Journal of pharmaceutical and biomedical analysis最新文献_第10页

Lipidome changes indicate oxidative stress, inflammation, and specific loss of glycerophosphoserine inflammatory protection in patients with lupus 脂质组改变提示狼疮患者氧化应激、炎症和甘油磷丝氨酸炎症保护的特异性丧失

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis

Pub Date : 2025-12-03 DOI: 10.1016/j.jpba.2025.117302

Jeremy P. Koelmel , Paula S. Ramos , Kaylie Anne Costa , Krystal J. Godri-Pollitt , Diane L. Kamen , John A. Bowden

Systemic lupus erythematosus (SLE, lupus) is a chronic autoimmune disease which has a complex etiology and suffers from both high false positive rates and false negative rates in diagnosis and classification. Substantial lipid changes have been observed previously in lupus patients, hence we carried out the most comprehensive lipidomics study in lupus to date using LipidMatch Flow. In this study, we investigated various sub-categories of lupus including lupus nephritis, active versus non-active lupus, as well as comparisons to non-lupus controls. A total of 1105 unique lipids spanning 36 lipid classes (or sub-classes) were annotated in blood plasma samples; of these, 111 lipids changed significantly between controls and active lupus. We determined for the first time, specific oxidized lipid markers, with oxidized triacylglycerols being the most significantly increased lipid sub-class in active lupus as compared to controls. Other indicators of oxidative stress included decreased lipids containing ether linkages and/or polyunsaturated fatty acids. Increased Cer(d18:1/16:0) and decreased C20–22 containing species (especially C20:4) indicated an inflammatory response in patients with active lupus. Furthermore, we determined a significant decrease of glycerophosphoserines, which are known inflammation suppressors, in patients with lupus and a decrease in Coenzyme Q9 and Q10; supplementation of lupus patients with Coenzyme Q10 has been shown to be protective [1–4]. Several unique lipids with unknown biology are also shown to significantly changed in active lupus. Many of these trends were also observed in non-active lupus, suggesting lipidomics related changes may occur early in disease development. In conclusion, this comprehensive lipidomics study expands our knowledge of the lipid alterations associated with lupus, providing insights into disease pathogenesis and depleted lipids, which could serve as therapeutic targets.

系统性红斑狼疮（SLE, lupus）是一种病因复杂的慢性自身免疫性疾病，在诊断和分类上假阳性率和假阴性率都很高。先前在狼疮患者中观察到大量的脂质变化，因此我们使用LipidMatch Flow进行了迄今为止最全面的狼疮脂质组学研究。在这项研究中，我们调查了狼疮的各种亚类别，包括狼疮肾炎，活动性与非活动性狼疮，以及与非狼疮对照的比较。在血浆样本中总共标注了1105种独特的脂质，跨越36个脂类（或亚类）；其中，111种脂质在对照组和活动期狼疮患者之间发生了显著变化。我们首次确定了特异性氧化脂质标志物，与对照组相比，氧化甘油三酯是活动期狼疮中最显著增加的脂质亚类。氧化应激的其他指标包括含有醚键和/或多不饱和脂肪酸的脂质减少。在活动期狼疮患者中，Cer（d18:1/16:0）升高，C20-22含种（尤其是C20:4）减少表明炎症反应。此外，我们确定了狼疮患者甘油磷酸丝氨酸（已知的炎症抑制因子）的显著减少，辅酶Q9和Q10的减少；狼疮患者补充辅酶Q10已被证明具有保护作用[1-4]。一些独特的脂质与未知的生物学也显示显着改变活动性狼疮。在非活动性狼疮中也观察到许多这些趋势，表明脂质组学相关的变化可能发生在疾病发展的早期。总之，这项全面的脂质组学研究扩展了我们对与狼疮相关的脂质改变的认识，提供了对疾病发病机制和脂质耗尽的见解，可以作为治疗靶点。

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引用次数: 0

Evaluation of photochemical behavior of ebastine and elucidation of its photoproducts 巴斯汀光化学行为的评价及其光产物的解析。

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis

Pub Date : 2025-12-02 DOI: 10.1016/j.jpba.2025.117288

Kohei Kawabata , Yukina Tokunaga , Yoko Nunome , Shiori Akimoto , Naoto Uramaru , Masanori Inagaki , Hiroyuki Nishi

Ebastine (EB) is a second-generation histamine H₁ receptor antagonist and utilized for the relief of allergy symptoms. In this study, the photodegradability of EB in an aqueous media was evaluated and the chemical structures of generated photoproducts were elucidated. EB photodegradation was monitored using high-performance liquid chromatography (HPLC), and two EB photoproducts were observed in HPLC chromatograms along with the decrease of EB contents in sample solutions. To elucidate their chemical structures, electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) analysis was carried out. From the mass to charge ratio values of molecular ion peaks and the fragmentation patterns, two EB photoproducts were designated as benzophenone and 4′-tert-butylacetophenone, respectively. Moreover, for the better understanding of EB photodegradation, photodegradation pathways of EB were speculated based on the structures of photoproducts. The photodegradation pathways of EB seemed to be an oxidative elimination of diphenyl methylene moiety and a Norrish type Ⅱ reaction. Finally, in silico toxicity prediction was performed for the estimation of toxicological potencies of EB photoproducts, suggesting the nature of EB might be changed by the photodegradation. In conclusion, two novel EB photoproducts were clarified and their formation mechanisms were proposed, which might make it possible to the better understanding of EB photodegradability.

依巴斯汀（EB）是第二代组胺H1受体拮抗剂，用于缓解过敏症状。本研究考察了EB在水介质中的光降解性，并对其光产物的化学结构进行了分析。采用高效液相色谱法（HPLC）监测EB的光降解情况，并观察到两种EB光产物随样品溶液中EB含量的降低而变化。采用电喷雾电离串联质谱（LC-ESI-MS/MS）分析了它们的化学结构。从分子离子峰的质量电荷比值和断裂模式可以确定两个EB光产物分别为二苯甲酮和4′-叔丁基lacetophenone。此外，为了更好地理解EB的光降解，根据光产物的结构推测了EB的光降解途径。EB的光降解途径似乎是氧化消除二苯基亚甲基和Norrish型Ⅱ反应。最后，对EB光产物的硅毒性进行了预测，表明EB的性质可能会因光降解而发生改变。总结了两种新的EB光产物，并提出了它们的形成机理，为更好地了解EB光降解性提供了可能。

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引用次数: 0

Quantification of Polymyxin E in Plasma and Epithelial Lining Fluid: Validation and Clinical Application 血浆和上皮内膜液中多粘菌素E的定量测定：验证及临床应用

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis

Pub Date : 2025-12-02 DOI: 10.1016/j.jpba.2025.117301

Shengnan Zhang , Ruwei Yang , Hongyi Tan , Ruiying Xie , Yejun Li , Jingjing Liu , Chun Liu , Qi Pei

Polymyxin E (PME) is an essential “last-resort” antibiotic for multidrug-resistant Gram-negative infections, but its narrow therapeutic window and high pharmacokinetic variability necessitate therapeutic drug monitoring (TDM). In this study, we developed and validated a sensitive LC–MS/MS method for quantifying PME in plasma and epithelial lining fluid (ELF) from patients receiving colistin sulfate therapy. Plasma and bronchoalveolar lavage samples were processed by protein precipitation with a 1:1 mixture of 5 % aqueous trichloroacetic acid and acetonitrile and analyzed on a triple quadrupole mass spectrometer, with validation according to FDA/EMA guidelines. Retrospective analysis of plasma samples from 40 critically ill patients revealed that trough concentrations, but not peak levels, differed significantly between patients with and without acute kidney injury (median, 1.50 vs. 0.79 μg/mL, p = 0.021). No clear correlation with clinical efficacy was observed. In a prospective cohort, paired plasma and ELF data from four patients suggested that inhaled administration produced markedly higher ELF concentrations than plasma concentrations, providing the first clinical evidence of pulmonary drug exposure after colistin sulfate inhalation. Overall, this validated method is suitable for routine TDM of PME. The findings support future studies to evaluate plasma trough levels and ELF concentrations in guiding individualized therapy for critically ill patients.

多粘菌素E （PME）是治疗多重耐药革兰氏阴性感染必不可少的“最后手段”抗生素，但其狭窄的治疗窗口和高药代动力学变异性需要治疗药物监测（TDM）。在这项研究中，我们开发并验证了一种灵敏的LC-MS /MS方法，用于定量接受硫酸粘菌素治疗的患者血浆和上皮衬里液（ELF）中的PME。血浆和支气管肺泡灌洗液样品用5 %三氯乙酸和乙腈的1:1混合物进行蛋白质沉淀处理，并在三重四极杆质谱仪上进行分析，并根据FDA/EMA指南进行验证。回顾性分析40例危重患者的血浆样本，发现急性肾损伤患者与非急性肾损伤患者的血药谷浓度差异显著（中位数为1.50 vs. 0.79 μg/mL, p = 0.021）。与临床疗效无明显相关性。在一项前瞻性队列研究中，来自4名患者的配对血浆和ELF数据表明，吸入给药产生的ELF浓度明显高于血浆浓度，这为吸入硫酸粘菌素后肺部药物暴露提供了第一个临床证据。总体而言，该方法适用于PME的常规TDM。该研究结果支持未来评估血浆谷水平和ELF浓度的研究，以指导危重患者的个体化治疗。

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引用次数: 0

Stability of expired tropane alkaloid ampoules using HPLC-UV/CAD HPLC-UV/CAD检测过期莨菪碱安瓿的稳定性。

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis

Pub Date : 2025-11-30 DOI: 10.1016/j.jpba.2025.117297

Sylvia Klapper, Ulrike Holzgrabe

Medicines often have a much longer shelf life than stated by the manufacturer. Due to the high costs of emergency stockpiling, but also due to supply shortages, an extended shelf life can offer many advantages. In this study, three injection solutions containing atropine, scopolamine and belladonna total alkaloids, respectively, manufactured between 1940 and 1960 and stored under uncontrolled conditions, were tested, to show that pharmaceutical products, containing tropane alkaloids, are significantly more stable than expected after some 80 years. To analyze the stability of the main alkaloids atropine and scopolamine, a method using charged aerosol detection (CAD) was developed and validated. CAD enables the detection of degradation products that lack a chromophore and cannot be detected using pharmacopoeial (UV) methods. For separation a SIELC Primesep 200 column (4.6 ×150 mm; 100 Å; 3 µm) and gradient elution with water, acetonitrile and formic acid were used. The results indicated a high stability of atropine, with a determined content of 101.9 % and a small amount of degradation products. Scopolamine, however, showed higher degree of degradation with a remaining content of 68 %.

药品的保质期通常比制造商所声明的要长得多。由于紧急储存的成本很高，而且由于供应短缺，延长保质期可以提供许多好处。在这项研究中，对1940年至1960年间生产并在无控制条件下储存的三种分别含有阿托品、东莨菪碱和颠茄总生物碱的注射溶液进行了测试，结果表明，含有莨菪总生物碱的药品在大约80年后的稳定性明显高于预期。为了分析其主要生物碱阿托品和东莨菪碱的稳定性，建立并验证了带电气溶胶检测法（CAD）。CAD能够检测缺乏发色团且无法使用药典（UV）方法检测的降解产物。分离采用SIELC Primesep 200色谱柱（4.6 ×150 mm; 100 Å； 3 µm），用水、乙腈和甲酸梯度洗脱。结果表明，阿托品稳定性高，测定含量为101.9 %，降解产物较少。而东莨菪碱的降解程度较高，残留含量为68% %。

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引用次数: 0

A MA-SSA-optimized XGBoost-MLP framework using LIBS for rapid classification and quantitative analysis of heavy metals in traditional chinese medicines 基于LIBS的ma - ssa优化的XGBoost-MLP框架用于中药中重金属的快速分类和定量分析

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis

Pub Date : 2025-11-29 DOI: 10.1016/j.jpba.2025.117296

Abulimiti Yasen , Yuxia Zhou , Wenhan Gao , Zhongxin Zhang , Reyihan Tudi , Mei Xiang , Bumaliya Abulimiti

Laser-Induced Breakdown Spectroscopy (LIBS) holds significant value for rapid elemental detection; however, strong spectral interference, matrix effects, and high-dimensional data characteristics pose considerable challenges to accurate quantitative analysis. To enhance the performance of LIBS quantitative analysis, this study proposes a novel machine learning framework that integrates XGBoost and Multilayer Perceptron (MLP), optimized by a Multi-dimensional Adaptive Sparrow Search Algorithm (MA-SSA). The framework employs XGBoost for automated feature selection, eliminating redundant spectral variables while retaining critical information, and utilizes MA-SSA to optimize the hyperparameters of the MLP in regression tasks, significantly improving model stability and prediction accuracy. Experimental results demonstrate that the proposed method achieves 100 % accuracy in multi-class classification, outperforming traditional classifiers such as Random Forest, XGBoost, and standalone MLP. In terms of quantitative detection, the MA-SSA-optimized model achieves an RMSE of 4.43 µg/g, surpassing other hybrid optimization models including XGBoost-SSA-MLP (RMSE=4.62 µg/g), XGBoost-PSO-MLP (RMSE=5.225 µg/g), and XGBoost-GA-MLP (RMSE=5.584 µg/g). XGBoost-based feature selection effectively reduces spectral dimensionality while maintaining predictive performance. The proposed MA-SSA algorithm further enhances convergence efficiency and generalization capability. This study provides a robust, efficient, and scalable solution for LIBS analysis, with broad application potential in the field of real-time quantitative detection.

激光诱导击穿光谱（LIBS）在元素快速检测中具有重要价值；然而，强烈的光谱干扰、矩阵效应和高维数据特征给准确的定量分析带来了相当大的挑战。为了提高LIBS定量分析的性能，本研究提出了一种新的机器学习框架，该框架集成了XGBoost和多层感知器（MLP），并通过多维自适应麻雀搜索算法（MA-SSA）进行优化。该框架采用XGBoost进行自动特征选择，在保留关键信息的同时消除冗余光谱变量，并利用MA-SSA优化回归任务中MLP的超参数，显著提高模型稳定性和预测精度。实验结果表明，该方法在多类分类中准确率达到100% %，优于传统的随机森林、XGBoost、独立MLP等分类器。在定量检测方面，ma - ssa优化模型的RMSE为4.43 µg/g，超过了XGBoost-SSA-MLP （RMSE=4.62 µg/g）、XGBoost-PSO-MLP （RMSE=5.225 µg/g）和XGBoost-GA-MLP （RMSE=5.584 µg/g）等混合优化模型。基于xgboost的特征选择有效地降低了谱维数，同时保持了预测性能。提出的MA-SSA算法进一步提高了收敛效率和泛化能力。本研究为LIBS分析提供了一个稳健、高效、可扩展的解决方案，在实时定量检测领域具有广阔的应用潜力。

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引用次数: 0

Comprehensive analysis of pore properties of ultra-wide pore size exclusion chromatography packing materials 超宽孔径排阻色谱填料的孔隙特性综合分析。

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis

Pub Date : 2025-11-29 DOI: 10.1016/j.jpba.2025.117280

Szabolcs Fekete , Mateusz Imiołek , Matthew Lauber , Siqi Ji , Oksana D. Tchoul , MingCheng Xu

Accurate characterization of size exclusion chromatography (SEC) packing materials is critical for understanding separation behavior, particularly for the emerging class of large biotherapeutic and nanoparticle analytes. In this study, we present a comprehensive and multi-technique assessment of the pore structure of modern wide-pore and ultra-wide-pore SEC columns. Mercury intrusion porosimetry (MIP) and advanced scanning electron microscopy (SEM) image analysis with broad ion beam milling were employed alongside SEC calibration using rigid gold nanoparticles (AuNPs) and double-stranded DNA (dsDNA) ladders as complementary pore probes. Various models (including Ogston, Tanford-type sigmoidal fits, and Richards' function) were applied to interpret partitioning data and estimate effective pore diameters and pore size distributions (PSDs). While general agreement among methods was observed, systematic differences in absolute pore size values and distribution shapes reflected the distinct physical principles and dimensionalities of each method. The integration of rigid nanoparticle and nucleic-acid probes provides a unified framework for evaluating pore accessibility across a broad size range, offering new insights into the performance of ultra-wide-pore SEC columns used in biopharmaceutical separations of viral vectors, plasmids, and lipid nanoparticles.

粒径排阻色谱（SEC）包装材料的准确表征对于理解分离行为至关重要，特别是对于新兴的大型生物治疗和纳米颗粒分析物。在本研究中，我们对现代宽孔和超宽孔SEC柱的孔隙结构进行了综合和多技术评价。采用汞侵入孔隙度法（MIP）和先进的扫描电子显微镜（SEM）图像分析与宽离子束铣刀结合，并使用刚性金纳米颗粒（AuNPs）和双链DNA （dsDNA）梯子作为互补的孔隙探针进行SEC校准。应用各种模型（包括Ogston、tanford型s型拟合和Richards’s函数）来解释分区数据并估计有效孔径和孔径分布（psd）。虽然观察到各种方法之间的总体一致，但绝对孔径值和分布形状的系统差异反映了每种方法不同的物理原理和维度。刚性纳米颗粒和核酸探针的集成提供了一个统一的框架，以评估在广泛的尺寸范围内的孔可达性，提供了新的见解，用于生物制药分离病毒载体，质粒和脂质纳米颗粒的超宽孔SEC柱的性能。

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引用次数: 0

Identification and quantification of sesquiterpenes, alkaloids, flavonoids and coumarins in Artemisia annua L: Potential artemisinin activity-enhancing compounds 黄花蒿中倍半萜、生物碱、黄酮类和香豆素的鉴定与定量：潜在的青蒿素活性增强化合物。

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis

Pub Date : 2025-11-29 DOI: 10.1016/j.jpba.2025.117295

Jing Zhang , Shuaichen Zhang , Cheng Wang , Yifan Zhao , Dunfang Wang , Peng Sun

Artemisia annua L. (qinghao) is renowned for its antimalarial properties, primarily attributed to artemisinin. However, the compounds that can enhance the antimalarial activity of artemisinin have not been fully explored. Here, we performed untargeted metabolomics using UHPLC-QTOF-MS/MS to characterize 103 chemical constituents in A. annua, including 31 sesquiterpenes (11 artemisinin-type compounds first discovered in QH), 24 alkaloids (21 first discovered in QH), 36 flavonoids, 8 coumarins, and 4 other types of compounds. Quantitative analysis revealed dynamic seasonal variations in these metabolites, with artemisinin content significantly higher in May and June than April. Intriguingly, April-collected samples exhibited superior antimalarial efficacy, suggesting the presence of active ingredients that enhance the efficacy of artemisinin. Heatmap and bioactivity correlation analyses identified seven candidate efficacy-enhancing active ingredients (compounds 3, 15, 18, 69, 87, 90 and 100) that were significantly enriched in April samples, and verified the potent enhance effect of compounds 69 and 90 with artemisinin. These findings validate sesquiterpenes, alkaloids, flavonoid and coumarins co-occurrence may enhance artemisinin's antimalarial activity. Our study establishes a metabolic foundation for optimizing A. annua harvesting and developing novel antimalarial formulations.

青蒿以其抗疟特性而闻名，主要归因于青蒿素。然而，能够增强青蒿素抗疟活性的化合物尚未得到充分的探索。本研究采用UHPLC-QTOF-MS/MS对黄花蒿中的103种化学成分进行了非靶向代谢组学分析，包括31种倍半萜（其中11种为首次发现的青蒿素类化合物）、24种生物碱（其中21种为首次发现的）、36种黄酮类化合物、8种香豆素和4种其他类型的化合物。定量分析显示，这些代谢物具有动态的季节变化，5月和6月的青蒿素含量显著高于4月。有趣的是，4月份采集的样品显示出优越的抗疟疾功效，这表明存在增强青蒿素功效的活性成分。通过热图和生物活性相关性分析，鉴定出7个候选增效活性成分（化合物3、15、18、69、87、90和100）在4月样品中显著富集，并验证了化合物69和90与青蒿素的强效增效作用。这些发现证实倍半萜、生物碱、类黄酮和香豆素的共存可能增强青蒿素的抗疟活性。本研究为优化黄花蒿采收和开发新型抗疟制剂奠定了代谢基础。

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引用次数: 0

Economical chiral and achiral separation of seven impurities in brivaracetam by supercritical fluid chromatography with polysaccharide-based chiral stationary phases 超临界流体色谱-多糖基手性固定相对布瓦西坦中7种杂质进行经济的手性和非手性分离。

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis

Pub Date : 2025-11-28 DOI: 10.1016/j.jpba.2025.117287

Qingying Jia , Xiaodan Qiu , Xuejia Zhao , Huiyi Liu , Yongsheng Gu , Kun Xiao , Xinran Zhang , Xun Ma , Guangzhi Shan

Due to the presence of multiple chiral centers in its structure, the analysis of brivaracetam and its enantiomers, diastereomers, as well as non-isomeric impurities imposes high requirements on the separation capability of chromatographic methods. In this study, a rapid, accurate, and environmentally friendly supercritical fluid chromatography (SFC) method was developed for the simultaneous separation and quantification of seven isomeric and non-isomeric impurities in brivaracetam. The effects of chromatographic parameters—including stationary phase, mobile phase composition, column temperature, and back pressure—on the selective separation and quantification of the target compounds were systematically investigated. The results indicated that optimal separation was achieved using an amylose tris(3,5-dimethylphenylcarbamate)-based stationary phase, with a mobile phase consisting of carbon dioxide and methanol (containing 0.2 % diethylamine, v/v) under gradient elution conditions. Van’t Hoff analysis revealed that the separation process was primarily enthalpy-driven. Molecular docking studies further confirmed that hydrogen bonding and π–σ interactions were the main binding forces between the analytes and the stationary phase. These thermodynamic and molecular simulation results complemented each other and provided a rational explanation for the elution order of the impurities. The method demonstrated good accuracy (95.5 % - 105.5 %) and intermediate precision (RSD < 3 %) over the validated concentration range, with limits of detection (LOD) ranging from 1.743 to 4.207 ng, indicating high reliability and sensitivity. Moreover, the developed SFC method outperformed the reference methods from the European Pharmacopoeia in terms of analysis throughput and environmental friendliness. This study serves as a reference for the development of efficient and environmentally sustainable impurity analysis methodologies for drugs with multiple chiral centers.

由于布瓦西坦结构中存在多个手性中心，分析布瓦西坦及其对映体、非对映体和非同分异构体杂质对色谱方法的分离能力提出了很高的要求。本研究建立了一种快速、准确、环保的超临界流体色谱（SFC）方法，用于同时分离和定量布瓦西坦中7种异构体和非异构体杂质。系统考察了固定相、流动相组成、柱温和背压等色谱参数对目标化合物选择性分离和定量的影响。结果表明，在梯度洗脱条件下，以直链淀粉三（3,5-二甲基苯基氨基甲酸酯）为固定相，以二氧化碳和甲醇（含0.2 %二乙胺，v/v）为流动相，分离效果最佳。范霍夫分析表明，分离过程主要是由焓驱动的。分子对接研究进一步证实了氢键和π-σ相互作用是分析物与固定相的主要结合力。这些热力学和分子模拟结果相互补充，为杂质的洗脱顺序提供了合理的解释。该方法在有效浓度范围内具有良好的准确度（95.5 % ~ 105.5 %）和中等精密度（RSD < 3 %），检出限（LOD）范围为1.743 ~ 4.207 ng，具有较高的可靠性和灵敏度。此外，该方法在分析通量和环境友好性方面优于欧洲药典的参考方法。本研究为开发高效、环保的多手性中心药物杂质分析方法提供了参考。

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引用次数: 0

Exploring the anti-tuberculosis activity mechanism of OTB-658: Multi-omics analysis 探讨OTB-658抗结核作用机制：多组学分析。

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis

Pub Date : 2025-11-27 DOI: 10.1016/j.jpba.2025.117286

Qiyue Jia , Shaochen Guo , Bin Wang , Hui Zhu , Yu Lu

OTB-658, a novel oxazolidinone for tuberculosis, is designed to provide improved efficacy and safety compared to linezolid (LZD) in combination with bedaquiline and pretomanid (BPaL). Preclinical evaluations have demonstrated its superior efficacy profile compared to LZD, coupled with enhanced safety characteristics in cellular models and animal studies, positioning it as a potential successor to address current therapeutic limitations. However, the mechanisms underlying these actions have not been completely elucidated. In this study, multi-omics analyses are employed to detect regularities and patterns that reveal the action mechanism of OTB-658. The clinically drug-resistant strains showed significant cross-resistance to both LZD and OTB-658, and identical mutation sites to those of LZD were also identified, indicating that these inhibitors might exert their effects through an overlapping mechanism. Through an integrative approach combining whole genome, proteomics, transcriptomics, the results suggest that OTB-658 exerts its antimicrobial effects by targeting the 50S ribosomal subunit, thereby disrupting bacterial protein synthesis. This study is significant for advancing the drug's clinical trial research process and the application of OTB-658 in the treatment.

OTB-658是一种治疗结核病的新型恶唑烷酮，与利奈唑胺（LZD）与贝达喹啉和普雷托马胺（BPaL）联合使用相比，其疗效和安全性更高。临床前评估表明，与LZD相比，其疗效优于LZD，并且在细胞模型和动物研究中具有增强的安全性，使其成为解决当前治疗局限性的潜在继任者。然而，这些作用背后的机制尚未完全阐明。本研究采用多组学分析方法检测OTB-658作用机制的规律和模式。临床耐药菌株对LZD和OTB-658均表现出明显的交叉耐药，并且发现了与LZD相同的突变位点，表明这两种抑制剂可能通过重叠机制发挥作用。通过结合全基因组、蛋白质组学和转录组学的综合方法，结果表明OTB-658通过靶向50S核糖体亚基，从而破坏细菌蛋白质合成来发挥其抗菌作用。本研究对推进该药物的临床试验研究进程及OTB-658在治疗中的应用具有重要意义。

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引用次数: 0

Integrating plant metabolomics, chemometrics and mimic processing to elucidate dynamic changes and underlying mechanisms in the chemical profiles of Rehmanniae Radix Carbonisata during stir-frying carbonization 整合植物代谢组学、化学计量学和模拟加工，阐明炒制碳化过程中地黄化学特征的动态变化及其潜在机制。

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis

Pub Date : 2025-11-26 DOI: 10.1016/j.jpba.2025.117284

Pei-Yao Huang , Meng-Tao Zhang , Bi-Xia Jin , Hu-Dong Lv , Qian Mao , Jing Zhou , Cheng-Ying Wu , Fang Long , Shan-Shan Zhou , Hong Shen , Song-Lin Li , Jin-Di Xu , Ming Kong

Rehmanniae Radix Carbonisata (RRC) is a carbonization-processed product of Rehmanniae Radix (RR). Exploring the dynamic chemical profile changes and involved mechanisms is key to exploring the quality markers and standardized processing of RRC. Here, hyphenated chromatographic techniques-based plant metabolomics, qualitative characterization of polysaccharides were integrated to explore the chemical dynamic changes of RRC with different stir-frying duration. Totally 41 non-sugar small molecules (NSMCs) and 26 oligosaccharides were screened as differential chemicals of RRC and RR. These chemicals together with polysaccharides showed two quantitative variation patterns: 1) furfural and its glycosides, acteoside, martynoside/isomartynoside/isomer, two unknown di/tri-saccharides, melibiose, mannotriose, dehydrated di/tri/tetra/penta-saccharides, and polysaccharides were increased initially, then decreased; 2) iridoid, phenylethanoid and ionone glycosides, as well as sucrose, raffinose, one unknown trisaccharide and tetra/penta-saccharides decreased gradually. Furthermore, the molecular weight distribution range of total polysaccharides was split from 1 peak to 4 peaks in RRC, with the main compositional monosaccharide, galactose and arabinose, dynamically changed oppositely. Mimic processing of polysaccharides as well as representative differential NSMCs and oligosaccharides revealed that the dynamic chemical changes might be attributed to the interconversion of these chemicals and transformation into other compounds via deglycosylation and/or dehydration, in addition to furfurals previously confirmed. This study provides scientific basis for exploring quality markers and the standardized processing of RRC.

生地黄是生地黄的碳化加工产品。探究其化学特征的动态变化及其机制是探究其质量标志和标准化加工的关键。本研究结合以联用色谱技术为基础的植物代谢组学、多糖的定性鉴定等方法，探讨不同炒制时间下RRC的化学动态变化。共筛选出41个非糖小分子（NSMCs）和26个低聚糖作为RRC和RR的鉴别化学物质。这些化学物质与多糖的数量变化呈现出两种模式：1)糠醛及其糖苷、毛囊苷、马丁苷/异马钱子苷/异构体、两种未知二/三糖、蜜利二糖、甘露糖、脱水二/三/四/五糖，多糖含量先增加后减少；2)环烯醚萜类、苯乙醇类和离子酮类糖苷，以及蔗糖、棉子糖、一种未知三糖和四/五糖逐渐减少。此外，RRC中总多糖的分子量分布范围从1个峰分裂为4个峰，主要成分单糖、半乳糖和阿拉伯糖的分子量动态变化相反。多糖的模拟加工以及具有代表性的差异NSMCs和低聚糖揭示了动态化学变化可能归因于这些化学物质的相互转化，并通过脱糖基化和/或脱水转化为其他化合物，除了先前证实的糠醛。本研究为开发红参质量标记及红参标准化加工提供了科学依据。

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