Journal of Pharmaceutical and Biomedical Analysis Open最新文献_第2页

Journal of Pharmaceutical and Biomedical Analysis Open

Pub Date : 2026-01-01

引用次数: 0

Journal of Pharmaceutical and Biomedical Analysis Open

Pub Date : 2026-01-01

引用次数: 0

Development and application of an LC-MS/MS method for the determination of 15 antipsychotic and 15 psychotic drugs and metabolites in plasma LC-MS/MS法测定血浆中15种抗精神病药物和15种精神药物及其代谢物的建立与应用

Journal of Pharmaceutical and Biomedical Analysis Open

Pub Date : 2025-12-21 DOI: 10.1016/j.jpbao.2025.100101

Hao-Zhu Wang , Masamitsu Maekawa , Toshihiro Sato , Yu Sato , Masaki Kumondai , Kumiko Fujii , Yuji Ozeki , Nariyasu Mano

Antipsychotic drugs play a critical role in the treatment of schizophrenia and related psychiatric disorders. However, their therapeutic effects and adverse reactions vary significantly due to individual metabolic differences and drug-drug interactions (DDIs) as well as genetic polymorphisms in drug-metabolizing enzymes. Although, therapeutic drug monitoring (TDM) is essential for optimizing treatment outcomes, TDM for most antipsychotics remains underutilized in Japan. This study builds upon our previous research, which developed a liquid chromatography–tandem mass spectrometry (LC-MS/MS) method for the simultaneous analysis of 15 antipsychotics, 15 psychiatric drugs and 4 active metabolites. The method was optimized for sensitivity, reproducibility, and accuracy by selected reaction monitoring transitions and optimizing gradient elution parameters. Validation followed FDA bioanalytical guideline, demonstrating excellent linearity (R² > 0.98), intra- and inter-day precision (<15 % RSD for 87 % compounds), and acceptable matrix effects. Stability tests revealed variable degradation patterns among certain analytes, necessitating further refinements. Application of this method to plasma samples from patients with schizophrenia revealed significant inter-individual variability in drug concentrations. Some patients exhibited plasma levels outside the therapeutic range, highlighting the clinical necessity of TDM. By integrating a broader range of psychotropic drugs, this study extends our previous findings and enhances clinical decision-making in psychiatric pharmacotherapy. The developed LC-MS/MS method enables rapid, same-mode quantification suitable for real-time clinical use and provides a valuable tool for assessing the impact of DDIs and optimizing therapeutic strategies in schizophrenia.

抗精神病药物在治疗精神分裂症及相关精神疾病中起着至关重要的作用。然而，由于个体代谢差异和药物-药物相互作用（ddi）以及药物代谢酶的遗传多态性，它们的治疗效果和不良反应差异很大。尽管治疗性药物监测（TDM）对于优化治疗结果至关重要，但在日本，大多数抗精神病药物的TDM仍未得到充分利用。本研究建立在我们之前的研究基础上，建立了液相色谱-串联质谱（LC-MS/MS）同时分析15种抗精神病药物、15种精神药物和4种活性代谢物的方法。通过选择反应监测过渡段和优化梯度洗脱参数，对方法的灵敏度、重现性和准确性进行了优化。验证遵循FDA生物分析指南，显示出良好的线性（R²> 0.98），日内和日内精密度（87 %化合物的RSD <；15 %）和可接受的基质效应。稳定性测试揭示了某些分析物的可变降解模式，需要进一步改进。将该方法应用于精神分裂症患者的血浆样本，揭示了药物浓度在个体间的显著差异。一些患者的血浆水平超出治疗范围，突出了TDM的临床必要性。通过整合更广泛的精神药物，本研究扩展了我们之前的发现，并提高了精神药物治疗的临床决策。所开发的LC-MS/MS方法能够实现快速，相同模式的定量，适合实时临床使用，并为评估ddi的影响和优化精神分裂症的治疗策略提供了有价值的工具。

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引用次数: 0

Quantitative analysis of D/L-serine and D/L-proline in serum by isotope-coded derivatization using an original chiral resolution labeling reagent 采用原始手性拆分标记试剂，同位素编码衍生法定量分析血清中D/ l -丝氨酸和D/ l -脯氨酸

Journal of Pharmaceutical and Biomedical Analysis Open

Pub Date : 2025-12-02 DOI: 10.1016/j.jpbao.2025.100099

Makoto Ozaki , Yasunari Yamada , Tsunehisa Hirose , Motoshi Shimotsuma , Akari Ikeda , Takahiro Kawase , Ai Tsuji , Shozo Tomonaga , Miyuki Matsui , Takefumi Kuranaga , Hideaki Kakeya

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。

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引用次数: 0

Investigation of the metabolic role of d-amino acid aminotransferase in Arabidopsis thaliana using a column-switching two-dimensional high-performance liquid chromatography system 利用柱切换二维高效液相色谱系统研究d-氨基酸转氨酶在拟南芥中的代谢作用

Journal of Pharmaceutical and Biomedical Analysis Open

Pub Date : 2025-11-29 DOI: 10.1016/j.jpbao.2025.100098

Masae Sekine, Masumi Katane, Tetsuya Miyamoto, Yasuaki Saitoh, Hiroshi Homma, Kumiko Sakai-Kato

To investigate the physiological role of Arabidopsis thaliana D-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.

为了研究拟南芥d-氨基酸转氨酶（AtDAAT）催化d-天冬氨酸（D-Asp）转化为d-谷氨酸（D-Glu）和d-丙氨酸（D-Ala）的生理作用，我们分析了AtDAAT缺失和野生型拟南芥在含有D-Asp的培养基中生长的各种d-氨基酸的数量。采用高选择性二维高效液相色谱（2D-HPLC）系统测定了atdaat缺陷型和野生型拟蓝中Asp、Glu、Ala、valine （Val）和leucine （Leu）对映体的含量。2D-HPLC系统由反相和手性分离柱组成，用4-氟-7-硝基-2,1,3-苯并恶二唑衍生检测氨基酸。为了分析拟南芥中多种d-氨基酸和l-氨基酸，我们对先前研究中报道的分离条件进行了修改，并对方法进行了验证。对所有氨基酸对映体的分离、线性和准确性均令人满意。缺乏AtDAAT的拟蓝藻D-Asp含量显著增加，而D-Glu、D-Ala和D-Val含量显著降低，说明AtDAAT在代谢外源D-Asp中的生理作用。所有l -对映体的数量在atdaat缺失的拟蓝藻中高于野生型，表明其他氨基酸代谢酶的参与。进一步研究这些酶在拟南芥中的生理作用将在我们的实验室进行。

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引用次数: 0

Microsampling for antidepressant drug analysis: Current state and perspectives 抗抑郁药物微采样分析：现状和前景

Journal of Pharmaceutical and Biomedical Analysis Open

Pub Date : 2025-11-25 DOI: 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.

微采样已经成为一种非常有前途的抗抑郁药物定量分析方法，在最小的侵入性、减少的血容量要求和适合分散和以患者为中心的样本收集方面提供了关键的好处。从历史上看，抗抑郁药的治疗性药物监测（TDM）的临床应用落后于其他中枢神经系统药物，这主要是由于人们认为治疗窗口较宽，毒性风险中等。然而，越来越多的人认识到药代动力学变异性，多药的挑战和个性化医疗模式的发展，现在突出了对该领域强大和适应性强的分析策略的迫切需要。干血斑（DBS）采样、体积吸收微采样（VAMS）、毛细管和微流体生成的DBS、毛细管微采样（CMS）和新型混合/自动化平台等技术已被开发并验证，可用于不同环境（包括临床、临床前和法医应用）的抗抑郁药定量。本综述全面分析了抗抑郁药物微采样的原理、方法和转化相关性，批判性地总结了原始研究论文和关键综述论文的证据。我们探讨了技术和分析方面的挑战，包括基质效应、红细胞压积变异性、样品稳定性和支撑定量桥接到传统基质（如血浆和血清）的过程。最近的主要进展，如独立于操作人员的体积测量设备和工作流程自动化，都是在更广泛地推动远程和家庭监控的背景下进行的。本文回顾了临床验证研究、动物模型研究和死后调查，以说明这些技术的广泛应用和适应性。通过强调成就和未解决的障碍，这项工作展示了微采样如何准备改变抗抑郁药TDM，研究和未来的精神药物治疗。

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引用次数: 0

A simple approach for amperometric determination of pyridoxine and caffeine in pre-workout supplements using batch injection analysis with boron-doped diamond electrode 用掺硼金刚石电极进行批量注射分析，建立了一种简便的运动前补品中吡哆醇和咖啡因的安培测定方法

Journal of Pharmaceutical and Biomedical Analysis Open

Pub Date : 2025-11-17 DOI: 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.

本研究报告了一种定量测定运动前配方中吡哆醇（PYR）和咖啡因（CAF）的分析策略，特别是多成分性能补充剂（MIPS）和胶囊瓜拉那粉（GP）。该方法采用掺硼金刚石电极（BDDE）作为工作电极，采用安培检测（BIA-AD）批量注入分析。采用直接校正因子（CF），在+ 1.5 V条件下，在吡哆醇存在下测定咖啡因。该方法的定量下限为吡哆醇9.64µmol L−1，咖啡因6.82µmol L−1。测定结果在90 % ~ 110 %之间，与高效液相色谱二极管阵列检测技术的测定结果吻合较好。该方法在实际样品中的应用表明，这两种分析物都能成功地测量多成分性能补充剂。对于瓜拉那粉末样品，咖啡因浓度与标签值一致。总的来说，该方法提供了一种快速、低成本、便携和环保的替代方法，用于测定运动前补充剂中的吡哆醇和咖啡因。

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引用次数: 0

In situ-generated volumetric dried plasma spots for the analysis of edaravone and metabolites in animal models 在现场产生的体积干燥血浆斑点分析依达拉奉和代谢物的动物模型

Journal of Pharmaceutical and Biomedical Analysis Open

Pub Date : 2025-11-04 DOI: 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.

本研究首次采用原位生成体积干燥血浆斑点（vDPS）技术进行大鼠血浆微采样，并将其应用于神经保护剂依达拉奉及其硫酸盐和葡萄糖醛酸盐代谢物的测定。使用Telimmune®血浆分离卡（vPSC）进行采样，该卡允许从沉积在其上的血滴形成体积精确的干燥血浆斑点（3 µL）。经过加速强制干燥和甲醇溶剂萃取，干燥和再溶解，分析物通过原始的HPLC-MS/MS分析方法进行基线分离和定量。验证分析结果优异，检测限在0.7 ~ 1.7 ng/mL之间，定量限在2.0 ~ 5.0 ng/mL之间。提取率大于81 %，精密度小于14.1 %（相对标准偏差，RSD）。体积微采样方法提供了一个更小的侵入性和压力采样。vPSC技术提供了一种简单、经济的替代方法来生产体积等离子体样品，该样品在干燥时是稳定的，并且消除了冷链和生物危害运输的要求。所开发的分析工作流程适合于依达拉奉及其代谢物的药代动力学和毒代动力学动物研究。

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引用次数: 0

Biosensory implications of scaffolds: Designing, integration and biomedical applications 支架的生物感觉意义：设计、集成和生物医学应用

Journal of Pharmaceutical and Biomedical Analysis Open

Pub Date : 2025-11-04 DOI: 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.

近年来医学科学和技术的进步使现有的给药系统的应用多样化。支架被认为是一种相对较新的药物传递系统，主要用于治疗和生物医学应用。近年来，支架在体内条件下的感官应用被广泛研究。感官应用中最常用的支架类型是纳米纤维、水凝胶、3d打印支架和微颗粒支架。由于其良好的物理化学性质，支架还可以同时作为生物环境的传感器和递送载体。聚合物支架的表面电荷、光学性质、多孔性、较高的机械强度和可生物降解性促使制药研究人员将其作为生物传感器进行研究。制造技术的简易性、定制化和功能化的兼容性使支架成为一种尚未充分探索的多功能系统。本文介绍了生物传感器在支架内集成的连接。本文综述了基于生物材料的支架在感官应用中的适用性，以及常用的制造技术和生物传感应用。

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引用次数: 0

Nano-liquid chromatography and electromigration techniques applied to the analysis of dietary supplements. A review 纳米液相色谱和电迁移技术在膳食补充剂分析中的应用。回顾

Journal of Pharmaceutical and Biomedical Analysis Open

Pub Date : 2025-10-25 DOI: 10.1016/j.jpbao.2025.100093

Chiara Fanali , Erica Cutè , Alessandra Gentili , Michele Pier Luca Guarino , Salvatore Fanali

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.

膳食补充剂（DSs）或食品补充剂（FSs）是广泛消费的产品，以支持饮食。它们可能含有氨基酸、多肽、蛋白质、维生素、矿物质、草药和植物性化合物。因为它们被认为是食物，所以不需要政府机构的批准。因此，它们很受欢迎，因为它们不需要处方就可以买到，而且很容易在网上买到。不允许在DSs/FSs中添加药物，因为这可能对健康造成严重损害。因此，需要能够对申报内容进行定性/定量分析并验证掺假物存在的分析方法。在所采用的分析技术中，小型化技术已成功地应用于此类产品的分析。本文综述了2018-2025年（7月）期间发表的毛细管电泳、纳米/毛细管-液相色谱和微芯片电泳的应用。

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引用次数: 0