significantly increased in AtDAAT-deficient A. thaliana, whereas the amounts of the D-Glu, D-Ala, and D-Val decreased significantly, indicating the physiological role of AtDAAT in metabolizing exogenous D-Asp. The amounts of all L-enantiomers were higher in AtDAAT-deficient A. thaliana than in the wild type, indicating the involvement of other amino acid-metabolizing enzymes. Further investigations focusing on the physiological roles of these enzymes in A. thaliana are to be conducted in our laboratory.
{"title":"Investigation of the metabolic role of d-amino acid aminotransferase in Arabidopsis thaliana using a column-switching two-dimensional high-performance liquid chromatography system","authors":"Masae Sekine, Masumi Katane, Tetsuya Miyamoto, Yasuaki Saitoh, Hiroshi Homma, Kumiko Sakai-Kato","doi":"10.1016/j.jpbao.2025.100098","DOIUrl":"10.1016/j.jpbao.2025.100098","url":null,"abstract":"<div><div>To investigate the physiological role of <em>Arabidopsis thaliana</em> <span>D-</span>amino acid aminotransferase (AtDAAT), which catalyzes the transformation of <span>D-</span>aspartate (<span><span>D</span></span>-Asp) to <span>D</span>-glutamate (<span><span>D</span>-</span>Glu) and <span><span>D</span></span>-alanine (<span>D-</span>Ala), we analyzed the amounts of various <span>D</span>-amino acids in AtDAAT-deficient and wild-type <em>A. thaliana</em> grown in a medium containing <span><span>D</span></span>-Asp. The amounts of Asp, Glu, Ala, valine (Val), and leucine (Leu) enantiomers in AtDAAT-deficient and wild-type <em>A. thaliana</em> were determined using a highly selective two-dimensional high-performance liquid chromatography (2D-HPLC) system. The 2D-HPLC system comprised reversed-phase and chiral separation columns, and amino acids were derivatized with 4-fluoro-7-nitro-2,1,3-benzoxadiazole for detection. To analyze the various <span>d</span>- and <span>l</span>-amino acids in <em>A. thaliana</em>, the separation conditions reported in our previous study were applied with modifications, and the method was validated. Enantioseparation, linearity, and accuracy were satisfactory for all the amino acid enantiomers studied. The amount of <span><span>D</span></span>-Asp significantly increased in AtDAAT-deficient <em>A. thaliana,</em> whereas the amounts of the <span>D</span>-Glu, <span>D</span>-Ala, and <span>D</span>-Val decreased significantly, indicating the physiological role of AtDAAT in metabolizing exogenous <span><span>D</span></span>-Asp. The amounts of all <span>L-</span>enantiomers were higher in AtDAAT-deficient <em>A. thaliana</em> than in the wild type, indicating the involvement of other amino acid-metabolizing enzymes. Further investigations focusing on the physiological roles of these enzymes in <em>A. thaliana</em> are to be conducted in our laboratory.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"7 ","pages":"Article 100098"},"PeriodicalIF":0.0,"publicationDate":"2025-11-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145685394","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}
Pub Date : 2025-11-25DOI: 10.1016/j.jpbao.2025.100097
Michele Protti , Roberto Mandrioli , Laura Mercolini
Microsampling has emerged as a highly promising approach for the quantitative analysis of antidepressant drugs, offering key benefits in terms of minimal invasiveness, reduced blood volume requirements and suitability for decentralised and patient-centric sample collection. Historically, the clinical adoption of therapeutic drug monitoring (TDM) for antidepressants has lagged behind that for other CNS drugs, largely due to perceptions of a wide therapeutic window and moderate toxicity risk. However, growing recognition of pharmacokinetic variability, challenges in polypharmacy and evolving models of personalised medicine, now highlight the critical need for robust and adaptable analytical strategies in this field. Technologies such as dried blood spot (DBS) sampling, volumetric absorptive microsampling (VAMS), capillary- and microfluidic-generated DBS, capillary microsampling (CMS) and novel hybrid/automated platforms have been developed and validated for antidepressant quantification across diverse settings (including clinical, preclinical and forensic applications). This review provides a comprehensive analysis of the principles, methodologies and translational relevance of microsampling for antidepressants, critically summarising evidence from original research papers and key review papers. We explore technical and analytical challenges including matrix effects, haematocrit variability, sample stability and the processes underpinning quantitative bridging to conventional matrices such as plasma and serum. Major recent advances, like operator-independent volumetric devices and workflow automation, are contextualised within the broader push toward remote and home-based monitoring. Clinical validation studies, animal model research and post-mortem investigations are reviewed to illustrate the wide range and adaptability of these technologies. By highlighting both achievements and unresolved barriers, this work demonstrates how microsampling is poised to transform antidepressant TDM, research and future psychiatric pharmacotherapy.
{"title":"Microsampling for antidepressant drug analysis: Current state and perspectives","authors":"Michele Protti , Roberto Mandrioli , Laura Mercolini","doi":"10.1016/j.jpbao.2025.100097","DOIUrl":"10.1016/j.jpbao.2025.100097","url":null,"abstract":"<div><div>Microsampling has emerged as a highly promising approach for the quantitative analysis of antidepressant drugs, offering key benefits in terms of minimal invasiveness, reduced blood volume requirements and suitability for decentralised and patient-centric sample collection. Historically, the clinical adoption of therapeutic drug monitoring (TDM) for antidepressants has lagged behind that for other CNS drugs, largely due to perceptions of a wide therapeutic window and moderate toxicity risk. However, growing recognition of pharmacokinetic variability, challenges in polypharmacy and evolving models of personalised medicine, now highlight the critical need for robust and adaptable analytical strategies in this field. Technologies such as dried blood spot (DBS) sampling, volumetric absorptive microsampling (VAMS), capillary- and microfluidic-generated DBS, capillary microsampling (CMS) and novel hybrid/automated platforms have been developed and validated for antidepressant quantification across diverse settings (including clinical, preclinical and forensic applications). This review provides a comprehensive analysis of the principles, methodologies and translational relevance of microsampling for antidepressants, critically summarising evidence from original research papers and key review papers. We explore technical and analytical challenges including matrix effects, haematocrit variability, sample stability and the processes underpinning quantitative bridging to conventional matrices such as plasma and serum. Major recent advances, like operator-independent volumetric devices and workflow automation, are contextualised within the broader push toward remote and home-based monitoring. Clinical validation studies, animal model research and post-mortem investigations are reviewed to illustrate the wide range and adaptability of these technologies. By highlighting both achievements and unresolved barriers, this work demonstrates how microsampling is poised to transform antidepressant TDM, research and future psychiatric pharmacotherapy.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"7 ","pages":"Article 100097"},"PeriodicalIF":0.0,"publicationDate":"2025-11-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145625408","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}
Pub Date : 2025-11-17DOI: 10.1016/j.jpbao.2025.100096
Maikon Thiago do Nascimento , Mayara S. Araujo , Leticia Abe de Sena , Roberta A. Medeiros , Mariana Gava Segatelli , Cesar Ricardo Teixeira Tarley
This work reports an analytical strategy for the quantification of pyridoxine (PYR) and caffeine (CAF) in pre-workout formulations, specifically multi-ingredient performance supplements (MIPS) and encapsulated guarana powder (GP). The approach relies on batch injection analysis with amperometric detection (BIA-AD) employing a boron-doped diamond electrode (BDDE) as the working electrode. A straightforward correction factor (CF) was applied to enable caffeine determination at + 1.5 V in the presence of pyridoxine. The method provided low limits of quantification, 9.64 µmol L−1 for pyridoxine and 6.82 µmol L−1 for caffeine. Accuracy was assessed through spiking and recovery assays, yielding values between 90 % and 110 %, and the results showed good agreement with those obtained by the reference High-Performance Liquid Chromatography with Diode-Array Detection technique. Application of the method to real samples demonstrated that both analytes were successfully measured in multi-ingredient performance supplements. For guarana powder samples, the caffeine concentrations were consistent with the labeled values. Overall, the method offers a rapid, low-cost, portable, and environmentally sustainable alternative for the determination of pyridoxine and caffeine in pre-workout supplements.
{"title":"A simple approach for amperometric determination of pyridoxine and caffeine in pre-workout supplements using batch injection analysis with boron-doped diamond electrode","authors":"Maikon Thiago do Nascimento , Mayara S. Araujo , Leticia Abe de Sena , Roberta A. Medeiros , Mariana Gava Segatelli , Cesar Ricardo Teixeira Tarley","doi":"10.1016/j.jpbao.2025.100096","DOIUrl":"10.1016/j.jpbao.2025.100096","url":null,"abstract":"<div><div>This work reports an analytical strategy for the quantification of pyridoxine (PYR) and caffeine (CAF) in pre-workout formulations, specifically multi-ingredient performance supplements (MIPS) and encapsulated guarana powder (GP). The approach relies on batch injection analysis with amperometric detection (BIA-AD) employing a boron-doped diamond electrode (BDDE) as the working electrode. A straightforward correction factor (CF) was applied to enable caffeine determination at + 1.5 V in the presence of pyridoxine. The method provided low limits of quantification, 9.64 µmol L<sup>−1</sup> for pyridoxine and 6.82 µmol L<sup>−1</sup> for caffeine. Accuracy was assessed through spiking and recovery assays, yielding values between 90 % and 110 %, and the results showed good agreement with those obtained by the reference High-Performance Liquid Chromatography with Diode-Array Detection technique. Application of the method to real samples demonstrated that both analytes were successfully measured in multi-ingredient performance supplements. For guarana powder samples, the caffeine concentrations were consistent with the labeled values. Overall, the method offers a rapid, low-cost, portable, and environmentally sustainable alternative for the determination of pyridoxine and caffeine in pre-workout supplements.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"6 ","pages":"Article 100096"},"PeriodicalIF":0.0,"publicationDate":"2025-11-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145578904","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}
Pub Date : 2025-11-04DOI: 10.1016/j.jpbao.2025.100094
Michele Protti , Roberta Di Lecce , Jiri Adamec , Luca G. Regazzoni , Valeria Valsecchi , Claudia Volpi , Roberto Mandrioli , Laura Mercolini
In this study, for the first time rat plasma microsampling was carried out by means of in situ-generated volumetric dried plasma spot (vDPS) technology and applied to the determination of the neuroprotective agent edaravone and its sulphate and glucuronide metabolites. Sampling was performed using Telimmune® plasma separation cards (vPSC), which allow the formation of volumetrically accurate dried plasma spots (3 µL) from blood drops deposited on them. After accelerated forced drying and solvent extraction in methanol, drying and redissolution, analytes were baseline separated and quantified through an original HPLC-MS/MS analytical method. Validation assays provided excellent results, with detection limits between 0.7 and 1.7 ng/mL, and quantitation limits between 2.0 and 5.0 ng/mL. Extraction yields were higher than 81 % and precision was lower than 14.1 % (relative standard deviation, RSD). The volumetric microsampling approach offers a much less invasive and stressful sampling. The vPSC technology offers a simple, cost-effective alternative method to produce a volumetric plasma sample that is stable when dried and eliminates requirements for both cold-chain and biohazard transport. The developed analytical workflow appears suitable for advantageous application to pharmacokinetic and toxicokinetic animal studies of edaravone and its metabolites.
{"title":"In situ-generated volumetric dried plasma spots for the analysis of edaravone and metabolites in animal models","authors":"Michele Protti , Roberta Di Lecce , Jiri Adamec , Luca G. Regazzoni , Valeria Valsecchi , Claudia Volpi , Roberto Mandrioli , Laura Mercolini","doi":"10.1016/j.jpbao.2025.100094","DOIUrl":"10.1016/j.jpbao.2025.100094","url":null,"abstract":"<div><div>In this study, for the first time rat plasma microsampling was carried out by means of in situ-generated volumetric dried plasma spot (vDPS) technology and applied to the determination of the neuroprotective agent edaravone and its sulphate and glucuronide metabolites. Sampling was performed using Telimmune® plasma separation cards (vPSC), which allow the formation of volumetrically accurate dried plasma spots (3 µL) from blood drops deposited on them. After accelerated forced drying and solvent extraction in methanol, drying and redissolution, analytes were baseline separated and quantified through an original HPLC-MS/MS analytical method. Validation assays provided excellent results, with detection limits between 0.7 and 1.7 ng/mL, and quantitation limits between 2.0 and 5.0 ng/mL. Extraction yields were higher than 81 % and precision was lower than 14.1 % (relative standard deviation, RSD). The volumetric microsampling approach offers a much less invasive and stressful sampling. The vPSC technology offers a simple, cost-effective alternative method to produce a volumetric plasma sample that is stable when dried and eliminates requirements for both cold-chain and biohazard transport. The developed analytical workflow appears suitable for advantageous application to pharmacokinetic and toxicokinetic animal studies of edaravone and its metabolites.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"6 ","pages":"Article 100094"},"PeriodicalIF":0.0,"publicationDate":"2025-11-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145528225","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}
Pub Date : 2025-11-04DOI: 10.1016/j.jpbao.2025.100095
Prajna Gupta , Saurav Sarkar , Sandip Karmakar , Sougata Jana , Gouranga Nandi , Sreejan Manna
The recent advancements in medical science and technology have enabled the diversified applications of existing drug delivery systems. Scaffolds are regarded as a relatively novel drug delivery system mostly employed in therapeutic and biomedical applications. In recent times, scaffolds are widely being investigated for sensory applications in in-vivo conditions. The mostly employed scaffold types for sensory applications are nanofibers, hydrogels, 3-D printed scaffolds and microparticulate scaffolds. Owing to its favorable physicochemical properties, scaffolds can also simultaneously function as a sensor in biological environment and also as delivery vectors. The surface charge, optical properties, porous nature, higher mechanical strength, and biodegradable behavior of polymeric scaffolds have encouraged pharmaceutical researchers to investigate upon it as biosensor. The ease of fabrication techniques, compatibility for customization and functionalization have made scaffolds a versatile system that is yet to be fully explored. The connection for integration of biosensor within scaffold has been described in this article. This review outlines the suitability of biomaterials-based scaffolds in sensory applications alongside the commonly employed fabrication techniques and biosensing applications.
{"title":"Biosensory implications of scaffolds: Designing, integration and biomedical applications","authors":"Prajna Gupta , Saurav Sarkar , Sandip Karmakar , Sougata Jana , Gouranga Nandi , Sreejan Manna","doi":"10.1016/j.jpbao.2025.100095","DOIUrl":"10.1016/j.jpbao.2025.100095","url":null,"abstract":"<div><div>The recent advancements in medical science and technology have enabled the diversified applications of existing drug delivery systems. Scaffolds are regarded as a relatively novel drug delivery system mostly employed in therapeutic and biomedical applications. In recent times, scaffolds are widely being investigated for sensory applications in in-vivo conditions. The mostly employed scaffold types for sensory applications are nanofibers, hydrogels, 3-D printed scaffolds and microparticulate scaffolds. Owing to its favorable physicochemical properties, scaffolds can also simultaneously function as a sensor in biological environment and also as delivery vectors. The surface charge, optical properties, porous nature, higher mechanical strength, and biodegradable behavior of polymeric scaffolds have encouraged pharmaceutical researchers to investigate upon it as biosensor. The ease of fabrication techniques, compatibility for customization and functionalization have made scaffolds a versatile system that is yet to be fully explored. The connection for integration of biosensor within scaffold has been described in this article. This review outlines the suitability of biomaterials-based scaffolds in sensory applications alongside the commonly employed fabrication techniques and biosensing applications.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"6 ","pages":"Article 100095"},"PeriodicalIF":0.0,"publicationDate":"2025-11-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145473490","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}
Dietary supplements (DSs) or food supplements (FSs) are products widely consumed to support the diet. They could contain amino acids, peptides, proteins, vitamins, minerals, herbs, and compounds of botanical origin. Since they are considered food, they are not subjected to approval by government agencies. Therefore, they are popular because they can be bought without a prescription and are easily available on the internet. The addition of drugs to DSs/FSs is not allowed because it could cause serious damage to health. Therefore, there is a need for analytical methods capable of performing qualitative/quantitative analysis of the declared content and to verify the presence of adulterants. Among the analytical techniques employed, miniaturized techniques have been successfully applied to the analysis of such products. In this review, applications performed with capillary electrophoresis and nano-/capillary-liquid chromatography, and microchip electrophoresis published in the period 2018–2025 (July), are reported and discussed.
{"title":"Nano-liquid chromatography and electromigration techniques applied to the analysis of dietary supplements. A review","authors":"Chiara Fanali , Erica Cutè , Alessandra Gentili , Michele Pier Luca Guarino , Salvatore Fanali","doi":"10.1016/j.jpbao.2025.100093","DOIUrl":"10.1016/j.jpbao.2025.100093","url":null,"abstract":"<div><div>Dietary supplements (DSs) or food supplements (FSs) are products widely consumed to support the diet. They could contain amino acids, peptides, proteins, vitamins, minerals, herbs, and compounds of botanical origin. Since they are considered food, they are not subjected to approval by government agencies. Therefore, they are popular because they can be bought without a prescription and are easily available on the internet. The addition of drugs to DSs/FSs is not allowed because it could cause serious damage to health. Therefore, there is a need for analytical methods capable of performing qualitative/quantitative analysis of the declared content and to verify the presence of adulterants. Among the analytical techniques employed, miniaturized techniques have been successfully applied to the analysis of such products. In this review, applications performed with capillary electrophoresis and nano-/capillary-liquid chromatography, and microchip electrophoresis published in the period 2018–2025 (July), are reported and discussed.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"6 ","pages":"Article 100093"},"PeriodicalIF":0.0,"publicationDate":"2025-10-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145473491","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}
Pub Date : 2025-10-04DOI: 10.1016/j.jpbao.2025.100092
İnci Uludağ Anıl, Mustafa Kemal Sezgintürk
The emergence of anti-drug antibodies (ADAs) poses a significant challenge in biological therapeutics, undermining drug efficacy and patient safety. This review thoroughly assesses existing and novel analytical methods for ADA detection, highlighting their principles, strengths, and limitations. Conventional techniques like ELISA and ECL provide great sensitivity but may be inadequate for detecting low-affinity ADAs. On the other hand, surface plasmon resonance (SPR) offers advantages in detecting low-affinity anti-drug antibodies (ADAs) due to its real-time kinetic assessment. Recent advancements in label-free technologies, such as thin-film interferometry, electrolyte-gated organic field-effect transistors, and quartz crystal microbalance, show significant potential for rapid, sensitive, and real-time ADA monitoring. These advanced platforms enable accurate kinetic characterization and offer promise for point-of-care applications. Additionally, novel approaches address limitations of conventional immunoassays by simplifying workflows and reducing assay time. This review underscores the importance of ADA assessment for optimizing personalized therapeutic strategies and improving patient outcomes.
{"title":"Advances in anti-drug antibody detection: Miniaturized biosensor technologies and beyond","authors":"İnci Uludağ Anıl, Mustafa Kemal Sezgintürk","doi":"10.1016/j.jpbao.2025.100092","DOIUrl":"10.1016/j.jpbao.2025.100092","url":null,"abstract":"<div><div>The emergence of anti-drug antibodies (ADAs) poses a significant challenge in biological therapeutics, undermining drug efficacy and patient safety. This review thoroughly assesses existing and novel analytical methods for ADA detection, highlighting their principles, strengths, and limitations. Conventional techniques like ELISA and ECL provide great sensitivity but may be inadequate for detecting low-affinity ADAs. On the other hand, surface plasmon resonance (SPR) offers advantages in detecting low-affinity anti-drug antibodies (ADAs) due to its real-time kinetic assessment. Recent advancements in label-free technologies, such as thin-film interferometry, electrolyte-gated organic field-effect transistors, and quartz crystal microbalance, show significant potential for rapid, sensitive, and real-time ADA monitoring. These advanced platforms enable accurate kinetic characterization and offer promise for point-of-care applications. Additionally, novel approaches address limitations of conventional immunoassays by simplifying workflows and reducing assay time. This review underscores the importance of ADA assessment for optimizing personalized therapeutic strategies and improving patient outcomes.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"6 ","pages":"Article 100092"},"PeriodicalIF":0.0,"publicationDate":"2025-10-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145265852","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}
Pub Date : 2025-09-20DOI: 10.1016/j.jpbao.2025.100091
Abdullah Al Faysal, Beril S. Kaya, Hatice Elmacioglu, Ayşegül Gölcü
Turkey has historically been a prominent player in the trade of medicinal and aromatic plants, a status attributed to its advantageous geographical position, favorable climate, rich plant diversity, agricultural capabilities, and extensive land area. The country's flora is home to numerous species that are integral to established practices in herbal medicine, as well as the global manufacturing of plant-based chemicals, food additives, cosmetics, and perfumery. Recent research has particularly emphasized the role of antioxidant substances and phenolic compounds found in plants in promoting health. This review thoroughly evaluates the analytical techniques utilized in assessing antioxidant activity, drawing attention to the essential chemical reactions that underpin these measurements. Furthermore, the article compellingly highlights the significant role of antioxidants across various industries, demonstrating their crucial contributions to health, food preservation, and beyond. Furthermore, an in-depth analysis of the antioxidant properties of Turkish plant extracts is presented, detailing their constituent components, the solvents utilized for extraction, and the methodologies applied in antioxidant research.
{"title":"A comprehensive evaluation of contemporary techniques employed to measure the antioxidant activity of plant extracts from Turkey, both in vitro and in vivo","authors":"Abdullah Al Faysal, Beril S. Kaya, Hatice Elmacioglu, Ayşegül Gölcü","doi":"10.1016/j.jpbao.2025.100091","DOIUrl":"10.1016/j.jpbao.2025.100091","url":null,"abstract":"<div><div>Turkey has historically been a prominent player in the trade of medicinal and aromatic plants, a status attributed to its advantageous geographical position, favorable climate, rich plant diversity, agricultural capabilities, and extensive land area. The country's flora is home to numerous species that are integral to established practices in herbal medicine, as well as the global manufacturing of plant-based chemicals, food additives, cosmetics, and perfumery. Recent research has particularly emphasized the role of antioxidant substances and phenolic compounds found in plants in promoting health. This review thoroughly evaluates the analytical techniques utilized in assessing antioxidant activity, drawing attention to the essential chemical reactions that underpin these measurements. Furthermore, the article compellingly highlights the significant role of antioxidants across various industries, demonstrating their crucial contributions to health, food preservation, and beyond. Furthermore, an in-depth analysis of the antioxidant properties of Turkish plant extracts is presented, detailing their constituent components, the solvents utilized for extraction, and the methodologies applied in antioxidant research.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"6 ","pages":"Article 100091"},"PeriodicalIF":0.0,"publicationDate":"2025-09-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145157521","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}
Pub Date : 2025-09-16DOI: 10.1016/j.jpbao.2025.100089
Erika Maria Ricci , Miryam Perrucci , Marcello Locatelli , Imran Ali , Halil I. Ulusoy , Abuzar Kabir , Fotouh R. Mansour
Growing concerns over environmental pollution have led to increased emphasis on Green Chemistry and, more specifically, Green Analytical Chemistry (GAC). These frameworks advocate for the reduction of hazardous substances, minimization of waste, and consideration of the entire life cycle of analytical procedures—from production to disposal. Within this context, miniaturized analytical techniques have emerged as sustainable and efficient alternatives to conventional methods. Among these, capillary liquid chromatography (cLC), nano-liquid chromatography (nano-LC), and various modes of capillary electrophoresis (CE)—including micellar electrokinetic chromatography (MEKC), capillary isotachophoresis (CITP), capillary zone electrophoresis (CZE), capillary isoelectric focusing (CIEF), and capillary gel electrophoresis (CGE) have gained significant traction. Their advantages in terms of reduced solvent and sample consumption, enhanced resolution, and faster analysis times have made them particularly valuable in pharmaceutical and biomedical applications. One critical application area is the chiral separation of active pharmaceutical ingredients (APIs), which is increasingly vital in biotechnology, chemistry, agriculture, and especially the pharmaceutical industry. Electrokinetic chromatography (EKC) has proven to be an effective and versatile technique for this purpose, offering high resolution, flexibility, speed, and cost-efficiency. The growing availability of novel chiral selectors further enhances its appeal for the separation of enantiomeric drug compounds. This review provides an overview of recent advancements in miniaturized analytical techniques and highlights their applications in the biomedical and pharmaceutical sectors, with a particular focus on chiral separations using EKC.
{"title":"Miniaturization in action: High-resolution, low-cost analytical platforms for biomedical and pharmaceutical research","authors":"Erika Maria Ricci , Miryam Perrucci , Marcello Locatelli , Imran Ali , Halil I. Ulusoy , Abuzar Kabir , Fotouh R. Mansour","doi":"10.1016/j.jpbao.2025.100089","DOIUrl":"10.1016/j.jpbao.2025.100089","url":null,"abstract":"<div><div>Growing concerns over environmental pollution have led to increased emphasis on Green Chemistry and, more specifically, Green Analytical Chemistry (GAC). These frameworks advocate for the reduction of hazardous substances, minimization of waste, and consideration of the entire life cycle of analytical procedures—from production to disposal. Within this context, miniaturized analytical techniques have emerged as sustainable and efficient alternatives to conventional methods. Among these, capillary liquid chromatography (cLC), nano-liquid chromatography (nano-LC), and various modes of capillary electrophoresis (CE)—including micellar electrokinetic chromatography (MEKC), capillary isotachophoresis (CITP), capillary zone electrophoresis (CZE), capillary isoelectric focusing (CIEF), and capillary gel electrophoresis (CGE) have gained significant traction. Their advantages in terms of reduced solvent and sample consumption, enhanced resolution, and faster analysis times have made them particularly valuable in pharmaceutical and biomedical applications. One critical application area is the chiral separation of active pharmaceutical ingredients (APIs), which is increasingly vital in biotechnology, chemistry, agriculture, and especially the pharmaceutical industry. Electrokinetic chromatography (EKC) has proven to be an effective and versatile technique for this purpose, offering high resolution, flexibility, speed, and cost-efficiency. The growing availability of novel chiral selectors further enhances its appeal for the separation of enantiomeric drug compounds. This review provides an overview of recent advancements in miniaturized analytical techniques and highlights their applications in the biomedical and pharmaceutical sectors, with a particular focus on chiral separations using EKC.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"6 ","pages":"Article 100089"},"PeriodicalIF":0.0,"publicationDate":"2025-09-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145104307","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}
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