Journal of Chromatography B最新文献_第10页

A cyclodextrin-deep eutectic solvent-based dispersive liquid-liquid microextraction method for quantitative determination of small molecules in fresh-cut Codonopsis Radix 环糊精-深共晶溶剂分散液-液微萃取法定量测定鲜切党参中的小分子。

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2026-01-01 Epub Date: 2025-11-05 DOI: 10.1016/j.jchromb.2025.124844

Yao Ma , Qing-nan Chen , Rui Liao , Yun-e Bai , Jian-kuan Li , Shuang Hu , Jian-ping Gao

In this study, a cyclodextrin-dispersive liquid-liquid microextraction-HPLC-based method was developed to quantitatively study four components of Codonopsis Radix (CR): carboxymethyl-β-cyclodextrin (CM-β-CD) was incorporated into the DES, then added to the sample solution, and the mixture was vortexed and centrifuged, the upper hydrophobic phase was then collected for HPLC analysis. The primary elements influencing the extraction efficiency were optimized to choose the circumstances for this experiment, including the type and consumption of cyclodextrin, the NaCl concentration, the pH level of the sample phase and the extraction time. The EFs for four target components extracted by cyclodextrin-DES were between 8.4 and 71.2, which were all higher than those extracted only by DES. In their respective linearity ranges, the four analytes exhibited good linearity (R² ≥ 0.99), with detection limits of 1.2 × 10⁻² μg/mL, 5.3 × 10⁻³ μg/mL, 3 × 10⁻⁴ μg/mL, and 1.1 × 10⁻⁴ μg/mL. The precision and accuracy of the method ranged from 0.8 % to 10.0 % and 90.0 % to 105.2 %. Finally, this method was applied to the quantification of fresh-cut CR and traditional-processed CR. The results showed that the content of tangshenoside I and lobetyolinin of fresh-cut CR was significantly higher than in traditionally processed CR, but there were no significant differences between fresh-cut CR and traditionally processed CR for lobetyolin and lobetyol. The use of CM-β-CD in combination with DES provides rapid, simple, and reliable quantification of the target analytes. By this method, differences between the two processing methods were compared at the level of small-molecule content, providing evidence for the feasibility of the fresh-cutting processing method and demonstrating a theoretical basis for the quality evaluation method of the fresh-cut process.

本研究建立了环糊精-分散液-液微萃取-高效液相色谱法定量研究党参（CR）的四种成分：将羧甲基-β-环糊精（CM-β-CD）掺入DES中，加入样品溶液中，旋涡离心，收集上部疏水相进行HPLC分析。对影响提取效率的主要因素进行了优化，选择了环糊精的种类、用量、NaCl浓度、样品相pH值、提取时间等条件。环糊精-DES法提取的4种目标成分的EFs均在8.4 ~ 71.2之间，均高于单纯DES法提取的结果，在各自的线性范围内，4种分析物均表现出良好的线性关系（R2≥0.99），检出限分别为1.2 × 10-2 μg/mL、5.3 × 10-3 μg/mL、3 × 10-4 μg/mL和1.1 × 10-4 μg/mL。方法精密度和准确度分别为0.8% ~ 10.0%和90.0% ~ 105.2%。最后，将该方法应用于鲜切CR和传统加工CR的定量分析，结果表明，鲜切CR中糖苷I和枇杷苷的含量显著高于传统加工CR，而鲜切CR与传统加工CR中枇杷苷和枇杷苷的含量差异不显著。CM-β-CD联合DES可快速、简便、可靠地定量分析目标分析物。通过该方法，比较了两种加工方法在小分子含量水平上的差异，为鲜切加工方法的可行性提供了依据，为鲜切工艺的质量评价方法提供了理论依据。

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引用次数: 0

Source and fate of ultra-short-chain PFAS in water and biota from an AFFF impacted site 受AFFF影响的水体和生物群中超短链PFAS的来源和命运。

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2026-01-01 Epub Date: 2025-11-09 DOI: 10.1016/j.jchromb.2025.124848

Magnus Sture , Stig Valdersnes , Stepan Boitsov , Bjørn Einar Grøsvik , Aasim Ali

This study adopted and validated a quantitative LC-MS/MS method for the rapid detection of five ultra-short-chain (USC) and three short chain (SC) per- and polyfluoroalkyl substances (PFAS) in diverse environmental matrices. The method was applied to soil from an active fire training site, as well as to freshwater and seawater, at and near Bergen airport, Norway, and was further validated for blue mussels. The total oxidizable precursor assay, applied to soil and aqueous film-forming foam (AFFF), provided evidence that AFFF-derived precursors in foam and contaminated soil degrade to USC PFAS, indicating the AFFF as continuing secondary source.

USC PFAS concentrations in freshwater ranged from 13 to 725 ng/L, with the highest levels detected at the fire training site. Seawater near the airport contained 10.4–14.9 ng/L, with concentration decreasing offshore. Depth profiling showed USC PFAS to be surface-associated. USC PFAS were also detected in mussels for the first time, both from urban and remote areas, indicating potential for bioaccumulation.

This study addresses an important methodological gap by validating and applying a reliable analytical approach for monitoring USC PFAS in complex matrices, thereby supporting advancements in environmental monitoring and regulation. The results reveal AFFF impacted sites as major point sources of USC-/SC-PFAS and highlight their high mobility, persistence, and potential bioaccumulation in mussels.

本研究采用并验证了LC-MS/MS定量检测不同环境基质中5种超短链（USC）和3种短链（SC）单氟烷基和多氟烷基物质（PFAS）的方法。该方法应用于一个活跃的火灾训练场地的土壤，以及挪威卑尔根机场及其附近的淡水和海水，并进一步验证了蓝贻贝的有效性。应用于土壤和水成膜泡沫（AFFF）的总可氧化前体测定提供了证据，证明泡沫和污染土壤中AFFF衍生的前体降解为USC PFAS，表明AFFF是持续的二次源。USC淡水中PFAS浓度范围为13至725 ng/L，在火灾训练现场检测到的浓度最高。机场附近海水浓度为10.4 ~ 14.9 ng/L，近海海水浓度逐渐降低。深度剖面显示USC PFAS与表面相关。在城市和偏远地区的贻贝中也首次检测到USC PFAS，表明其具有生物积累的潜力。本研究通过验证和应用一种可靠的分析方法来监测复杂矩阵中的USC PFAS，从而解决了一个重要的方法差距，从而支持环境监测和监管的进步。结果表明，AFFF影响位点是USC-/SC-PFAS的主要点源，并强调了它们在贻贝中的高移动性、持久性和潜在的生物积累。

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引用次数: 0

Validation and sample bioanalysis of protoporphyrin IX in rat plasma by the surrogate matrix approach 用替代基质法验证大鼠血浆中原卟啉IX的有效性及样品生物分析

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-12-15 Epub Date: 2025-09-22 DOI: 10.1016/j.jchromb.2025.124799

Aliz Széles , Károly Schöll , Gábor Hirka , Katalin Monostory , Tibor Renkecz

Protoporphyrin IX (PPIX) plays a pivotal role in the heme biosynthesis pathway and serves as both a valuable biomarker in clinical diagnostics and a photosensitizer in photodynamic applications. Despite its physiological importance, accurate quantification of endogenous PPIX in biological matrices remains challenging due to the lack of an analyte-free authentic control matrix and inherent baseline variability. This study describes the development and validation of a high-performance liquid chromatography method with fluorescence detection (HPLC-FLD) for PPIX quantification in rat plasma, applying a surrogate matrix strategy in full compliance with the International Council for Harmonisation M10 guideline.

Endogenous PPIX was removed from rat plasma by visible light-induced analyte stripping, enabling the in-house preparation of a surrogate matrix, for accurate calibration sample generation. The method showed appropriate selectivity, excellent linearity over the range of 10 and 700 ng/mL (r ≥ 0.995), satisfactory precision and accuracy across all validation levels. The lower limit of quantification was established at 10 ng/mL. The stability of both the analyte and internal standard was confirmed under various conditions, including 3 freeze–thaw cycles, short- and long-term storage, and autosampler residence. The method was successfully applied in an in vivo study in which male rats were treated with aminolevulinic acid to induce PPIX formation, thereby confirming its suitability for study sample analysis.

This fluorescence-based HPLC method offers a practical and cost-effective solution for monitoring PPIX in plasma samples. The bioanalytical method validation using a surrogate matrix approach for endogenous PPIX quantification fully aligned with current international regulatory standards may set a precedent for future method development in this field.

原卟啉IX （PPIX）在血红素生物合成途径中起着关键作用，在临床诊断中是一种有价值的生物标志物，在光动力学应用中是一种光敏剂。尽管其在生理上具有重要意义，但由于缺乏无分析物的真实对照基质和固有的基线可变性，对生物基质中内源性PPIX的准确定量仍然具有挑战性。本研究描述了一种用于大鼠血浆中PPIX定量的高效液相色谱荧光检测（HPLC-FLD）方法的开发和验证，该方法采用替代基质策略，完全符合国际协调理事会M10指南。内源性PPIX通过可见光诱导的分析物剥离从大鼠血浆中去除，使替代基质的内部制备成为可能，以准确校准样品的生成。该方法在10 ~ 700 ng/mL范围内具有良好的选择性和良好的线性关系（r≥0.995），在所有验证水平上具有良好的精密度和准确度。定量下限为10 ng/mL。分析物和内标物在3次冻融循环、短期和长期储存、自动进样器停留等条件下的稳定性得到了证实。该方法已成功应用于雄性大鼠氨基乙酰丙酸诱导PPIX形成的体内研究，从而证实了该方法适用于研究样本分析。这种基于荧光的高效液相色谱方法为监测血浆样品中的PPIX提供了一种实用且具有成本效益的解决方案。使用替代矩阵方法进行内源性PPIX定量的生物分析方法验证完全符合当前的国际监管标准，可能为该领域未来的方法开发开创先例。

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引用次数: 0

Development of a bispecific antibody-homodimer separation process by cation exchange chromatography based on mechanistic modelling 基于机制模型的双特异性抗体-同型二聚体阳离子交换色谱分离工艺的建立。

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-12-15 Epub Date: 2025-09-20 DOI: 10.1016/j.jchromb.2025.124801

Zichen Wang , Guohong Qin , Xiaoying Liang, Qingquan He, Qian Li, Hongyang Zhao, Guozhu Li, Dan Xu

During the recombinant production of IgG-like bispecific antibodies (bsAbs), homodimer formation, which stems from unbalanced chain expression and incorrect chain pairing, presents a major purification challenge. Despite its utility in addressing such charge-based separations, the development of cation exchange chromatography processes remains inherently complex due to the interplay of multiple parameters (e.g., salt concentration, loading conditions) that govern protein-resin interactions. For the separation of bsAb and homodimer, a mechanistic model of cation exchange chromatography was employed to predict the elution behavior, thereby facilitating the optimization of process conditions. The calibration processes and validation results of the extended Langmuir and steric mass action (SMA) two adsorption models were compared. The latter was selected for process optimization due to its streamlined calibration workflow, enabling efficient prediction of elution behavior. The optimal eluent concentration was determined to be 120 mM NaCl. Under this condition, the target bsAb yield reached 96.4 %, and homodimer 1 content was reduced from 26.4 % to 0.5 %. Deviations between the predicted and experimental results for both yield and impurity content were confined within 1.5 %, demonstrating the high accuracy and reliability of the established chromatographic mechanistic model for guiding process optimization.

在重组生产igg样双特异性抗体（bsAbs）的过程中，同源二聚体的形成是一个主要的纯化挑战，它源于不平衡的链表达和不正确的链配对。尽管阳离子交换色谱法在处理这种基于电荷的分离方面具有实用性，但由于控制蛋白质-树脂相互作用的多个参数（例如盐浓度、负载条件）的相互作用，其发展仍然具有内在的复杂性。对于bsAb和同型二聚体的分离，采用阳离子交换色谱的机理模型来预测洗脱行为，从而优化工艺条件。比较了扩展Langmuir和空间质量作用（SMA）两种吸附模型的标定过程和验证结果。后者被选择用于工艺优化，因为它简化了校准工作流程，能够有效地预测洗脱行为。确定最佳洗脱液浓度为120 mM NaCl。在此条件下，bsAb的产率达到96.4%，同型二聚体1的含量由26.4%降至0.5%。产率和杂质含量的预测结果与实验结果的偏差均在1.5%以内，表明所建立的色谱机理模型具有较高的准确性和可靠性，可指导工艺优化。

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引用次数: 0

Discrimination of isomeric dihydroflavone and chalcone by the boosting optimal collision energy-liquid chromatography-tandem mass spectrometry: A case study of pharmacokinetics in honey-fried licorice 增强最佳碰撞能-液相色谱-串联质谱法鉴别异构体二氢黄酮和查尔酮：以蜂蜜炒甘草中的药代动力学为例

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-12-15 Epub Date: 2025-09-03 DOI: 10.1016/j.jchromb.2025.124785

Yueting Li , Yan Cao , Tengteng Wang , Shengnan Cai , Yun Qiao , Chao Cheng , Jiale Gao , Jie Liu , Hongbin Xiao

The occurrence of isomeric dihydroflavone and chalcone, two important subfamilies of flavonoid class, extensively happens in herbal medicines. However, identical MS/MS spectra make the identity confirmation a tough job, the complexity will be further boosted in biological samples. Inspired by that isomers possess distinct inherent physicochemical parameters, optimal collision energy (OCE), which is positively correlated with the bond dissociation energies (BDEs), was evaluated towards differentiating isomeric dihydroflavone and chalcone. It was achieved by plotting their relative response-collision energy curves (RRCECs) and comparing the unique OCEs obtained. As a result, difference were observed for either OCE of bond dissociations involving Retro Diels-Alder (RDA) reaction as well as glycosidic cleavage when comparing two pairs of isomers, which were liquiritin vs. isoliquiritin and liquiritigenin vs. isoliquiritigenin, because the energies required for bond dissociation to produce identical fragment ions varies among isomers. Furthermore, OCEs consistently ranked dihydroflavone higher than chalcone, aligning with their BDEs determined through quantum calculation. These results suggested great potential for OCEs in distinguishing between dihydroflavone and chalcone. By applying the discriminating criterion, successful identity recognition was achieved for the two pairs of isomers among the many signals sharing identical MRM transitions in honey-fried licorice treated plasma. Thereafter, the confidence-enhanced OCE-LC-MS/MS method was applied to characterize and determine these 4 isomers along with 3 components of honey-fried licorice in rat plasma, the definite determination as well as the pharmacokinetic courses were subsequently accomplished and discussed. Overall, this study boosted the application of OCE-LC-MS/MS in isomers discrimination of isomeric dihydroflavone and chalcone.

异构体二氢黄酮和查尔酮是类黄酮的两个重要亚科，广泛存在于中草药中。然而，相同的MS/MS谱使鉴定工作变得困难，在生物样品中进一步增加了鉴定的复杂性。由于同分异构体具有不同的内在物理化学参数，本文利用最佳碰撞能（OCE）与键解离能（BDEs）之间的正相关关系，对二氢黄酮和查尔酮的同分异构体进行了判别。通过绘制它们的相对响应-碰撞能量曲线（RRCECs）并比较得到的唯一能量曲线来实现。结果，当比较两对异构体（甘草素与异甘草素、甘草素与异甘草素）时，观察到涉及Retro Diels-Alder （RDA）反应的键解离的OCE以及糖苷解离，两者都存在差异，因为不同异构体产生相同片段离子所需的键解离能量不同。此外，oce始终将二氢黄酮排在查尔酮之前，这与量子计算确定的bde一致。这些结果表明，OCEs在区分二氢黄酮和查尔酮方面具有很大的潜力。应用该判别准则，成功地对蜂蜜甘草处理血浆中具有相同MRM过渡的信号中的两对异构体进行了身份识别。随后，采用置信度增强的ce- lc -MS/MS方法对这4种异构体及3种蜂蜜炒甘草成分在大鼠血浆中的含量进行了表征和测定，并对其药代动力学过程进行了分析和讨论。本研究促进了ce - lc -MS/MS在二氢黄酮和查尔酮异构体鉴别中的应用。

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引用次数: 0

Retention time prediction of forensic compounds using ensemble machine learning and molecular descriptors 基于集成机器学习和分子描述符的法医化合物保留时间预测。

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-12-15 Epub Date: 2025-10-02 DOI: 10.1016/j.jchromb.2025.124812

Asena Avci Akca Ph.D. , Sefa Akca Ph.D.

Retention time (RT) prediction can greatly improve the efficiency of chromatographic workflows in forensic toxicology, especially in high-throughput or non-targeted analytical workflows. In the present study, we compare the performance of four ensemble machine learning models—Random Forest (RF), Extra Trees, XGBoost, and LightGBM—in predicting RTs of 229 structurally diverse forensic compounds. Each compound was represented by a minimal set of RDKit-derived descriptors and an extended feature space that combines Mordred descriptors and Morgan circular fingerprints. All RTs were experimentally measured under standardized reversed-phase liquid chromatographic conditions. Model performance was evaluated using coefficient of determination (R²) and root-mean-square error (RMSE). Results show that models trained on extended descriptors (>2000 molecular features) outperformed those trained on basic descriptors, with XGBoost showing the highest predictive power (R² = 0.718, RMSE = 1.23). Feature importance analysis showed that RTs are not only affected by global molecular properties like hydrophobicity and size but also by topological and electronic features. These results highlight the value of ensemble learning in RT prediction and demonstrate its practical utility in compound screening and chromatographic method development in forensic toxicology.

保留时间（RT）预测可以大大提高法医毒理学色谱工作流程的效率，特别是在高通量或非靶向分析工作流程中。在本研究中，我们比较了四种集成机器学习模型——随机森林（random Forest， RF）、Extra Trees、XGBoost和lightgbm——在预测229种结构不同的法医化合物的RTs中的性能。每个化合物都由rdkit派生的描述符的最小集合和一个扩展的特征空间来表示，该特征空间结合了莫德雷德描述符和摩根圆形指纹。所有rt均在标准化反相液相色谱条件下进行实验测量。采用决定系数（R2）和均方根误差（RMSE）评价模型的性能。结果表明，基于扩展描述符（bbb2000分子特征）训练的模型优于基于基本描述符训练的模型，其中XGBoost的预测能力最高（R2 = 0.718, RMSE = 1.23）。特征重要性分析表明，RTs不仅受疏水性和大小等整体分子性质的影响，还受拓扑和电子特征的影响。这些结果突出了集成学习在RT预测中的价值，并展示了其在法医毒理学中化合物筛选和色谱方法开发中的实际应用。

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引用次数: 0

Development and evaluation of CD45-conjugated magnetic particles-based host cell depletion for enhanced metagenomic next-generation sequencing in bloodstream infection 基于cd45共轭磁颗粒的宿主细胞耗竭技术的开发和评估，用于增强血液感染的新一代宏基因组测序。

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-12-15 Epub Date: 2025-10-15 DOI: 10.1016/j.jchromb.2025.124823

Weiwei Wu , Jingjing Song , Qiuyue Wu , Xin Wu , Ning Sun , Xinyi Xia

Metagenomic next-generation sequencing (mNGS) enables unbiased detection of human pathogens without prior assumptions. However, the direct detection of bloodstream infection pathogens is limited by host DNA interference, leading to the clinical adoption of microbial cell-free DNA mNGS (plasma cfDNA mNGS). This study developed a host cell depletion method based on immunomagnetic separation using CD45-conjugated magnetic particles (CD45-MPs, termed the IP method) to reduce host DNA interference and enhance mNGS performance for bloodstream pathogen detection. In simulated samples, known concentrations of pathogens (intact Escherichia coli and Candida albicans cells, fragmented Staphylococcus aureus genomic DNA) were spiked into whole blood samples, serially diluted 10-fold, and divided into whole blood, plasma, and IP-treated groups. These groups were analyzed using hematological analysis, microscopic smear, DNA concentration measurement, relative quantification of GAPDH using qPCR, and mNGS. Results showed that CD45-conjugated magnetic particles effectively removed host cells from whole blood (reducing cell count by 99.9%). The results of nucleic acid measurement and qPCR indicated that the supernatant from IP-treated samples contained significantly lower host DNA compared to whole blood and plasma groups. mNGS detection of simulated samples demonstrated that the IP method enabled detection of pathogens at concentrations as low as 100 CFU/mL for E. coli and S. aureus, and 50 CFU/mL for C. albicans. In clinical testing of 77 samples from patients with suspected bloodstream infections, mNGS combined with the IP method showed significantly higher positivity rates than plasma cfDNA mNGS. In conclusion, CD45-conjugated magnetic particles effectively deplete human cells and enhance the clinical performance of mNGS on the detection of bloodstream infections.

新一代宏基因组测序（mNGS）能够在没有事先假设的情况下公正地检测人类病原体。然而，直接检测血液感染病原体受到宿主DNA干扰的限制，导致临床采用微生物无细胞DNA mNGS（血浆cfDNA mNGS）。本研究开发了一种基于免疫磁分离的宿主细胞耗尽方法，使用CD45-MPs （CD45-MPs，称为IP方法）来减少宿主DNA干扰，提高mNGS在血液病原体检测中的性能。在模拟样本中，将已知浓度的病原体（完整的大肠杆菌和白色念珠菌细胞，金黄色葡萄球菌基因组DNA片段）加入全血样本中，依次稀释10倍，并分为全血、血浆和ip处理组。通过血液学分析、显微镜涂片、DNA浓度测定、qPCR相对定量GAPDH和mNGS对各组进行分析。结果表明，cd45偶联磁颗粒能有效去除全血中的宿主细胞（使细胞计数减少99.9%）。核酸测定和qPCR结果表明，与全血和血浆组相比，ip处理样品的上清液中宿主DNA含量明显降低。模拟样品的mNGS检测表明，IP方法可以检测到大肠杆菌和金黄色葡萄球菌浓度低至100 CFU/mL，白色念珠菌浓度低至50 CFU/mL。在77例疑似血流感染患者的临床检测中，mNGS联合IP法的阳性率明显高于血浆cfDNA mNGS。综上所述，cd45偶联磁颗粒能有效消耗人体细胞，增强mNGS检测血流感染的临床性能。

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引用次数: 0

A pharmacokinetic study on punicalagin following oral and intravenous administration to the rat using UPLC-MS/MS 采用超高效液相色谱-质谱联用技术对大鼠口服和静脉注射槟榔苷的药代动力学进行研究

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-12-15 Epub Date: 2025-10-26 DOI: 10.1016/j.jchromb.2025.124837

Zhanying Chang , Guihua Liu , Zixin Chen , Pengxia Yao , Xiaoli Gao

Punicalagin (PUN) is a high abundant ellagitannin and the principal bioactive component existing in Pomegranate (Punica granatum L.) peel, juice, and extract, yet its absorption, bioavailability and pharmacokinetic parameters have not been adequately investigated after oral administration in vivo model. Thus, this study developed a reproducible UPLC-MS/MS method (linear range: 0.125–70 μg/mL; LLOQ: 0.125 μg/mL) to characterize PUN pharmacokinetic profile in Sprague-Dawley rats. After intravenous (iv, 10 mg/kg) administration, PUN exhibited slow elimination (iv, t_1/2 = 6.45 ± 2.11 h) and plasma-restricted distribution (V_d = 0.94 ± 0.23 L/kg). By intragastric route (ig, 100–400 mg/kg), PUN showed dose-dependent absorption (T_max ≈ 2 h), critically low absolute bioavailability (3.22–5.38%) and extensive tissue distribution (V_d = 14.0–44.5 L/kg). The area under the plasma concentration-time curve from time zero to last sampling time (AUC_0-t) and AUC_0-∞ (from time zero to infinity) were 30.0–211.5, 32.0–213.8 μg*h/mL. The C_max of PUN in plasma samples was ranged from 1.91 to 34.8 μg/mL. The dose proportionality study demonstrated the C_max and AUC_0-t values were positively correlated with ig doses, with R² (95% CI) being 0.858 (0.770–0.959) for C_max and 0.904 (0.847–0.956). Overall, the comprehensively detailed pharmacokinetic parameters of pure PUN have been determined, providing valuable information for preclinical study.

Punicalagin （PUN）是一种含量较高的鞣花单宁，是石榴（Punica granatum L.）果皮、果汁和提取物中存在的主要生物活性成分，但经体内模型口服后，其吸收、生物利用度和药代动力学参数尚未得到充分研究。因此，本研究建立了一种可重复的UPLC-MS/MS方法（线性范围：0.125 ~ 70 μg/mL；下限：0.125 μg/mL）来表征双关醇在Sprague-Dawley大鼠体内的药动学特征。经静脉（iv, 10 mg/kg）给药后，PUN消除缓慢（iv, t1/2 = 6.45±2.11 h），血浆分布受限（Vd = 0.94±0.23 L/kg）。经灌胃（ig, 100 ~ 400 mg/kg）， PUN具有剂量依赖性吸收（Tmax≈2 h），极低的绝对生物利用度（3.22 ~ 5.38%）和广泛的组织分布（Vd = 14.0 ~ 44.5 L/kg）。从时间0到最后一次采样时间的血浆浓度-时间曲线下面积（AUC0-t）和AUC0-∞（从时间0到无穷远）分别为30.0 ~ 211.5、32.0 ~ 213.8 μg*h/mL。血浆样品中PUN的Cmax为1.91 ~ 34.8 μg/mL。剂量比例研究表明，Cmax和AUC0-t值与大剂量呈正相关，Cmax和AUC0-t值的R2 （95% CI）分别为0.858（0.77 ~ 0.959）和0.904（0.847 ~ 0.956）。总之，我们全面详细地确定了纯双关醇的药代动力学参数，为临床前研究提供了有价值的信息。

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引用次数: 0

Novel isotope-coded derivatization of carboxylic acids provides accurate quantification of Azaspiracids in shellfish by liquid chromatography–tandem mass spectrometry 新型的同位素编码衍生化羧酸提供了液相色谱-串联质谱法对贝类中氮杂螺酸的准确定量

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-12-15 Epub Date: 2025-10-22 DOI: 10.1016/j.jchromb.2025.124826

Shimba Kawasue, Kyoko Kuniyoshi, Takashi Kurohara, Koji Fujihara, Yutaka Abe, Naoki Sugimoto, Masashi Uema, Naomasa Oshiro

The combination of isotope-coded derivatization (ICD) and liquid chromatography–tandem mass spectrometry (LC–MS/MS) is an excellent analytical method that could be applied to various compounds. However, the ICD reagents are expensive, which limits the use of this method for general testing including the evaluation of food safety and quality. Therefore, we synthesized reasonable ICD reagents, isopropyl piperidine carboxylic acid hydrazide (IPPAH) and isopropyl-piperidine carboxylic acid hydrazide-d₆ (IPPAH-d₆) using readily available acetone‑d₆, which reacts with the carboxy groups in the presence of a condensing agent to give a mass difference of six. It is applicable to carboxylic acids with a wide range of molecular weights. The application of the combination of ICD and LC/MS method to the analysis of the shellfish toxin azaspiracid in shellfish showed a significant improvement in the matrix effects (93.5–99.6 %). The method quality was evaluated by analyzing the certified reference material. The established method achieved an accurate quantification (95.7–103 %) of AZAs in shellfish specimens.

同位素编码衍生化（ICD）与液相色谱-串联质谱（LC-MS /MS）相结合是一种适用于多种化合物的优良分析方法。然而，ICD试剂价格昂贵，这限制了该方法用于一般检测，包括食品安全和质量评价。因此，我们利用丙酮-d6合成了合理的ICD试剂，异丙基哌啶羧酸肼（IPPAH）和异丙基哌啶羧酸肼-d6 (IPPAH-d6)，丙酮-d6在缩合剂的存在下与羧基反应，得到6的质量差。适用于分子量范围广的羧酸。将ICD与LC/MS相结合的方法应用于贝类中贝类毒素氮氮唑酸的分析，基质效应明显改善（93.5 ~ 99.6%）。通过对标准物质的分析，评价了方法的质量。建立的方法对贝类标本中AZAs的定量准确度为95.7 ~ 103%。

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引用次数: 0

Therapeutic effects of Panax ginseng polysaccharides on qi deficiency diabetes: Insights from microbiomics and metabolomics 人参多糖对气虚型糖尿病的治疗作用：来自微生物学和代谢组学的见解

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-12-15 Epub Date: 2025-08-29 DOI: 10.1016/j.jchromb.2025.124781

Yang Gao , Yi Wu , Meiyuan Wang , Shu Liu , Zhongying Liu

Panax ginseng, a traditional medicinal and edible plant valued for its tonifying properties, exhibits diverse pharmacological activities, including anti-fatigue, anti-oxidation and anti-diabetes. Polysaccharides represent a key active ingredient of Panax ginseng, known for their immunomodulatory properties and potential for development as health foods. However, the effect and mechanism of Panax ginseng polysaccharides (GP) on improving qi deficiency diabetes (QDD) is still unclear. In this study, a multi-omics approach integrating microbiomics, untargeted and targeted metabolomics was used to elucidate the protective effect and mechanisms of GP based on the QDD rat model. Furthermore, the prebiotic effects of GP were explored through microbiome and metabolome profiling. GP demonstrated significant therapeutic efficacy in QDD rats, manifested by the amelioration of hyperlipidemia and insulin resistance, reduction of oxidative stress, enhancement of immune responses, and restoration of intestinal injury. Untargeted fecal metabolomics and 16S rRNA gene sequencing revealed that GP significantly altered the abundance of 31 metabolites and corrected gut microbiota dysbiosis in QDD rats. Additionally, GP ameliorated bile acid metabolism disorders, significantly increased short-chain fatty acids (SCFAs) levels, and reduced branched-chain amino acids (BCAAs) concentrations. Spearman correlation analysis further confirmed significant associations between gut microbes and metabolites. Thus, GP exerts its therapeutic effect on QDD by ameliorating intestinal flora imbalance and associated metabolic disorders involving bile acids, branched-chain amino acids, and short-chain fatty acids. Together, these findings provide a foundation for the further development of GP-based functional foods.

人参是一种具有滋补功效的传统药用和食用植物，具有抗疲劳、抗氧化、抗糖尿病等多种药理活性。多糖是人参的一种关键活性成分，以其免疫调节特性和发展为保健食品的潜力而闻名。然而，人参多糖（GP）对气虚型糖尿病（QDD）的改善作用及其机制尚不清楚。本研究基于QDD大鼠模型，采用微生物组学、非靶向代谢组学和靶向代谢组学相结合的多组学方法，阐明GP的保护作用及其机制。此外，通过微生物组和代谢组分析探讨了GP的益生元效应。GP对QDD大鼠表现出明显的治疗效果，表现为改善高脂血症和胰岛素抵抗，降低氧化应激，增强免疫反应，恢复肠道损伤。非靶向粪便代谢组学和16S rRNA基因测序显示，GP显著改变了QDD大鼠31种代谢物的丰度，并纠正了肠道微生物群失调。此外，GP改善了胆汁酸代谢紊乱，显著增加了短链脂肪酸（SCFAs）水平，降低了支链氨基酸（BCAAs）浓度。Spearman相关分析进一步证实了肠道微生物与代谢物之间的显著相关性。由此可见，GP对QDD的治疗作用是通过改善肠道菌群失衡及相关的胆胆酸、支链氨基酸和短链脂肪酸代谢紊乱来实现的。总之，这些发现为进一步开发以gp为基础的功能性食品提供了基础。

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引用次数: 0