Journal of Chromatography B最新文献_第6页

An optimized LC-ESI-MS/MS assay for erythrocyte 6-TG and 6-MMPD: Addressing critical methodological considerations for thiopurine metabolite monitoring 红细胞6-TG和6-MMPD的优化LC-ESI-MS/MS分析：解决硫嘌呤代谢物监测的关键方法学问题。

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-11-26 DOI: 10.1016/j.jchromb.2025.124872

Ya-Min Chu , Yuan-Yuan Zhang , Ya-Hui Hu , Jie Wang , Hong-Li Guo , Jin Xu , Yong-Jun Fang , Jing Xu , Xuan-Sheng Ding , Feng Chen

Thiopurines, a class of antimetabolites widely used in patients with inflammatory bowel disease (IBD) and acute lymphoblastic leukemia (ALL), are associated with two predominant adverse effects: delayed myelotoxicity and hepatotoxicity. The erythrocyte-based active metabolites 6-thioguanine nucleotides (6-TGN) and 6-methylmercaptopurine nucleotides (6-MMPN) serve as biomarkers reflecting systemic drug exposure and predicting both therapeutic efficacy and adverse reactions. In this study, we successfully developed and validated a rapid, sensitive, and accurate liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) analytical method for simultaneous quantification of erythrocyte 6-TG and 6-MMPD concentrations. During method development and validation, we focused on addressing the following five key challenges currently of significant interest in the field: 1) Erythrocytes proved superior to whole blood as biological matrix; 2) Perchloric acid was essential in sample pretreatment; 3) Dual mobile phase additives (HCOOH+NH₄Ac) enhanced chromatographic peak shape and detection sensitivity; 4) Incomplete hydrolysis of 6-TGN and 6-MMPN occurred with heating durations < 60 min; 5) The linear correlation coefficient of the 6-MMPD (6-MMP derivative, 4-amino-5-(methylthio)carbonyl imidazole) standard curve reflected the stable conversion efficiency of 6-MMP. The method exhibited excellent linearity over the concentration ranges of 0.06–50 μmol/L for 6-TG (r = 0.9906) and 0.18–150 μmol/L for 6-MMPD (r = 0.9914). Selectivity, carry-over, intra- and inter-batch accuracy and precision, reproducibility, recovery, matrix effect, and stability all complied with the acceptance criteria outlined in the US Food and Drug Administration (FDA) Bioanalytical Method Validation Guidance (2018). The validated method was successfully employed to quantify 6-TG and 6-MMPD in samples obtained from 20 patients with IBD or ALL.

硫嘌呤是一类广泛用于炎症性肠病（IBD）和急性淋巴细胞白血病（ALL）患者的抗代谢物，它与两种主要的不良反应相关：延迟性骨髓毒性和肝毒性。红细胞活性代谢物6-硫鸟嘌呤核苷酸（6-TGN）和6-甲基巯基嘌呤核苷酸（6-MMPN）可作为反映全身药物暴露的生物标志物，预测治疗疗效和不良反应。在本研究中，我们成功建立并验证了一种快速、灵敏、准确的液相色谱-电喷雾电离-串联质谱（LC-ESI-MS/MS）同时定量红细胞6-TG和6-MMPD浓度的分析方法。在方法开发和验证期间，我们专注于解决以下五个关键挑战，目前该领域的重大兴趣：1)红细胞被证明优于全血作为生物基质；2)样品预处理必须使用高氯酸；3)双流动相添加剂（HCOOH+NH4Ac）增强了色谱峰形和检测灵敏度；4) 6-TGN和6-MMPN在加热时间< 60 min时发生不完全水解；5) 6-MMPD （6-MMP衍生物，4-氨基-5-（甲基硫）羰基咪唑）标准曲线的线性相关系数反映了6-MMP稳定的转化效率。6-TG在0.06 ~ 50 μmol/L （r = 0.9906）和6-MMPD在0.18 ~ 150 μmol/L （r = 0.9914）的浓度范围内具有良好的线性关系。选择性、结转、批内和批间准确度和精密度、重现性、回收率、基质效应和稳定性均符合美国食品和药物管理局（FDA）生物分析方法验证指南（2018）中概述的验收标准。该方法被成功用于定量20例IBD或ALL患者样品中的6-TG和6-MMPD。

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引用次数: 0

Refreshing the Aims and Scope of the Journal of Chromatography B 更新色谱杂志的目标和范围B。

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-11-25 DOI: 10.1016/j.jchromb.2025.124865

David S. Hage, Huwei Liu, Georgios Theodoridis, Dimitrios Tsikas, Christina Virgilliou, Ian D. Wilson

引用次数: 0

UPLC-MS/MS-based targeted analysis of human serum revealed that aberrant arachidonic acid metabolism may contribute to the pathogenesis of type 2 diabetes mellitus 基于UPLC-MS/ ms的人血清靶向分析显示，花生四烯酸代谢异常可能与2型糖尿病的发病机制有关

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-11-25 DOI: 10.1016/j.jchromb.2025.124871

Peng Jin , Kun Wang , Xiao-wan Hu , Yi-fan Yang , Xian-jie Huang , Yan Du , Dao-quan Tang

The aberrant arachidonic acid (ARA) metabolism may contribute to the pathogenesis of type 2 diabetes mellitus (T2DM), and some metabolites from ARA may have benefits for the differential diagnosis of T2DM. Thus, the aim of this study was to develop an ultra-high performance liquid phase coupled with mass spectrometry (UPLC-MS/MS) for determination of ARA and its 11 metabolites in the serum of patients with T2DM and explore the relation between ARA metabolites and T2DM pathogenesis. A cohort of 66 healthy individuals and 141 patients with T2DM enrolled from Suining People's Hospital Affiliated to Xuzhou Medical University was studied. The UPLC-MS/MS technique was developed and applied to obtain the serum ARA and its 11 metabolite profiles. Multivariate statistical analysis referring to metabolomics were applied for the metabolites data analysis and the differential metabolites screening. The results showed that a total number of 6 differential metabolites were presented between T2DM patients and healthy control subjects. Among these differential metabolites, (±)14(15)-epoxyeicosatrienoic acid (EET) presented the 1.64-fold elevation in T2DM patients versus healthy control subjects, significant correlation with biochemical index [fasting blood glucose (FBG) and glycated hemoglobin (HbA1c)] (P < 0.01), and Receiver Operating Characteristic (ROC) area under the curve (AUC) of 0.6063 with the sensitivity of 26.95% and specificity of 93.94% (95% confidence interval, 0.5280–0.6846) for the diagnosis of T2DM. This study advances previous findings by establishing eicosatetraenoic acids flux imbalance as a hallmark of early T2DM pathogenesis, while providing an analytical blueprint for clinical translation of lipid mediator biomarkers in type 2 diabetic patients.

花生四烯酸（ARA）代谢异常可能与2型糖尿病（T2DM）的发病机制有关，ARA的一些代谢物可能有助于T2DM的鉴别诊断。因此，本研究的目的是建立一种超高效液相联用质谱法（UPLC-MS/MS）检测T2DM患者血清中ARA及其11种代谢物，并探讨ARA代谢物与T2DM发病机制的关系。选取徐州医科大学附属遂宁人民医院66名健康个体和141名T2DM患者作为研究对象。建立并应用UPLC-MS/MS技术获得血清ARA及其11种代谢物谱。代谢物数据分析和差异代谢物筛选采用代谢组学的多变量统计分析。结果显示，T2DM患者与健康对照组之间共存在6种差异代谢物。在这些差异代谢物中，（±）14(15)-环氧二碳三烯酸（EET）在T2DM患者中比健康对照组升高1.64倍，与生化指标[空腹血糖（FBG）和糖化血红蛋白（HbA1c）]有显著相关性（P < 0.01），受试者工作特征（ROC）曲线下面积（AUC）为0.6063，诊断T2DM的敏感性为26.95%，特异性为93.94%（95%可信区间为0.528 ~ 0.6846）。本研究进一步证实了二十碳四烯酸通量失衡是早期T2DM发病机制的标志，同时为2型糖尿病患者脂质介质生物标志物的临床翻译提供了分析蓝图。

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引用次数: 0

A method for simultaneous determination of triiodothyronine and thyroxine in fingernail clippings by LC/ESI-MS/MS hplc /ESI-MS/MS同时测定指甲屑中三碘甲状腺原氨酸和甲状腺素的方法

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-11-24 DOI: 10.1016/j.jchromb.2025.124869

Kenjiro Shibata , Sakurako Tanaka , Shuhei Baba , Arina Miyoshi , Norio Wada , Tatsuya Higashi

A fingernail clipping is a promising specimen for evaluating the medium-to-long term status of low-molecular weight hormones. However, the nail concentrations of thyroid hormones and their clinical significance remain poorly understood. In this study, a liquid chromatography/electrospray ionization-tandem mass spectrometry (LC/ESI-MS/MS) method was developed and validated for simultaneously quantifying triiodothyronine (T₃) and thyroxine (T₄) in the thumbnail clippings. The nail T₃ and T₄ were extracted with 50 % ethanol and purified using a Strata-X cartridge, then injected into the LC/ESI-MS/MS. ¹³C₆-T₄ was used as the internal standard for both T₃ and T₄. Validation results demonstrated that the method was precise (relative standard deviations in five repetitive measurements were ≤ 4.5 %) and accurate (analytical recovery rates were 98.3–103.3 %). The lower limits of quantification were 0.20 ng/g for both thyroid hormones. By using this method, we found that the nail concentrations of T₃ (0.74 ± 0.26 ng/g, mean ± standard deviation) were at the same level as those of T₄ (0.90 ± 0.27 ng/g) in euthyroid subjects (n = 40). This result might be caused due to the greater free and albumin-bound fractions of circulating T₃ compared to T₄. The patients with Graves' disease showed significantly higher nail T₃ and T₄ concentrations than the euthyroid subjects. The patients with hypothyroidism due to Hashimoto's thyroiditis tended to have lower nail T₃ and T₄ concentrations compared to the euthyroid subjects. Thus, the developed method would be useful for evaluating the medium-to-long term status of thyroid hormone production and has sufficient clinical applicability.

指甲修剪是评估低分子量激素中长期状态的有希望的标本。然而，指甲中甲状腺激素的浓度及其临床意义仍然知之甚少。本研究建立了一种液相色谱/电喷雾电离-串联质谱（LC/ESI-MS/MS）方法，用于同时测定缩略指甲剪影中的三碘甲状腺原氨酸（T3）和甲状腺素（T4）。采用50%乙醇提取T3、T4，经Strata-X试剂盒纯化后，进样于LC/ESI-MS/MS中。T3和T4均采用13C6-T4作为内标。验证结果表明，该方法精密度高（5次重复测定的相对标准偏差≤4.5%），准确度高（分析回收率为98.3 ~ 103.3%）。两种甲状腺激素的定量下限均为0.20 ng/g。结果显示，40例甲状腺功能正常的患者T3指甲浓度（0.74±0.26 ng/g，平均值±标准差）与T4指甲浓度（0.90±0.27 ng/g）基本一致。这一结果可能是由于与T4相比，循环T3的游离和白蛋白结合部分更大。Graves病患者指甲T3、T4浓度明显高于甲状腺功能正常者。桥本甲状腺炎所致甲状腺功能减退患者甲3、T4浓度较甲状腺功能正常者低。因此，该方法可用于评估甲状腺激素产生的中长期状态，具有足够的临床适用性。

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引用次数: 0

Coupling complementary sample preparation methods and two-dimensional gas chromatography mass spectrometry with novel data workflows to the case of pollution in and from salmon aquaculture 耦合互补样品制备方法和二维气相色谱质谱与新的数据工作流程，以鲑鱼养殖污染的情况下

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-11-22 DOI: 10.1016/j.jchromb.2025.124860

Lisbet Sørensen , Mari Egeness Creese , Marie Ibrekk , Rikke Torvanger , Raymond Nepstad , Julie Metzger , Trond R. Størseth , Julia Farkas , Bjørn Henrik Hansen

Abstract

Navigating in the intersection between constantly increasing knowledge about ‘novel’ pollutants and their potential impact on the environment and human health, and answering the demand by consumers for evidence of seafood safety, is a challenge for the aquaculture industry and regulators both. Non-target and suspect analytical methods may offer part of the solution to this challenge. In the current study, we developed and tested a novel pipeline for non-target screening for the presence of organic pollutants using complementary extraction protocols and two-dimensional gas chromatography coupled with mass spectrometry. The pipeline was applied to identify organic pollutants in muscle samples of farmed Atlantic salmon (Salmo salar). Potential sources (intrinsic or environmental) were investigated through comparative analysis of feed pellets and local sediment samples. While no legacy contaminants were detected in either sample, a small suite of compounds of anthropogenic origin (preservatives, biocides, plasticizers and other plastic or chemical-industry-related compounds, as well as antioxidants and UV-stabilizers) was confidently detected, some of which may be candidates for future monitoring and mitigation actions.

摘要在不断增长的关于“新型”污染物及其对环境和人类健康的潜在影响的知识之间导航，以及回答消费者对海产品安全证据的需求，是水产养殖业和监管机构面临的挑战。非目标和可疑分析方法可能为这一挑战提供部分解决方案。在目前的研究中，我们开发并测试了一种新的管道，用于使用互补提取协议和二维气相色谱与质谱相结合的非目标筛选有机污染物的存在。该管道被用于鉴定养殖大西洋鲑鱼（Salmo salar）肌肉样本中的有机污染物。通过对饲料颗粒和当地沉积物样本的比较分析，调查了潜在的来源（内在或环境）。虽然在两个样品中都没有检测到遗留污染物，但有信心检测到一小部分人为来源的化合物（防腐剂、杀菌剂、增塑剂和其他与塑料或化学工业有关的化合物，以及抗氧化剂和紫外线稳定剂），其中一些可能是未来监测和缓解行动的候选物质。

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引用次数: 0

Development and validation of an LC-MS/MS method for the simultaneous detection of urinary inflammatory biomarkers in a Flemish birth cohort 在佛兰德出生队列中同时检测尿液炎症生物标志物的LC-MS/MS方法的开发和验证。

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-11-21 DOI: 10.1016/j.jchromb.2025.124867

Fatima den Ouden , Adam Cseresznye , Liesa Engelen , Elias Maris , Ellen De Paepe , Giulia Poma , Sebastian Proost , Arnau Vich i Vila , Lieselot Y. Hemeryck , Roger Pero-Gascon , Sarah De Saeger , Jeroen Raes , Lynn Vanhaecke , Tim S. Nawrot , Adrian Covaci

Chronic inflammation is a significant contributor to various diseases but its assessment via blood sampling presents challenges, particularly in children. The evaluation of urinary biomarkers, including 3-bromotyrosine (Bty), 3-chlorotyrosine (Cty) and leukotriene E4 (LTE4), offers a non-invasive alternative. This study presents the optimization and validation of a sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the simultaneous quantification of Bty, Cty and LTE4 in urine. Under optimized conditions, sample preparation was based on SPE using Oasis MAX cartridges, followed by LC-MS/MS analysis. Method performance was validated using the ICH 10 guidelines, resulting in satisfactory results for all analytes in terms of recovery, linearity, limits of quantification, precision and accuracy. Recovery rates ranged from 82 % to 97 %, while matrix effects were observed within the range of −11 % to 26 %. Linear range spanned from 0.08 to 20 ng/mL for the three analytes. Application to 332 urine samples from the ENVIRONAGE birth cohort (Belgium), comprising of children aged 4–11 years, revealed detection frequencies of 18 % for LTE4, 19 % for Cty and 50 % for Bty. Notably, creatinine-corrected Cty and LTE4 exhibited statistically significant Spearman correlations with established systemic inflammation markers. Specifically, Cty was positively correlated with absolute monocyte count (ρ = 0.53, p < 0.05), while LTE4 showed a positive correlation with relative eosinophil levels (ρ = 0.46, p < 0.05) and a negative correlation with the relative neutrophil levels (ρ = −0.56, p < 0.01). These results highlight the validated method as a valuable tool for investigating distinct inflammatory pathways in epidemiological settings and clinical research.

慢性炎症是各种疾病的重要因素，但通过血液采样进行评估存在挑战，特别是在儿童中。尿液生物标志物的评估，包括3-溴酪氨酸（Bty）、3-氯酪氨酸（Cty）和白三烯E4 (LTE4)，提供了一种非侵入性的替代方法。本研究优化并验证了液相色谱-串联质谱（LC-MS/MS）同时定量尿液中Bty、Cty和LTE4的方法。在优化后的条件下，采用Oasis MAX色谱筒进行固相萃取制备样品，然后进行LC-MS/MS分析。使用ICH 10指南验证了方法的性能，在回收率、线性度、定量限、精密度和准确度方面，所有分析物的结果都令人满意。回收率为82% ~ 97%，基质效应为- 11% ~ 26%。三种分析物的线性范围为0.08 ~ 20 ng/mL。应用来自ENVIRONAGE出生队列（比利时）的332份尿液样本，包括4-11岁的儿童，显示LTE4的检测频率为18%，Cty为19%，Bty为50%。值得注意的是，肌酐校正后的Cty和LTE4与已建立的全身性炎症标志物具有统计学上显著的Spearman相关性。具体而言，Cty与绝对单核细胞计数呈正相关(ρ = 0.53, p

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引用次数: 0

Optimizing the uptake of deuterated docosapentaenoic acid by salmonid liver cells using a uniform shell design and liquid chromatography triple-quadrupole mass spectrometry 采用均匀壳设计和液相色谱三重四极杆质谱法优化鲑鱼肝细胞对氘化二十五烯酸的吸收

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-11-21 DOI: 10.1016/j.jchromb.2025.124863

Pedro Araujo , Zhenxiao Zhuang , Maren Hoff Austgulen , Bjørg Kristine Hundal

Stable isotope-labelled fatty acids are valuable tracers for studying lipid metabolism in cell models. However, published methods rarely provide guidance on selecting the optimal concentration and incubation time to ensure accurate and reproducible measurements of cellular uptake and metabolism that reflect physiological conditions. This study systematically evaluated the uptake of deuterated docosapentaenoic acid (DPA-d₅) in Atlantic salmon (Salmo salar L.) liver cells using a uniform shell design methodology. Cultures were exposed to DPA-d₅ at concentrations ranging from 0 to 100 μM for 24, 48, or 72 h and the uptake was quantified in cell lysates by liquid chromatography–mass spectrometry. Results indicate that the concentration of DPA-d₅ has the strongest positive influence on signal intensity. Incubation time slightly reduces the signal, but when combined with higher concentration, it increases the uptake of DPA-d₅. Modelling of the data allowed selecting 60 μM DPA-d₅ and 48 h as the optimal culturing condition that provides a balance between achieving a strong signal and minimizing the risk of oversaturation or metabolic artifacts. This work provides a methodological foundation for future fatty acid tracer experiments in aquaculture research.

稳定的同位素标记脂肪酸是研究细胞脂质代谢模型的重要示踪剂。然而，已发表的方法很少对选择最佳浓度和孵育时间提供指导，以确保准确和可重复地测量反映生理条件的细胞摄取和代谢。本研究采用统一的壳设计方法，系统地评估了大西洋鲑鱼（Salmo salar L.）肝细胞对氘化二十五烯酸（DPA-d5）的吸收。培养物暴露于浓度从0到100 μM的DPA-d5中24、48或72小时，并通过液相色谱-质谱法定量细胞裂解物的摄取。结果表明，DPA-d₅的浓度对信号强度有最强的正向影响。孵育时间会略微降低信号，但当与更高浓度结合时，它会增加DPA-d₅的吸收。数据建模允许选择60 μM DPA-d5和48 h作为最佳培养条件，在获得强信号和最小化过饱和或代谢伪像风险之间提供平衡。本研究为今后脂肪酸示踪剂在水产养殖研究中的实验奠定了方法学基础。

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引用次数: 0

Quantification of a sea lamprey (Petromyzon marinus) pheromone antagonist in river water using ion pairing solid phase extraction coupled with liquid chromatography-tandem mass spectrometry 离子对固相萃取-液相色谱-串联质谱法定量测定河水中一种海鳗信息素拮抗剂。

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-11-21 DOI: 10.1016/j.jchromb.2025.124866

Anne M. Scott, Sonam Tamrakar , Weiming Li

Pheromones mediate species-wide communication for many aquatic organisms, and the measurement of pheromones in natural waters is essential to understanding the environmental context of their function. However, chemical measurement of environmental pheromones and their antagonists is technically demanding and remains underdeveloped relative to assays for characterizing biological functions and application efficacy. In this study, we developed and validated an accurate and sensitive method to quantify a sea lamprey (Petromyzon marinus) pheromone and its antagonists. In this species, males release a multi-component sex pheromone containing 3-keto petromyzonol sulfate (3kPZS) that attracts females, while related compounds petromyzonol sulfate (PZS) and petromyzonol tetrasulfate (3sPZS) antagonize and disrupt female attraction. Developing methods to quantify 3sPZS in river water that contains pheromone is essential for understanding concentration-dependent effects of antagonists on invasive sea lamprey spawning. The target compound 3sPZS was extracted using triethylamine as an ion-pairing reagent during solid phase extraction followed by quantification using liquid chromatography-tandem mass spectrometry. The method showed a limit of detection of 0.1 ng/mL and limit of quantification of 0.5 ng/mL with linearity in the range of 10–1000 ng/mL. The intra- and inter-day accuracy, precision, recovery, and matrix effect of this method were evaluated. The method was applied to quantify 3sPZS, PZS, and 3kPZS in water sampled during field application in a river with sea lamprey and further evaluated for robustness by quantifying 3sPZS in 16 rivers across diverse environmental matrices. Our approach may be adapted to inform management strategies for detecting and mitigating invasive or imperiled aquatic species.

信息素介导了许多水生生物在物种范围内的交流，对自然水体中信息素的测量对于了解其功能的环境背景至关重要。然而，环境信息素及其拮抗剂的化学测量技术要求很高，相对于表征生物功能和应用效果的测定方法仍不发达。在本研究中，我们建立并验证了一种准确、灵敏的定量海七鳃鳗（Petromyzon marinus）信息素及其拮抗剂的方法。该物种雄性释放一种多组分性信息素，其中含有3-酮基石化苯二酚硫酸盐（3kPZS）吸引雌性，而相关化合物石化苯二酚硫酸盐（PZS）和石化苯二酚四硫酸酯（3sPZS）拮抗和破坏雌性的吸引力。研究含有信息素的河水中3sPZS的定量方法对于了解拮抗剂对入侵海七鳃鳗产卵的浓度依赖性作用至关重要。目的化合物3sPZS以三乙胺为离子配对试剂，固相萃取，液相色谱-串联质谱法定量。方法检出限为0.1 ng/mL，定量限为0.5 ng/mL，在10 ~ 1000 ng/mL范围内呈线性关系。评价了该方法的日内、日间准确度、精密度、回收率和基质效应。将该方法应用于一条有海七鳃鳗的河流的实地应用中，对采样水中的3sPZS、PZS和3kPZS进行量化，并通过对16条河流中不同环境矩阵的3sPZS进行量化，进一步评估其稳健性。我们的方法可以为检测和减轻入侵或濒危水生物种的管理策略提供信息。

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引用次数: 0

Recent advances in three-dimensional graphene and its derivatives for sample preparation in food contaminant analysis: A review 三维石墨烯及其衍生物在食品污染物分析样品制备中的研究进展

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-11-20 DOI: 10.1016/j.jchromb.2025.124862

Xuesheng Zhou , Fangyuan Li , Kun Jiang , Na Wang , Bo Cui

Due to their high specific surface area and extended π-conjugated systems, various three-dimensional graphene and its derivatives have been successfully synthesized and widely utilized for the enrichment of contaminants in food matrices. However, the diversity of synthetic approaches for these materials, coupled with their broad applicability in food contaminant extraction, has limited their effectiveness as a coherent and unified framework for guiding the development of detection methods. Therefore, it is assumed that a systematic review of these synthesis strategies, together with a comprehensive elucidation of the mechanisms underlying the extraction of various contaminants, would provide precise guidance for the design of detection methods based on such advanced materials. Based on this rationale, the review presents a systematic overview of the synthesis methods for three-dimensional graphene and its derivatives, accompanied by a critical evaluation of the advantages and limitations of each approach. Furthermore, it summarizes recent applications of these materials in the enrichment of diverse food contaminants and elucidates the underlying adsorption mechanisms. The results indicate that each synthetic method entails specific limitations: high energy consumption in hydrothermal and solvothermal methods, the use of toxic reagents in chemical reduction method, reliance on cross-linking agents in freeze-drying and three-dimensional printing techniques, and the requirement for sophisticated equipment in chemical vapor deposition. Nevertheless, integrating multiple approaches can effectively overcome the inherent drawbacks of individual methods, as demonstrated by the microwave-assisted hydrothermal method. Moreover, π–π stacking, hydrophobic, electrostatic interactions and hydrogen bonding collectively confer a distinct advantage in adsorption of aromatic food contaminants.

由于其高比表面积和扩展的π共轭体系，各种三维石墨烯及其衍生物已被成功合成，并广泛应用于食品基质中污染物的富集。然而，这些材料的合成方法的多样性，加上它们在食品污染物提取中的广泛适用性，限制了它们作为指导检测方法发展的连贯和统一框架的有效性。因此，假设对这些合成策略的系统回顾，以及对各种污染物提取机制的全面阐明，将为基于这些先进材料的检测方法的设计提供精确的指导。基于这一基本原理，本文对三维石墨烯及其衍生物的合成方法进行了系统概述，并对每种方法的优点和局限性进行了批判性评估。综述了近年来这些材料在各种食品污染物富集中的应用，并阐述了其潜在的吸附机制。结果表明，每种合成方法都有特定的局限性：水热法和溶剂热法的高能耗，化学还原法使用有毒试剂，冷冻干燥和三维打印技术依赖交联剂，化学气相沉积对精密设备的要求。然而，结合多种方法可以有效地克服单个方法的固有缺陷，微波辅助水热法证明了这一点。此外，π -π堆积、疏水、静电相互作用和氢键共同赋予了芳香食品污染物吸附的明显优势。

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引用次数: 0

Hierarchical C-Fe2O3@MnO2 nanostructured sorbent; application in dispersive-μ-solid phase extraction of antifungal drugs 分级C-Fe2O3@MnO2纳米结构吸附剂；分散μ-固相萃取法在抗真菌药物中的应用。

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-11-19 DOI: 10.1016/j.jchromb.2025.124858

Hanieh Riazi Bonab , Amir Abbas Matin , Mustafa Soylak

In the current work, a hierarchical nanocomposite based on MnO₂ nanosheets attached to the C-Fe₂O₃ substrate (C-Fe₂O₃@MnO₂) was introduced as a novel and efficient dispersive-μ-solid phase extraction sorbent. The well-prepared nanocomposite with unique morphology leading to higher surface area, high porosity, and excellent adsorptive capacity was used for preconcentration of antifungal drugs (ketoconazole, clotrimazole, and miconazole) from plasma and wastewater samples before analysis using high-performance liquid chromatography (HPLC-UV). The synthesized nanosorbent was characterized using XRD, FTIR, FE-SEM, BET/BJH, and EDX analysis. In the optimal condition, the limit of detection (LODs) and the limit of quantification (LOQs) were acquired as 1.5, 5.0 μg L⁻¹ in the linear range of 5–500 μg L⁻¹ in plasma samples and 0.3, 1.0 μg L⁻¹ in the linear range of 1–150 μg L⁻¹ in wastewater samples for all analytes. Furthermore, the relative standard deviations (RSD%) for the repeatability of the sorbent synthesis method and reusability of one sorbent were found to be 0.92, 1.23, 1.32 % and 2.43, 3.15, 4.28 % for ketoconazole, clotrimazole, and miconazole, respectively.

本文介绍了一种新型、高效的分散μ固相萃取吸附剂——MnO2纳米片与C-Fe2O3衬底（C-Fe2O3@MnO2）的层次化纳米复合材料。制备的纳米复合材料具有独特的形貌，具有更高的表面积、高孔隙率和优异的吸附能力，用于预富集血浆和废水样品中的抗真菌药物（酮康唑、克霉唑和咪康唑），然后使用高效液相色谱（HPLC-UV）进行分析。采用XRD、FTIR、FE-SEM、BET/BJH和EDX对合成的纳米吸附剂进行了表征。在最佳条件下，血浆样品在5 ~ 500 μ L-1线性范围内的检出限（lod）和定量限（loq）分别为1.5、5.0 μ L-1，废水样品在1 ~ 150 μ L-1线性范围内的定量限（loq）分别为0.3、1.0 μ L-1。酮康唑、克霉唑和咪康唑的重复性和可重复使用性的相对标准偏差（RSD%）分别为0.92、1.23、1.32%和2.43、3.15、4.28%。

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