Journal of Pharmaceutical and Biomedical Analysis Open最新文献

Process analytical technologies applied to quality control of emerging alternative protein food products: Challenges and future trends 应用于新兴替代蛋白食品质量控制的过程分析技术：挑战和未来趋势

Journal of Pharmaceutical and Biomedical Analysis Open

Pub Date : 2026-02-08 DOI: 10.1016/j.jpbao.2026.100105

Ana Paula Ayub da Costa Barbon , Irene Marivel Nolasco-Perez , Sylvio Jr Barbon , Ademar Domingos Viagem Máquina , Wen-Hao Su , Douglas Fernandes Barbin

The escalating global demand for sustainable and health-conscious dietary options has fostered interest in alternative protein food products, ranging from plant-based to cell-based proteins. This review proposes a critical synthesis for integrating Process Analytical Technologies (PAT) into the quality control of these emerging food matrices, focusing on their inherent complexity. The study explores the fundamental technical hurdles posed by the high compositional heterogeneity and the variable structural characteristics of diverse alternative proteins. We discuss various PAT methodologies such as Near-Infrared (NIR) spectroscopy, Raman spectroscopy, and digital imaging, which offer real-time data critical for monitoring product quality. These techniques are characterized by strong spectral interferences from water, lipids, polysaccharides, and novel functional ingredients, which directly affect the robustness and transferability of the model. Consequently, the effective implementation of PAT increasingly depends on advanced chemometrics and data fusion strategies to harmonize heterogeneous data streams. The application of these technologies enables continuous monitoring and control during production, facilitating adherence to evolving regulations and standards. This review highlights the need for advancements in PAT to ensure the consistent quality and safety of alternative protein products, suggesting a future where these technologies are pivotal in the scalability of alternative protein sources.

全球对可持续和注重健康的饮食选择的需求不断上升，促进了人们对替代蛋白质食品的兴趣，从植物蛋白到细胞蛋白。本文综述了将过程分析技术（PAT）集成到这些新兴食品基质的质量控制中的关键综合，重点是其固有的复杂性。该研究探讨了由不同替代蛋白的高组成异质性和可变结构特征构成的基本技术障碍。我们讨论了各种PAT方法，如近红外（NIR）光谱，拉曼光谱和数字成像，这些方法为监测产品质量提供了关键的实时数据。这些技术的特点是来自水、脂类、多糖和新型功能成分的强烈光谱干扰，这直接影响了模型的稳健性和可转移性。因此，PAT的有效实施越来越依赖于先进的化学计量学和数据融合策略来协调异构数据流。这些技术的应用可以在生产过程中进行持续监测和控制，促进遵守不断变化的法规和标准。这篇综述强调了PAT的发展需要，以确保替代蛋白质产品的一致质量和安全性，并表明这些技术在替代蛋白质来源的可扩展性方面具有关键作用。

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引用次数: 0

Enantio-selective analytical method for ergothioneine using chemical tagging coupled with LC-MS/MS and D/L ratio measurements in mushrooms 化学标记联用LC-MS/MS和D/L测定对映体选择性分析蘑菇中麦角硫因的方法

Journal of Pharmaceutical and Biomedical Analysis Open

Pub Date : 2026-02-02 DOI: 10.1016/j.jpbao.2026.100103

Takahiro Takayama , Miu Nakanishi , Yuki Makita, Rena Ohnishi, Koichi Inoue

Ergothioneine (EGT), a strong natural antioxidant, is a promising healthcare product owing to its anti-aging activity. EGT is found in various mushrooms, and investigations into its quantity and properties, including chirality, are important from a biological perspective. This study aimed to develop an enantioselective analytical method for EGT and histidine (His) using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The method is developed based on paired enantio-chemical tags, (4-chloro-6-methoxy-1,3,5-triazin-2-yl)-d- and l-leucine, to thiol sites or amine groups. The developed method achieved clear enantioseparation of d- and l‑EGT and d- and l-His with high sensitivity (limits of quantification reached 70–200 fmol). After linearity estimation using a standard reference, the quantification of d- and l-EGT and d- and l-His in 15 mushroom species was performed. The results suggested that the d-EGT and d-His contents were low in all mushroom species tested, whereas sub-milligram-to-milligram-scale l-forms were detected in Pleurotus citrinopileatus, Pleurotus ostreatus, and Pleurotus eryngii var. ferulae species. Although %D was low, the presence of d-EGT in mushroom species was quantified for the first time. Furthermore, docking simulations were performed to investigate the differences in enzymatic interactions between carnitine/organic cation transporter 1 and 3‑mercaptopyruvate sulfurtransferase. The enantiomers of EGT demonstrate different affinities for 3-mercaptopyruvate sulfurtransferase.

麦角硫因（EGT）是一种天然强抗氧化剂，具有抗衰老作用，是一种很有前景的保健产品。EGT存在于各种蘑菇中，从生物学的角度研究其数量和性质，包括手性，是很重要的。本研究旨在建立一种液相色谱-串联质谱（LC-MS/MS）对映选择性分析EGT和组氨酸（His）的方法。该方法是基于对映化学标签（4-氯-6-甲氧基-1,3,5-三嗪-2-基）-d-和l-亮氨酸，到硫醇位点或胺基。该方法实现了d-和l- EGT以及d-和l- his对映体的清晰分离，灵敏度高（定量限达到70-200 fmol）。采用标准参比进行线性估计后，对15种蘑菇的d-和l-EGT以及d-和l-His进行了定量分析。结果表明，d-EGT和d-His在所有被试菌种中含量均较低，而在柑桔侧耳、平菇和阿魏侧耳中均检测到亚毫克-毫克级的l-形态。虽然%D含量较低，但首次对蘑菇中D - egt的含量进行了定量分析。此外，进行对接模拟以研究肉碱/有机阳离子转运体1和3巯基丙酮酸硫转移酶之间酶相互作用的差异。EGT的对映体对3-巯基丙酮酸硫转移酶表现出不同的亲和力。

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引用次数: 0

Machine learning and optical imaging for pharmaceutical forensic toxicology: A comprehensive review 药物法医毒理学的机器学习和光学成像：综合综述

Journal of Pharmaceutical and Biomedical Analysis Open

Pub Date : 2026-01-30 DOI: 10.1016/j.jpbao.2026.100104

Christian H. Pérez-Beltrán , Ana M. Jiménez-Carvelo , Eslim S. Sandoval-Sicairos , Ulises Osuna-Martínez , Cress L. Santos-Ballardo , Pablo Y. Carrazco-Ávila , Edith O. Cuevas-Rodríguez , Luis Cuadros-Rodríguez

Pharmaceutical forensic toxicology is undergoing a profound transformation driven by the convergence of optical imaging technologies and machine learning methodologies. Traditionally focused on post hoc legal investigations, the field is increasingly expanding toward proactive roles in pharmaceutical quality control, counterfeit drug detection, and public health protection. This review provides a comprehensive and critical overview of the integration of machine learning–based chemometrics with optical imaging techniques in pharmaceutical forensic toxicology. Imaging modalities ranging from grayscale and red, green, blue (RGB) imaging to infrared, Raman, multispectral, and hyperspectral imaging (MSI & HSI) are discussed, with emphasis on their physical principles, data structures, and analytical capabilities. The role of supervised and unsupervised chemometric multivariate models is examined in the context of classification, authentication, and quantitative assessment of pharmaceutical products. Current applications are reviewed across key forensic scenarios, including optical identification of counterfeit and illicit drugs, non-destructive evaluation of confiscated products, retrospective toxicological investigations, and emerging portable artificial intelligence-enabled platforms. Beyond technical performance, this review critically addresses regulatory, ethical, and legal challenges associated with artificial intelligence in forensic environments, highlighting the importance of explainability, traceability, and data governance. Finally, future perspectives are discussed, emphasizing the transition toward integrated forensic ecosystems that combine optical imaging, spectral databases, and interpretable machine learning to support robust, transparent, and legally defensible toxicological decision-making.

由于光学成像技术和机器学习方法的融合，药物法医毒理学正在经历一场深刻的变革。传统上侧重于事后的法律调查，该领域正在日益扩大，在药品质量控制、假药检测和公共卫生保护方面发挥积极作用。这篇综述提供了基于机器学习的化学计量学与光学成像技术在药物法医毒理学集成的全面和关键概述。讨论了从灰度和红、绿、蓝（RGB）成像到红外、拉曼、多光谱和高光谱成像（MSI & HSI）的成像模式，重点讨论了它们的物理原理、数据结构和分析能力。监督和非监督的化学计量多元模型的作用是在药品的分类，认证和定量评估的背景下进行检查。目前的应用在关键的法医场景中进行了审查，包括假药和非法药物的光学识别、没收产品的非破坏性评估、回顾性毒理学调查和新兴的便携式人工智能平台。除了技术性能之外，本综述还批判性地解决了与法医环境中人工智能相关的监管、道德和法律挑战，强调了可解释性、可追溯性和数据治理的重要性。最后，讨论了未来的前景，强调向综合法医生态系统的过渡，该生态系统结合了光学成像、光谱数据库和可解释的机器学习，以支持稳健、透明和法律上可辩护的毒理学决策。

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引用次数: 0

Advancements in magnetic MIP-based miniaturized techniques for pharmaceutical and biomedical analysis 基于磁性mip的药物和生物医学分析小型化技术的进展

Journal of Pharmaceutical and Biomedical Analysis Open

Pub Date : 2026-01-14 DOI: 10.1016/j.jpbao.2026.100102

Monireh Bakhshpour-Yücel , Fatma Yılmaz , Bilgen Osman , Adil Denizli

Magnetic materials have become essential for detecting and quantifying various analytes. Advances in technology and molecular recognition have further enhanced the capabilities of these materials, making them crucial components in developing efficient and versatile analytical systems across diverse fields, such as pharmaceuticals, biomedicine, and environmental analysis. One of the most promising innovations in this area is magnetic molecularly imprinted polymers. These materials combine molecular selectivity with the magnetic responsiveness of traditional magnetic materials. This hybrid technology improves analyte recognition and isolation, leading to increased extraction efficiency, speed, and reproducibility. Magnetic molecularly imprinted polymer-based materials allow for easier manipulation and separation of the polymer matrix using an external magnetic field, further enhancing their performance. They are particularly beneficial in applications that require rapid and reliable analyte extraction, facilitating faster on-site analysis and high-throughput screening. This review provides a comprehensive exploration of the principles, design strategies, and applications of magnetic molecularly imprinted polymers, focusing on their use in pharmaceuticals and biomedicine. These innovative materials also play an important role in enhancing the sensitivity and selectivity of sensor systems used in precise analyte detection. Magnetic molecularly imprinted polymers improve analyte extraction efficiency and enable rapid, real-time detection in various analytical applications. It also addresses current challenges and potential future directions for this technology.

磁性材料已成为检测和定量各种分析物的必要材料。技术和分子识别的进步进一步增强了这些材料的能力，使它们成为在制药、生物医学和环境分析等不同领域开发高效和通用分析系统的关键组成部分。磁性分子印迹聚合物是这一领域最有前途的创新之一。这些材料结合了传统磁性材料的分子选择性和磁性响应性。这种混合技术提高了分析物的识别和分离，从而提高了提取效率、速度和重现性。磁性分子印迹聚合物基材料允许使用外部磁场更容易地操作和分离聚合物基质，进一步提高其性能。它们在需要快速可靠的分析物提取的应用中特别有用，有助于更快的现场分析和高通量筛选。本文综述了磁性分子印迹聚合物的原理、设计策略和应用，重点介绍了磁性分子印迹聚合物在制药和生物医学方面的应用。这些创新材料在提高用于精确分析物检测的传感器系统的灵敏度和选择性方面也发挥着重要作用。磁性分子印迹聚合物提高了分析物的提取效率，并在各种分析应用中实现了快速、实时的检测。它还讨论了该技术当前面临的挑战和潜在的未来方向。

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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