Journal of Chromatography B最新文献_第4页

Overcoming the challenge of Protein A resin sanitisation: Evaluating the efficacy of peracetic acid as a novel sanitisation solution for MabSelect SuRe LX resin impacted by spore-forming bacteria 克服蛋白A树脂消毒的挑战：评估过氧乙酸作为一种新型消毒溶液对受孢子形成细菌影响的MabSelect SuRe LX树脂的效果

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-12-03 DOI: 10.1016/j.jchromb.2025.124889

Aoife Corr, Aoife Kearney, Aida Aliefendic, Beth Kirschenheiter, Donal Monaghan, Adam Curtin, Pamela O'Brien

Effective sanitisation of Protein A chromatography resin is critical for commercial monoclonal antibody (mAb) production, enabling microbial control and resin reuse. An effective strategy encompasses; resin compatibility with sanitising agents, microbial inactivation, and the removal of residual impurities from the resin. Sodium hydroxide (NaOH) is typically used for resin sanitisation. However, certain spore-forming microorganisms demonstrate resistance to NaOH, even at high concentrations. Alternative sanitising approaches are required to address potential spore-forming bioburden ingress. This paper introduces peracetic acid (PAA) as an alternative to NaOH for remediating MabSelect SuRe LX (MSLX) Protein A resin impacted by spore forming bacteria such as Paenibacillus glucanolyticus, Bacillus subtilis, and Paenibacillus polymyxa. PAA at a 20 mM concentration demonstrated superior microbial control to 0.5 M NaOH. A single 60 min exposure to 20 mM PAA was carried out, followed by continuous cycling until 100 h of NaOH exposure was achieved. Protein A chromatography cycles were conducted at laboratory scale using two distinct mAbs under two loading conditions. A reduction in step yield was observed at the maximum loading condition, suggesting that PAA exposure contributes to a reduction in resin binding capacity. Sufficient binding capacity was maintained when loading at manufacturing-scale relevant ranges for both mAb A & mAb B. Impurity clearance was not impacted following PAA exposure. A manufacturing-scale verification assessment confirmed that a single exposure to 20 mM PAA for 60 min is a suitable remedial treatment for MSLX resin in response to NaOH-resistant bioburden ingress.

蛋白A层析树脂的有效消毒对于商业单克隆抗体（mAb）生产至关重要，可以实现微生物控制和树脂再利用。有效的策略包括：树脂与杀菌剂的相容性，微生物灭活，并从树脂中去除残留杂质。氢氧化钠（NaOH）通常用于树脂消毒。然而，某些孢子形成微生物表现出对NaOH的抗性，即使在高浓度。需要替代的消毒方法来解决潜在的孢子形成的生物负担进入。本文介绍了过氧乙酸（PAA）作为NaOH的替代品，用于修复MabSelect SuRe LX （MSLX）蛋白A树脂，该树脂受到产孢细菌如葡解芽孢杆菌、枯草芽孢杆菌和多粘芽孢杆菌的影响。20 mM浓度的PAA对0.5 M NaOH的微生物控制效果较好。单次暴露于20 mM PAA 60分钟，然后连续循环，直到NaOH暴露100小时。在两种负载条件下，使用两种不同的单抗在实验室规模上进行蛋白A层析循环。在最大负载条件下，观察到阶梯产率的降低，表明PAA暴露有助于树脂结合能力的降低。当在生产规模的相关范围内加载mAb和mAb时，保持足够的结合能力。接触PAA后，杂质清除不受影响。一项生产规模的验证评估证实，单次暴露于20 mM PAA 60分钟是MSLX树脂对耐氢氧化钠生物负荷侵入的一种合适的补救处理。

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引用次数: 0

Integrated chemometric and spectrum-effect analysis discriminates Belamcanda chinensis and Iris tectorum in treating A549 lung cancer cells 综合化学计量学和光谱效应分析鉴别了白菖蒲和鸢尾对A549肺癌细胞的治疗作用

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-12-01 DOI: 10.1016/j.jchromb.2025.124875

Li-Jun Ruan , Bing-Xiong Yan , Yun-Qiu Wu , Ru-Xin Liu , Shan-Shan Song , Cai-Yun Yao , Feng-Li Huang , Zhi-Jun Song

Belamcanda chinensis (射干, She Gan, SG) and Iris tectorum (川射干, Chuan She Gan, CS), morphologically similar Iridaceae species with overlapping phytochemistry and respiratory applications, are frequently misused in traditional and modern practice. This study established a comprehensive differentiation strategy for SG and CS by integrating chemical characterization with pharmacological evaluation to identify bioactive markers. Twenty-nine herbal samples (11 CS, 18 SG) were analyzed for extraction yields, HPLC fingerprints, isoflavone quantification, multivariate chemometric analysis, in vitro cytotoxicity assessment, and spectrum-effect correlations. CS exhibited significantly higher extraction yields (44.8 % vs. 23.4 %) and total isoflavonoid content (168.7 vs. 42.6 mg/g) than SG, which correlated with stronger cytotoxicity against A549 cells. Chemometric analysis (PCA, PLS-DA and HCA) distinguished species-specific markers: tectoridin/ iristectorin A & B/ iristectorigenin B dominated CS, while irigenin characterized SG. In cytotoxicity assays using A549 cells at concentrations of 50–400 μg/mL, CS extracts showed significantly stronger dose-dependent cytotoxicity (93.6 % to 32.1 % viability reduction) compared to SG extracts (102.8 % to 68.3 %). PLSR-based spectrum-effect relationship analysis at 100/200 μg/mL linked eleven chromatographic peaks to bioactivity, with tectoridin, iristectorin A, and iristectorigenin B demonstrating strong correlations. Experimental validation confirmed these monomers as key cytotoxic agents. In summary, our integrated chemometric and spectrum-effect analysis showed stronger cytotoxicity of CS versus SG in A549 cells, with tectoridin, iristectorin A, and iristectorigenin B identified as potential quality markers. This study establishes a reliable chemometric-bioassay approach for bioactive marker discovery and herb-herb differentiation in traditional medicine. Further validation in diverse models and mechanistic studies is needed.

Belamcanda对(射干,她甘,SG)和虹膜tectorum(川射干,栓她甘,CS),形态相似的鸢尾科物种与重叠的植物化学和呼吸系统应用程序,在传统和现代实践中经常被误用。本研究通过化学表征与药理评价相结合的方法，建立了SG和CS的综合鉴别策略，以鉴定其生物活性标记物。对29份中草药样品（11份CS， 18份SG）进行了提取率、HPLC指纹图谱、异黄酮定量、多元化学计量分析、体外细胞毒性评估和光谱效应相关性分析。CS的提取率（44.8% vs. 23.4%）和总异黄酮含量（168.7 vs. 42.6 mg/g）显著高于SG，且CS对A549细胞具有较强的细胞毒性。化学计量分析（PCA， PLS-DA和HCA）区分了种特异性标记：鸢尾苷/鸢尾苷A和鸢尾苷B/鸢尾苷B以CS为主，而鸢尾苷以SG为特征。在浓度为50 ~ 400 μg/mL的A549细胞的细胞毒性实验中，CS提取物的细胞毒性（活性降低93.6% ~ 32.1%）明显强于SG提取物（活性降低102.8% ~ 68.3%）。在100/200 μg/mL浓度下，基于plsr的光谱效应关系分析将11个色谱峰与生物活性联系起来，鸢尾鸢尾素、鸢尾鸢尾鸢尾素A和鸢尾鸢尾鸢尾素B显示出很强的相关性。实验验证证实这些单体是关键的细胞毒性药物。综上所述，我们的综合化学计量学和光谱效应分析显示，CS比SG在A549细胞中具有更强的细胞毒性，鸢尾鸢尾素、鸢尾鸢尾鸢尾素A和鸢尾鸢尾鸢尾素B被确定为潜在的质量标记。本研究为中药生物活性标志物的发现和中草药鉴别建立了一种可靠的化学计量学-生物测定方法。需要在不同的模型和机制研究中进一步验证。

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引用次数: 0

Development and validation of a UPLC-MS/MS assay for serum choline and phosphocholine with a pilot application to obesity 开发和验证UPLC-MS/MS测定血清胆碱和磷脂胆碱的方法，并试点应用于肥胖。

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-11-30 DOI: 10.1016/j.jchromb.2025.124870

Yingting Wu , Jiaqi Xin , Haiyan Cao , Yongsheng Zhao , Mengxi Jiang

The rising global burden of obesity underscores the need to better characterize metabolic alterations associated with this condition. Choline (Cho) and its derivative phosphocholine (ChoP) are key intermediates in phospholipid metabolism, yet their relationships with obesity remain unclear. In this study, we established and validated a UPLC-MS/MS method for quantifying serum Cho and ChoP, and investigated their associations with obesity and fasting glucose in a pilot human cohort. Serum samples from 62 participants (obese vs. nonobese) were analyzed. The primary analysis compared metabolite levels between groups, and key secondary analyses included Pearson correlations with fasting glucose and receiver operating characteristic (ROC)-based discrimination; two-sample Mendelian randomization (MR) was conducted using external GWAS summary statistics. Obese individuals had lower ChoP levels and ChoP/Cho ratios. ChoP and the ChoP/Cho ratio were inversely associated, and Cho was positively associated, with fasting glucose. ChoP showed modest discriminative ability for obesity, and MR suggested that higher ChoP levels may be related to a lower risk of obesity. Overall, we validated a UPLC-MS/MS assay for serum Cho and ChoP, and our findings indicate that ChoP and the ChoP/Cho ratio are linked to obesity and glucose status.

全球肥胖负担的增加强调了更好地描述与肥胖相关的代谢变化的必要性。胆碱（Cho）及其衍生物磷脂胆碱（ChoP）是磷脂代谢的关键中间体，但它们与肥胖的关系尚不清楚。在这项研究中，我们建立并验证了一种UPLC-MS/MS定量血清Cho和ChoP的方法，并研究了它们与肥胖和空腹血糖的关系。分析了62名参与者（肥胖与非肥胖）的血清样本。主要分析比较各组之间的代谢物水平，关键的次要分析包括与空腹血糖的Pearson相关性和基于受试者工作特征（ROC）的区分；采用外部GWAS汇总统计进行双样本孟德尔随机化（MR）。肥胖个体的ChoP水平和ChoP/Cho比值较低。ChoP和ChoP/Cho比值与空腹血糖呈负相关，Cho呈正相关。ChoP对肥胖表现出适度的区分能力，MR表明较高的ChoP水平可能与较低的肥胖风险有关。总之，我们验证了血清Cho和ChoP的UPLC-MS/MS分析，我们的研究结果表明，ChoP和ChoP/Cho比值与肥胖和血糖状态有关。

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引用次数: 0

Assessment of serum concentrations of α-pinene, β-pinene, and limonene in the U.S. population from the 2013–2014 National Health and nutrition examination survey 2013-2014年国家健康与营养调查中美国人群血清α-蒎烯、β-蒎烯和柠檬烯浓度的评估

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-11-30 DOI: 10.1016/j.jchromb.2025.124873

Lalith Silva, Cody Newman, Deepak Bhandari, Wanzhe Zhu, Benjamin Blount

Terpenes are a class of ubiquitous chemicals with many potential health benefits and harms. Human exposure to terpenes can occur through pathways such as cleaning products, fragrances, diet, or drug-use. α-pinene, β-pinene, and limonene are known to be present in trees, citrus fruits, herbs, marijuana, and cigarette smoke. With little known about human exposure to these compounds, it was important to characterize the baseline level of exposure for the general U.S. population. Using results for 2213 samples for participants 6–80 years with surplus serum available from NHANES 2013–2014, obtained with previously published quantitation methods, we compared serum terpene concentrations in demographic groups and identified likely exposure routes. Multiple linear regression found smoking 10–19 cigarettes per day (CPD) was associated with 35.8 % higher serum limonene and smoking >19 CPD was associated with 44.9 % higher serum limonene compared with non-smokers with no secondhand smoke exposure (p = 0.0002). In addition, we found that recent consumption of citrus-rich foods (rates per 1 kg consumed) was associated with significantly higher serum α-pinene (32.8 %, p = 0.0042) and limonene (82.1 % p = 0.0002). Finally, we observed significant associations between serum terpenes and demographic groups. Females had significantly lower serum limonene (p = 0.0243) compared to males. Hispanic and non-Hispanic Asian people had significantly higher serum β-pinene (p < 0.05) and limonene (p < 0.05) compared to non-Hispanic White people. This work characterizes the baseline of terpene exposure in the general U.S. population.

萜烯是一类普遍存在的化学物质，对健康有许多潜在的益处和危害。人类可以通过清洁产品、香水、饮食或吸毒等途径接触到萜烯。α-蒎烯、β-蒎烯和柠檬烯已知存在于树木、柑橘类水果、草药、大麻和香烟烟雾中。由于对人类暴露于这些化合物的情况知之甚少，因此确定美国普通人群暴露的基线水平是很重要的。使用NHANES 2013-2014中6-80岁参与者的2213份样本的结果，通过先前发表的定量方法获得剩余血清，我们比较了人口统计学组的血清萜烯浓度，并确定了可能的暴露途径。多元线性回归发现，与没有二手烟暴露的非吸烟者相比，每天吸烟10-19支（CPD）与血清柠檬烯升高35.8%相关，吸烟bbb19支（CPD）与血清柠檬烯升高44.9%相关（p = 0.0002）。此外，我们发现，最近食用富含柑橘类的食物（每1公斤食用的比例）与血清α-蒎烯（32.8%,p = 0.0042）和柠檬烯（82.1%,p = 0.0002）显著升高相关。最后，我们观察到血清萜烯与人口统计学群体之间的显著关联。女性血清柠檬烯明显低于男性（p = 0.0243）。西班牙裔和非西班牙裔亚洲人血清β-蒎烯显著升高(p

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引用次数: 0

From chemical profiling to bioactivity: Integrating spectrum-effect relationship and activity validation to discover anti-inflammatory markers in Wuwei Qingzhuo Pill 从化学分析到生物活性：整合光谱效应关系和活性验证发现武味清浊丸的抗炎标志物。

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-11-29 DOI: 10.1016/j.jchromb.2025.124876

Tiantian Shi , Wenhua Yang , Lizhu Yin , Xuena Zhang , Yuewu Wang , Liang Bao , Ren Bu , Jingkun Lu , Tuya Bai , Peifeng Xue , Xin Dong

Efficacy-oriented quality control represents a persistent challenge in traditional medicine due to complex multi-component compositions and the inadequacy of single-compound quantification methods. This study establishes an integrated analytical paradigm combining in vivo pharmacological validation with comprehensive chemical profiling, using the traditional Mongolian formulation Wuwei Qingzhuo Pill (WQP) as an investigative model. We initially demonstrated WQP's significant anti-arthritic efficacy in a collagen-induced arthritis (CIA) rat model, observing marked reduction in joint swelling, arthritis scores, and bone destruction. Subsequent chemical characterization established validated HPLC fingerprints across 19 production batches, revealing consistent quality patterns. Through innovative spectrum-effect relationship analysis integrating gray relational analysis (GRA) and orthogonal partial least squares-discriminant analysis (OPLS-DA), we successfully correlated chromatographic features with anti-inflammatory potency, identifying gallic acid, punicalagin, and ellagic acid as critical quality markers. The bioactivity of these markers was further confirmed in lipopolysaccharide (LPS)-stimulated RAW264.7 macrophages, which significantly inhibited TNF-α and IL-1β release. This research presents the first comprehensive application of HPLC fingerprinting combined with spectrum-effect relationship analysis for quality assessment of WQP, offering a robust methodology that transcends traditional quality control approaches. The identified quality markers provide a scientific foundation for efficacy-based quality control and standardization of WQP, with potential implications for quality evaluation of other traditional medicines.

由于复杂的多组分组成和单一化合物定量方法的不足，以疗效为导向的质量控制在传统医学中是一个持续的挑战。本研究以蒙方乌味清浊丸为研究模型，建立了体内药理验证与综合化学分析相结合的综合分析范式。我们最初在胶原诱导关节炎（CIA）大鼠模型中证明了WQP的显著抗关节炎功效，观察到关节肿胀、关节炎评分和骨破坏明显减少。随后的化学表征在19个生产批次中建立了有效的HPLC指纹图谱，揭示了一致的质量模式。通过结合灰色关联分析（GRA）和正交偏最小二乘法判别分析（OPLS-DA）的创新的光谱效应关系分析，我们成功地将色谱特征与抗炎效力关联起来，确定没食子酸、果酸苷和鞣花酸是关键的质量标记。在脂多糖（LPS）刺激的RAW264.7巨噬细胞中进一步证实了这些标记物的生物活性，显著抑制TNF-α和IL-1β的释放。本研究首次将高效液相色谱指纹图谱与光谱效应关系分析相结合，全面应用于WQP的质量评价，提供了一种超越传统质量控制方法的可靠方法。所鉴定的质量标记为WQP基于疗效的质量控制和标准化提供了科学依据，并对其他传统药物的质量评价具有潜在的指导意义。

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引用次数: 0

MOF-199@ tryptophan coated on magnetic bar for stir-bar sorptive extraction of warfarin and aspirin from biological samples followed by quantification through HPLC-UV 磁棒包被MOF-199@色氨酸用于搅拌棒吸附提取生物样品中的华法林和阿司匹林，并通过高效液相色谱-紫外定量。

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-11-29 DOI: 10.1016/j.jchromb.2025.124877

Parastoo Fouladi , Milad Ghani , Jahan Bakhsh Raoof

Tryptophan-functionalized MOF-199 was synthesized via a simple solvothermal method and employed as a novel sorbent for the development of stir-bar sorptive extraction (SBSE) method. The extraction efficiency of the SBSE method was systematically investigated using warfarin and aspirin as model compounds. The extracted drugs were analyzed using high-performance liquid chromatography with ultraviolet detection (HPLC-UV). Key parameters affecting SBSE, including stirring rate, desorption solvent, pH, extraction and desorption time, and salt concentration, were optimized, resulting in 800 rpm stirring rate, 5 min extraction, 1 min desorption, 11 % (w/v) salt concentration, 100.0 μL desorption solvent, and pH = 3.0 as optimal condition. Under the condition, the method exhibited excellent linearity (0.10–200.00 μg L⁻¹ for aspirin and 0.10–100.00 μg L⁻¹ for warfarin), low limits of detection (0.04 and 0.03 μg L⁻¹) and limits of quantification (0.13 and 0.09 μg L⁻¹), and satisfactory precision (%RSD = 4.40–7.60 % for aspirin and 5.10–6.50 % for warfarin). Enrichment factors (EFs) of 56.00 and 64.00 were achieved for aspirin and warfarin, respectively. The proposed SBSE-HPLC-UV method was successfully applied to biological samples, including plasma and urine, demonstrating high reproducibility, efficiency, and suitability for trace-level drug analysis. These results highlight the potential of tryptophan-functionalized MOF-199 as an effective sorbent for analytical applications in pharmaceutical and biological matrices. The method was further evaluated using the Blue Applicability Grade Index (BAGI), achieving a score of 82.5.

采用简单的溶剂热法合成了色氨酸功能化MOF-199，并将其作为一种新型吸附剂用于搅拌棒吸附萃取（SBSE）方法的开发。以华法林和阿司匹林为模型化合物，系统考察了SBSE法的提取效率。采用高效液相色谱-紫外检测（HPLC-UV）对提取的药物进行分析。对影响SBSE的搅拌速率、解吸溶剂、pH、萃取和解吸时间、盐浓度等关键参数进行了优化，结果表明：搅拌速率为800 rpm，萃取时间为5 min，解吸时间为1 min，盐浓度为11% (w/v)，解吸溶剂为100.0 μL, pH = 3.0为最佳条件。在此条件下，该方法具有良好的线性（阿司匹林为0.10 ~ 200.00 μ L-1，华法林为0.10 ~ 100.00 μ L-1）、低检出限（0.04、0.03 μ L-1）和定量限（0.13、0.09 μ L-1），精密度（%RSD = 4.40 ~ 7.60%，华法林为5.10 ~ 6.50%）。阿司匹林和华法林的富集因子（EFs）分别为56.00和64.00。该方法成功地应用于生物样品，包括血浆和尿液，具有高重现性、高效率和痕量药物分析的适用性。这些结果突出了色氨酸功能化MOF-199作为一种有效的吸附剂在药物和生物基质分析中的应用潜力。采用蓝色适用性等级指数（BAGI）对该方法进行进一步评价，得分为82.5分。

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引用次数: 0

Comparative evaluation between Geenius™ dual-path migration immunochromatography platform and Western blot HIV-1 for confirmatory assays in the Brazilian population Geenius™双路迁移免疫层析平台和Western blot HIV-1在巴西人群验证性检测中的比较评价

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-11-29 DOI: 10.1016/j.jchromb.2025.124885

Rubia Heloisa Vanderlinde, Graziele Cristina Ferreira, Jussimara Monteiro Nurmberger, Daniela Calciolari Marques, Flavia Maria Correa Cristaldi, Renata Chiavarini, Debora Ribeiro Ramadan, Sergio Tufik, Carolina Xavier Lima Piccinini, Mariana do Nascimento Viana

Human immunodeficiency virus (HIV) diagnosis requires both screening and confirmatory assays to accurately differentiate antigen and antibody reactivity. The Western blot (WB) method has long been considered the gold standard for confirming HIV infection. However, due to its labor-intensive workflow and technical complexity, the WB has become challenging for many clinical laboratories. Therefore, newer diagnostic techniques, such as the Dual-Path Platform (DPP) lateral flow immunochromatography assays, have been developed and approved by regulatory agencies. Automated interpretation of DPP enhances analytical sensitivity by minimizing subjectivity and allowing detection of faint bands, reducing the probability of false-negative results. This study compared the performance of the WB and DPP as confirmatory methods following chemiluminescent immunoassay (CLIA) screening. All samples were previously screened using CLIA and subsequently analyzed by both WB and DPP assays. Samples yielding borderline CLIA results underwent additional testing by RT-qPCR. The DPP platform demonstrated high concordance with the WB assay, achieving an agreement rate of 97.2 % and a kappa index of 93.9 %, indicating excellent predictive performance. Borderline results were confirmed as reactive by both DPP and RT-qPCR but remained indeterminate by WB. Although complete agreement between both confirmatory methods was not achieved, no clinically significant discrepancies were observed, suggesting that such variations did not impact patient outcomes. Despite the WB remaining as a reference confirmatory method for HIV diagnosis, the DPP method offers substantial advantages, including shorter turnaround time, greater operational simplicity, and automated digital documentation, making it a practical alternative for routine use in high-throughput or resource-limited laboratory settings.

人类免疫缺陷病毒（HIV）的诊断需要筛查和确认试验来准确区分抗原和抗体的反应性。长期以来，Western blot （WB）方法一直被认为是确认HIV感染的金标准。然而，由于其劳动密集型工作流程和技术复杂性，WB已成为许多临床实验室的挑战。因此，新的诊断技术，如双路径平台（DPP）横向流动免疫层析分析，已经开发并得到监管机构的批准。DPP的自动解释通过最大限度地减少主观性和允许检测微弱波段来提高分析灵敏度，减少假阴性结果的可能性。本研究比较了WB和DPP作为化学发光免疫测定（CLIA）筛选后的验证性方法的性能。所有样品先前使用CLIA筛选，随后使用WB和DPP分析。获得CLIA临界结果的样品通过RT-qPCR进行了额外的检测。DPP平台与WB法具有较高的一致性，一致性率为97.2%，kappa指数为93.9%，具有良好的预测性能。DPP和RT-qPCR均证实边缘性结果具有反应性，但WB仍不确定。虽然两种验证性方法之间没有完全一致，但没有观察到临床上显著的差异，这表明这些差异不会影响患者的预后。尽管WB仍然是HIV诊断的参考验证方法，但DPP方法具有实质性优势，包括周转时间更短，操作更简单，自动化数字文档，使其成为高通量或资源有限的实验室环境中常规使用的实用替代方案。

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引用次数: 0

Rapid biocompatible solid phase microextraction: Nirogacestat protein binding in post dose human serum samples 快速生物相容性固相微萃取：硝加司他蛋白在给药后人血清样品中的结合。

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-11-29 DOI: 10.1016/j.jchromb.2025.124874

Helen Patten , Rochelle Burke , Sohrab Habibi Goudarzi , Cassie Manning , Rex L. Williams Jr , Todd Baughman

Protein binding can influence the ability of a drug to permeate biologic membranes and can therefore be a limiting factor in the passage of drugs across a membrane. Most drugs must be unbound (free) to have a pharmacological effect. To quantitate free active drug in blood plasma, protein binding is typically assessed based on permeation techniques using devices such as a rapid equilibrium dialysis (RED) device. Caveats to this approach include the time to equilibration, which can introduce drug instability, and/or non-specific binding that confound accurate estimation of protein binding. Initial experiments with a RED device showed nirogacestat in clinical samples had non-specific binding in the buffer chamber which resulted in a low percent bound of 24.1 %. Clearly a different approach is needed to accurately characterize the protein binding of nirogacestat in clinical samples. For this reason, adsorption-based technologies, such as biocompatible solid phase microextraction (BioSPME), provide a potentially suitable alternative to permeation-based protein binding for highly bound drugs like nirogacestat.

BioSPME was used to measure protein binding for nirogacestat for both in vitro and clinical samples. A biocompatible sorbent material selectively extracts unbound analytes from a sample matrix as sample passes through the BioSPME cartridge, where the analyte is adsorbed onto the solid phase while the sample's base liquid passes through then eluted with a solvent. This approach allows for control of equilibration/incubation times and container types. The results show that BioSPME provides an accurate and reliable method for measuring protein binding in both in vitro and clinical samples.

Significance statement

BioSPME accurately measures the protein binding of nirogacestat in clinical serum samples and is an alternative to RED for measuring protein binding in vitro and in clinical samples.

蛋白质结合可以影响药物通过生物膜的能力，因此可以成为药物通过膜的限制因素。大多数药物必须是游离的才能产生药理作用。为了定量测定血浆中的游离活性药物，通常使用快速平衡透析（RED）装置等渗透技术来评估蛋白质结合。该方法的注意事项包括平衡时间，这可能会引入药物不稳定性和/或非特异性结合，从而混淆蛋白质结合的准确估计。用RED装置进行的初步实验表明，临床样品中的硝格司他在缓冲腔中具有非特异性结合，其结合率较低，为24.1%。显然，需要一种不同的方法来准确表征临床样品中硝格司他的蛋白质结合。出于这个原因，基于吸附的技术，如生物相容性固相微萃取（BioSPME），为像硝格司他这样的高结合药物提供了一种潜在的替代基于渗透的蛋白质结合的合适选择。BioSPME用于测定体外和临床样品中氮醋司他的蛋白结合。当样品通过BioSPME药筒时，生物相容性吸附剂材料选择性地从样品基质中提取未结合的分析物，其中分析物被吸附到固相上，而样品的基础液体通过，然后用溶剂洗脱。这种方法允许控制平衡/孵育时间和容器类型。结果表明，BioSPME在体外和临床样品中都提供了一种准确可靠的蛋白质结合测定方法。意义声明：BioSPME可准确测量临床血清样品中硝格司他的蛋白结合，是在体外和临床样品中测量蛋白结合的替代方法。

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引用次数: 0

Pesticide residues in aquaculture salmon filet and feed: Quantitative and qualitative screening profiles of legacy and current-use pesticides using GC-EI-MS/MS and LC-ESI-IMS-QToF 水产养殖鲑鱼鱼片和饲料中的农药残留：使用GC-EI-MS/MS和LC-ESI-IMS-QToF对遗留和当前使用的农药进行定量和定性筛选。

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.2025.124864

Carey E. Donald, Annette Bernhard, Marianne F. Hauglid , Annie Fürstenberg, Marc H.G. Berntssen, Anne-Katrine Lundebye, Veronika Sele

In recent decades, the ingredients used in aquaculture feeds have changed from marine-based to more plant-based. As a result, the content of legacy, organochlorine pesticides has decreased, but the potential increase of current use, land-based pesticides has not been documented. In this work, two analytical techniques were developed and applied to characterize the pesticide profile in current Norwegian salmon aquaculture after the shift to more plant-based feed ingredients. Samples of salmon filet, feed, and feed ingredients were analyzed using two different chromatographic methods, a quantitative gas-chromatography-triple quadrupole mass spectrometry method (43 analytes) and a broader, presence/absence screen using liquid chromatography-high resolution mass spectrometry (215 analytes). Among all samples and between both methods, a total of 43 different pesticide analytes were identified. Results show that the major pesticides present in the filet of farm-raised salmon are the legacy, organochlorine pesticides as contaminants. Conversely the feed is dominated by current-use, organophosphate and pyrethroid pesticides. There were no exceedances of the few established maximum residue limits for contaminants in fish and feed. No pesticides in salmon filet exceeded the default limit of 10 μg/kg, while there were several observations in feed above this level. These results suggest low risk in terms of food safety, however, issues related to animal health cannot be ruled out. The two chromatography methods are compared, and they complement each other by giving an overview of pesticides with both breadth and depth.

近几十年来，水产养殖饲料中使用的成分已经从以海洋为基础转变为以植物为基础。因此，遗留有机氯农药的含量有所下降，但目前使用的陆基农药的潜在增加尚未得到记录。在这项工作中，开发了两种分析技术，并应用于在转向更多植物性饲料成分后，目前挪威鲑鱼水产养殖中的农药特征。使用两种不同的色谱方法分析鲑鱼片、饲料和饲料成分样品，一种是定量气相色谱-三重四极杆质谱法（43种分析物），另一种是更广泛的存在/不存在屏幕，使用液相色谱-高分辨率质谱法（215种分析物）。在所有样品中以及两种方法之间，共鉴定出43种不同的农药分析物。结果表明，养殖鲑鱼鱼片中的主要农药是遗留的有机氯农药。相反，饲料主要是目前使用的有机磷和拟除虫菊酯农药。鱼类和饲料中没有超过规定的几项污染物最大残留限量。鲑鱼鱼片中农药残留量未超过10 μg/kg的默认限值，饲料中农药残留量超过10 μg/kg的情况较多。这些结果表明，就食品安全而言，风险较低，但不能排除与动物健康有关的问题。这两种色谱方法进行了比较，它们通过对农药的广度和深度进行概述来相互补充。

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引用次数: 0

Per- and polyfluoroalkyl substances (PFAS) in marine sediments from a Norwegian fjord near an airport: Historical records, distribution, and controlling factors 机场附近挪威峡湾海洋沉积物中的全氟和多氟烷基物质（PFAS）：历史记录、分布和控制因素

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.2025.124868

Stepan Boitsov, Jon Albretsen, Hilde Elise Heldal, Stig Valdersnes, Bjørn Einar Grøsvik, Bashir Abdulkader, Aasim Ali

Airports have been identified as one of numerous sources of extremely persistent, toxic and bioaccumulative per- and polyfluoroalkyl substances (PFAS), as part of aqueous film-forming foams (AFFF) during fire drills. The historically strongly contaminated terrestrial environment around Flesland airport in Bergen, Norway, raised concern for potential contamination in the surrounding fjords. To investigate this, surface sediments and sediment cores were collected from several locations adjacent to the airport area. One of the cores was dated by ²¹⁰Pb. Two analytical methods, a target method for 24 specific PFAS compounds in marine sediments, and a total oxidizable precursor (TOP) assay method, were established, validated and applied to the samples. The results were combined with previously collected data on surface sediments from fjords and open sea areas in Western Norway. While TOP assay results for sediments and pore water indicated a significant PFAS precursor load at locations close to the airport, and sediment cores showed a continuous increase in PFAS levels (since at least 1980s in the dated core), relatively low levels of PFAS were found in marine sediments off the airport area (1.1 μg/kg dry weight or less for the sum of nine most abundant PFAS in surface sediments). The results agree with earlier data on PFAS background levels in marine sediments from unaffected areas and imply a dispersion of the contamination from the airport elsewhere. Sea current modeling and grain size determination suggest local hydrodynamical and sedimentological conditions as the main factors of influence for the contamination status in the area.

机场已被确定为消防演习期间作为水成膜泡沫（AFFF）的一部分的极持久、有毒和生物蓄积性全氟烷基和多氟烷基物质（PFAS）的众多来源之一。挪威卑尔根的弗莱斯兰机场周围的陆地环境历来受到严重污染，这引起了人们对周围峡湾潜在污染的关注。为了调查这一点，从机场附近的几个地点收集了地表沉积物和沉积物岩心。其中一个岩心的年代为210Pb。建立了海洋沉积物中24种特定PFAS化合物的靶法和总氧化前体（TOP）法两种分析方法，并对其进行了验证和应用。研究结果与之前收集的挪威西部峡湾和公海表面沉积物数据相结合。虽然沉积物和孔隙水的TOP分析结果表明，靠近机场的位置有显著的PFAS前体负荷，沉积物岩心显示PFAS水平持续增加（至少从20世纪80年代开始），但在机场区域附近的海洋沉积物中发现的PFAS水平相对较低（地表沉积物中9种最丰富的PFAS的总和为1.1 μg/kg干重或更低）。这一结果与早期关于未受影响地区海洋沉积物中PFAS背景水平的数据一致，表明污染从其他地方的机场扩散开来。海流模拟和粒度测定表明，当地的水动力和沉积条件是影响该地区污染状况的主要因素。

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引用次数: 0