Journal of Chromatography A最新文献_第7页

Post-synthetic click chemistry-mediated surface engineering of fluorinated COFs for ultrahigh PFASs uptake 合成后点击化学介导的氟化COFs表面工程用于超高全氟烷烃吸收。

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2026-01-06 DOI: 10.1016/j.chroma.2026.466680

Chenchen Lin , Yan Wu , Tuo Zhen , Jinxin Chi , Xucong Lin

Fluorinated covalent organic frameworks (F-COFs) have attracted widespread attention, owing to their capacity to enhance the adsorption of per- and polyfluoroalkyl substances (PFASs) through F-F affinity and the intrinsic adsorption properties of COFs. F-COFs were usually synthesized based on “de novo synthesis” with commercial fluorinated monomers. However, challenges still remain due to the limited availability of fluorinated monomers, harsh control of crystal growth, and difficult adjustment of surface fluorination. Post-synthetic surface engineering offers great potential for flexibly fabricating F-COFs with tailored functions by modifying functional moieties into the predefined frameworks. Herein, a post-synthetic strategy was pioneered for the fabrication of novel F-COFs with tunable fluorination degrees (noted as COF-V-x-F, x=0-1.0). The approach integrates two synergistic processes: aniline-modulated room-temperature synthesis of the COF-V precursor, and the flexible surface engineering on COF-V via click chemistry to realize controllable fluorination. Using this method, the optimal COF-V-0.33-F was achieved, which contains sufficient fluorinated groups for F-F affinity, high hydrophobicity, and strong molecular adsorption, thus enabling ultra-high PFAS uptake by solid-phase microextraction (SPME). A highly sensitive detection was achieved with limits of detection at 0.2–1.4 ng·L⁻¹ using COF-V-0.33-F fiber coupled with LC-MS/MS. Compared to the commercial PDMS, COF-V and amorphous COP-V-0.33-F, the designed COF-V-0.33-F fiber exhibited rather high extraction capacity with 2.7-65.8, 2.1-10.8, and 2.8-367.1 fold enhancement, respectively. The proposed method was successfully used for PFASs determination in tap, pond and river water. Seven trace PFASs were detected with satisfactory recoveries of 71.0%-117.9%, 75.7%-109.1% and 82.8%-118.2% at spiked concentrations of 20 ng/L, 200 ng/L and 2000 ng/L, respectively. This work posed a simple but powerful access to efficient synthesis of F-COFs with good crystallinity and flexible adjustment of fluorination.

氟化共价有机骨架（F-COFs）由于其对全氟烷基和多氟烷基物质的亲和作用以及其固有的吸附特性而引起了广泛的关注。氟氯化碳通常是用商用氟化单体“从头合成”的方法合成的。然而，由于氟化单体的可用性有限，晶体生长的严格控制以及表面氟化的难以调整，挑战仍然存在。后合成表面工程为灵活地制造具有定制功能的F-COFs提供了巨大的潜力，通过将功能部分修改为预定义的框架。本文提出了一种后合成策略，用于制造具有可调氟化度（称为COF-V-x-F， x=0-1.0）的新型F-COFs。该方法集成了苯胺调制的COF-V前驱体的室温合成和通过点击化学对COF-V进行柔性表面工程以实现可控氟化两个协同过程。利用该方法，获得了最佳的COF-V-0.33-F，该COF-V-0.33-F含有足够的F-F亲和氟基团，具有高疏水性和强分子吸附能力，从而实现了固相微萃取（SPME）对PFAS的超高吸收率。一个高度敏感的检测是通过检测的局限性在0.2 - -1.4 ng·L⁻¹使用咖啡- v - 0.33 f加上纤维质/女士。与商用PDMS、COF-V和非晶COP-V-0.33-F相比，设计的COF-V-0.33- f光纤的萃取能力分别提高了2.7 ~ 65.8倍、2.1 ~ 10.8倍和2.8 ~ 367.1倍。该方法成功地用于自来水、池塘和河流中PFASs的测定。在加标浓度为20 ng/L、200 ng/L和2000 ng/L时，共检出7种痕量PFASs，加标回收率分别为71.0% ~ 117.9%、75.7% ~ 109.1%和82.8% ~ 118.2%。本工作为高效合成结晶度好、氟化调节灵活的氟- cofs提供了一条简单而有力的途径。

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引用次数: 0

Polyimide nanosheets based magnetic solid-phase extraction for the extraction of parabens from cosmetic samples followed by gas chromatography–mass spectrometry 基于聚酰亚胺纳米片的磁固相萃取-气相色谱-质谱法从化妆品样品中提取对羟基苯甲酸酯。

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2026-01-06 DOI: 10.1016/j.chroma.2026.466682

Yue Li , Xianzhong Chen , Xiaohui Yan , Liuxin Wang , Dapeng Wu , Dechen Jiang

This study introduces a novel magnetic composite based on polyimide nanosheets (Fe₃O₄@PINSs), designed for the highly efficient extraction of parabens from cosmetics. The composite was fabricated by combining Fe₃O₄ nanoparticles with polyimide nanosheets, yielding a material with excellent magnetic responsiveness (21.3 emu/g) and a high surface area (141 m²/g), both of which enhance separation and adsorption performance. The Fe₃O₄@PINSs composite was employed as the adsorbent in a magnetic solid-phase extraction (MSPE) protocol targeting six prevalent parabens in cosmetics, followed by gas chromatography–mass spectrometry (GC–MS) detection. A comprehensive study was carried out to optimize critical extraction and desorption parameters, including adsorbent dosage, extraction time, ionic strength, pH, desorption solvent selection, solvent volume, and desorption time. Under the optimized conditions, the Fe₃O₄@PINSs-based MSPE/GC–MS method exhibited a wide linear range (0.1–100 μg/L or 0.2–100 μg/L), high sensitivity (limits of detection of 0.037–0.077 μg/L), and good reproducibility (relative standard deviations ≤ 9.6%, n = 3). The calculated enrichment factors were between 15 and 19. When applied to real cosmetic samples—including hand creams, facial cleansers, and moisturizing lotions—the method provided reliable results, with recoveries ranging from 82.8% to 114.7%. Compared with previously reported methods, the proposed method shows comparable or better performance, with the notable advantage of a short extraction time (5 min). These findings suggest that the Fe₃O₄@PINSs composite has great potential as an adsorbent material in MSPE. The developed method is suitable for routine monitoring of parabens in cosmetic products, offering advantages of simplicity, rapidity, high sensitivity, accuracy, and precision.

本研究介绍了一种基于聚酰亚胺纳米片的新型磁性复合材料（Fe3O4@PINSs），用于从化妆品中高效提取对羟基苯甲酸酯。通过将Fe3O4纳米颗粒与聚酰亚胺纳米片结合，制备出具有优异磁响应性（21.3 emu/g）和高表面积（141 m2/g）的复合材料，增强了分离和吸附性能。以Fe3O4@PINSs复合材料为吸附剂，对化妆品中常见的6种对羟基苯甲酸酯进行了磁固相萃取（MSPE），并进行了气相色谱-质谱（GC-MS）检测。对吸附剂用量、萃取时间、离子强度、pH、解吸溶剂选择、溶剂体积和解吸时间等关键萃取和解吸参数进行了优化研究。在优化条件下，Fe3O4@PINSs-based MSPE/GC-MS方法线性范围宽（0.1 ~ 100 μg/L或0.2 ~ 100 μg/L），灵敏度高（检出限为0.037 ~ 0.077 μg/L），重现性好（相对标准偏差≤9.6%,n = 3）。计算的富集因子在15 ~ 19之间。当应用于真正的化妆品样品时，包括护手霜、洗面奶和保湿乳液，该方法提供了可靠的结果，回收率在82.8%到114.7%之间。与已有报道的方法相比，该方法具有相当或更好的性能，其显著优势是提取时间短（5 min）。这些结果表明Fe3O4@PINSs复合材料作为MSPE的吸附剂具有很大的潜力。该方法简便、快速、灵敏、准确、精密度高，适用于化妆品中对羟基苯甲酸酯类物质的常规监测。

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引用次数: 0

Nontarget screening and suspect identification of organic chlorinated compounds in cosmetics and personal care products using UHPLC-Q-Orbitrap-HRMS UHPLC-Q-Orbitrap-HRMS对化妆品和个人护理产品中有机氯化合物的非靶筛选和可疑鉴定

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2026-01-06 DOI: 10.1016/j.chroma.2026.466681

Tao Yang , Xinling Li , Jianhua Tan , Wenyao Liang , Xianzhi Peng

Organic chlorinated compounds have been extensively incorporated into cosmetics and personal care products (CPCPs) as germicides, surfactants, and oil-controlling agents, leading to potential human exposure and associated health risks. However, available research has mostly been limited to several chlorinated compounds in CPCPs, e.g., triclosan and triclocarban. In this study, an integrated analytical framework was established combining isotope-pattern–based nontarget screening with database-assisted suspect identification to comprehensively characterize organic chlorinated compounds in CPCPs. The framework was successfully validated by screening and identification of chlorinated compounds in children’s skincare products for sale in China. A total of 227 chlorinated compounds were tentatively identified, including 3 confidence level (CL)1, 9 CL2, 93 CL3, and 122 CL4 compounds with RDBE values of 0 - 29 and molecular masses of 128 - 931 Da. Heterocyclics and ethers were predominant among the CL1–CL3 compounds. Chlorhexidine was quantified maximally at 0.456 %. Triclosan, elubiol, and 4-chloroaniline were also detected in at least one product although they have been banned in skincare products. Overall, the results demonstrated robustness of the comprehensive analytical framework in identifying and characterizing chlorinated compounds in CPCPs. In addition, this research shed light on potential exposure of young children to a cocktail of chlorinated compounds, underscoring urgent need for strict regulations of chemical addition and transparent ingredient labeling to ensure safe use of CPCPs.

有机氯化合物作为杀菌剂、表面活性剂和控油剂被广泛地添加到化妆品和个人护理产品中，导致潜在的人类接触和相关的健康风险。然而，现有的研究大多局限于cpcp中的几种氯化化合物，例如三氯生和三氯卡班。本研究建立了基于同位素模式的非靶点筛选与数据库辅助可疑鉴定相结合的综合分析框架，以全面表征CPCPs中的有机氯化化合物。通过对在中国销售的儿童护肤品中含氯化合物的筛选和鉴定，成功验证了该框架。初步鉴定出227个氯化化合物，包括3个置信水平（CL）1, 9个CL2, 93个CL3和122个CL4化合物，RDBE值为0 ~ 29，分子质量为128 ~ 931 Da。杂环化合物和醚类化合物在CL1-CL3化合物中占主导地位。氯己定含量最高，为0.456 %。三氯生、elubiol和4-氯苯胺也在至少一种产品中被检测出，尽管它们已被禁止在护肤品中使用。总体而言，结果证明了综合分析框架在cpcp中鉴定和表征氯化化合物方面的稳健性。此外，这项研究揭示了幼儿可能暴露于氯化化合物混合物的情况，强调迫切需要严格的化学添加法规和透明的成分标签，以确保cpcp的安全使用。

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引用次数: 0

Enhanced metabolite profiling of herbal products using an integrated 4-in-1 analysis system and the MetaboTarget algorithm 使用集成的4合1分析系统和MetaboTarget算法增强草药产品的代谢物分析。

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2026-01-05 DOI: 10.1016/j.chroma.2026.466671

Mengyuan Wang, Yunuo Fan, Ye Zhang, Ling Chen, Bin Li, Ping Li

The inherent chemodiversity and complexity of herbal products make their quality control extremely challenging. In this work, a comprehensive analysis strategy through combining a polarity-extended liquid chromatography-mass spectrometry system (4-in-1 analysis system) and a metabolite-oriented targeted screening algorithm (MetaboTarget) for herbal products was proposed. The 4-in-1 analytical technique significantly expanded detection coverage of analytes through polarity extension. The Python-based MetaboTarget algorithm constructs a predictive database of potential metabolites by integrating Phase I/II metabolic reaction rules with parent drug components absorbed into the blood. Using precursor ions for targeted DDA scanning of plasma samples enables comprehensive metabolite characterization through integration with feature-based molecular networking (FBMN). The developed strategy was successfully applied to the deep in vitro and in vivo analysis of chemical components of Gegen Qinlian Decoction (GQD). As a result, 303 components in GQD and 181 metabolites in plasma were annotated. This integrated strategy enables simultaneous detection of compounds across the full polarity spectrum (high/medium/low) while overcoming key challenges in metabolite identification through the MetaboTarget algorithm, which effectively addresses issues arising from strong endogenous interference and low target abundance, thereby providing a powerful tool for comprehensive characterization of complex herbal products.

草药产品固有的化学多样性和复杂性使其质量控制极具挑战性。本文提出了一种结合极性扩展液相色谱-质谱分析系统（4合1分析系统）和代谢物定向筛选算法（MetaboTarget）的草药产品综合分析策略。4合1分析技术通过极性扩展显着扩大了分析物的检测范围。基于python的MetaboTarget算法通过整合I/II期代谢反应规律和母体药物成分被血液吸收，构建了潜在代谢物的预测数据库。利用前体离子对血浆样品进行靶向DDA扫描，通过与基于特征的分子网络（FBMN）相结合，可以实现全面的代谢物表征。该方法成功地应用于葛根芩连汤的体内外深层化学成分分析。结果，GQD中的303个组分和血浆中的181个代谢物被注释。这种集成策略能够同时检测全极性谱（高/中/低）的化合物，同时通过MetaboTarget算法克服代谢物鉴定的关键挑战，有效地解决了强内源干扰和低目标丰度带来的问题，从而为复杂草药产品的综合表征提供了强大的工具。

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引用次数: 0

Development of a chiral mass spectrometry derivatization reagent for amino acid enantiomer analysis: Metabolic investigation of DL-amino acids in the serum of nephritis patients 一种用于氨基酸对映体分析的手性质谱衍生试剂的研制：肾炎患者血清中dl -氨基酸的代谢研究。

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2026-01-05 DOI: 10.1016/j.chroma.2026.466677

Xinxin Kong , Zongshuo Sun , Xinyi Xu, Xi-Ling Li, Jin Ji Li, Jun Zhe Min

A chiral mass spectrometry derivatization reagent, (R)/(S)-(5-(2-(((1-(p-toluenesulfonylmethylamino)vinyl)oxy)carbonyl)pyrrolidin-1-yl)-5-oxopentyl) triphenylphosphonium bromide (TPP-(R)/(S)-BSA), was developed in this study. The derivatization reagent carries a permanent positive charge and incorporates an α-acyloxy acetylenamide moiety, enabling highly sensitive detection and stereochemical resolution of amino-containing enantiomers. Exposure of DL-amino acids to TPP-(R)/(S)-BSA under heating at 70 °C for 60 min resulted in formation of the corresponding diastereomers. Fine-tuning of the separation conditions enabled clear resolution of fifteen enantiomeric amino acid pairs on a BEH C18 column, with Rs values spanning 1.02–14.49. Except for Pro, Gln, and His, all DL-amino acid pairs showed Rs values above 1.5, indicating effective enantiomeric separation under standardized conditions. Based on the TPP-(S)-BSA derivatization strategy, we developed a UHPLCHRMS assay with excellent sensitivity and selectivity, enabling concurrent resolution and determination of 13 DL-amino acid enantiomeric pairs together with glycine in human serum. The method provided excellent linearity within 0.05–1000 μM (R² ≥ 0.9914), with limits of detection (LOD) between 0.2 and 4.5 fmol. For both intra-day and inter-day evaluations, the observed precision fell within the range of 0.92%–14.00%, while recovery rates averaged 97.88%–111.78%, and matrix effects were within 3.82%–14.58%. Furthermore, statistical analysis of DL-amino acid metabolic concentrations in serum from healthy volunteers and nephritis patients enabled the construction of a diagnostic model integrating differentially expressed enantiomers, providing a potential screening tool for nephritis.

本研究开发了一种手性质谱衍生试剂(R)/(S)-（5-（2-（（1-（对甲苯磺基甲基胺）乙烯基）氧羰基）吡咯烷-1-基）-5-氧戊基）三苯基溴化磷(TPP-(R)/(S)- bsa)。衍生化试剂带有永久正电荷，并包含α-酰基乙酰胺部分，可对含氨基对映体进行高灵敏度检测和立体化学分辨。dl -氨基酸与TPP-(R)/(S)- bsa在70℃下加热60 min，形成相应的非对映体。通过对分离条件的微调，在BEH C18色谱柱上可以清晰地分离出15对对映体氨基酸对，Rs值在1.02 ~ 14.49之间。除Pro、Gln和His外，所有dl -氨基酸对的Rs值均大于1.5，表明在标准化条件下对映体分离有效。基于TPP-(S)- bsa衍生化策略，我们开发了一种具有良好灵敏度和选择性的UHPLCHRMS方法，可以同时解析和测定人血清中与甘氨酸一起存在的13对dl氨基酸对映体。在0.05 ~ 1000 μM （R²≥0.9914）范围内具有良好的线性关系，检出限（LOD）在0.2 ~ 4.5 fmol之间。日内、日间评价的精密度在0.92% ~ 14.00%之间，平均回收率在97.88% ~ 111.78%之间，基质效应在3.82% ~ 14.58%之间。此外，通过对健康志愿者和肾炎患者血清中dl -氨基酸代谢浓度的统计分析，构建了整合差异表达对映体的诊断模型，为肾炎的筛查提供了一种潜在的工具。

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引用次数: 0

Determination of nucleosides in serum by two-dimensional magnetic solid-phase extraction microfluidic chip/liquid chromatography-mass spectrometry 二维磁固相萃取微流控芯片/液相色谱-质谱法测定血清中核苷类。

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2026-01-05 DOI: 10.1016/j.chroma.2026.466678

Yongzhe Cheng , Yangkun Sun , Ningning Wang , Qiangqiang Jia , Linghao Zhao , Zeyu Wu , Yuerong Wang , Hongyang Zhang , Min Zhang , Ping Hu

A two-dimensional magnetic solid-phase extraction microfluidic chip (2D-MSPE-chip) was designed in this paper. A microcolumn array was integrated before two serially connected extraction chambers to filter particles in the sample. The two magnetic nanomaterials with orthogonal separation mechanism of Fe₃O₄@UiO-66-C18 and Fe₃O₄@MOF@COF-B(OH)₂ were filled into the extraction chamber, respectively, and were used to effectively eliminate matrix effects and enrich the targets. The 2D-MSPE-chip was combined with liquid chromatography-mass spectrometry (LC-MS) for the determination of eight nucleosides in serum samples. The validation results showed that the 2D-MSPE-chip/LC-MS method had excellent linear range (2–1000 ng/mL), high sensitivity (detection limit of 0.02–0.22 ng/mL), good repeatability (intra-day precision ≤5.2%, inter-day precision ≤7.2%) and a negligible absolute matrix effect (93.1%-101.9%). The recovery rate of the spiked serum samples of prostate cancer patients and healthy person was 90.8%-109.1%, indicating a high accuracy. The inosine level decreased and adenosine level increased in the serum of prostate cancer patients (p < 0.01), suggesting the correlation between nucleosides and the cancer.

设计了一种二维磁固相萃取微流控芯片（2d - mspe芯片）。微柱阵列集成在两个串联的萃取室之前，以过滤样品中的颗粒。将两种具有Fe3O4@UiO-66-C18和Fe3O4@MOF@COF-B(OH)2正交分离机制的磁性纳米材料分别填充到萃取室中，用于有效消除基体效应和富集靶材。将2d - mspe芯片与液相色谱-质谱（LC-MS）联用，用于血清样品中8种核苷的测定。验证结果表明，2D-MSPE-chip/LC-MS方法线性范围好（2 ~ 1000 ng/mL），灵敏度高（检出限0.02 ~ 0.22 ng/mL），重复性好（日内精密度≤5.2%，日内精密度≤7.2%），绝对基质效应可忽略（93.1% ~ 101.9%）。前列腺癌患者和健康人加标血清样品的加标回收率为90.8% ~ 109.1%，准确度较高。前列腺癌患者血清肌苷水平降低，腺苷水平升高（p < 0.01），提示核苷类与前列腺癌有相关性。

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引用次数: 0

A green and practical strategy for therapeutic drug monitoring of teicoplanin A2 components in human plasma using functionalized liquid film solvent bar microextraction coupled with high-performance liquid chromatography–ultraviolet detection 功能化液膜溶剂棒微萃取-高效液相色谱-紫外检测技术用于人血浆中替柯planin A2成分的绿色实用监测策略

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2026-01-03 DOI: 10.1016/j.chroma.2026.466673

Jie Tian , Yi-fang Zhang , Yu-feng Sun , Dou Yan , Shuang Hu , Rong-rong Xing , Run-qin Wang , Li Yang , Xuan Chen

A novel functionalized liquid film solvent bar microextraction (FLF-SBME) method coupled with high-performance liquid chromatography–ultraviolet detection (HPLC/UV) was developed for the extraction and subsequent determination of five A₂-components of teicoplanin, TA_2-1, TA_2-2, TA_2-3, TA_2-4 and TA_2-5, simultaneously in human plasma. The microextraction mechanism of FLF-SBME was systematically elucidated, in which tri-n-octyl methyl ammonium chloride (TOMAC) was employed to modify polypropylene hollow fibers (PP-HFs), enabling efficient enrichment and separation of the target analytes from plasma. The key extraction parameters influencing efficiency were thoroughly optimized. Under optimal conditions, the method provided high enrichment factors (36–59) for all five A₂ components, along with good linearity (1.0–110 µg/mL; r > 0.99), limits of detection of 0.5–3.0 µg/mL, and lower limits of quantification of 1.0–5.0 µg/mL. The intra- and inter-day precision (RSD < 12.2 %) and accuracy (recoveries: 91.5–110.3 %) were satisfactory. With its notable enrichment capability, high selectivity, sensitivity, and reliability, the proposed FLF-SBME–HPLC/UV method is well-suited for the monitoring of teicoplanin in human plasma.

建立了一种新型功能化液膜溶剂棒微萃取(FLF-SBME) -高效液相色谱-紫外检测（HPLC/UV）联用方法，用于同时提取并测定人血浆中替可planin中TA2-1、TA2-2、TA2-3、TA2-4和TA2-5种a2组分。系统阐述了FLF-SBME的微萃取机理，利用三正辛基甲基氯化铵（TOMAC）修饰聚丙烯中空纤维（PP-HFs），实现了血浆中目标分析物的高效富集和分离。对影响提取效率的关键参数进行了优化。在最佳条件下，该方法对5种A2组分均具有较高的富集因子（36 ~ 59），线性度（1.0 ~ 110µg/mL; r ~ 0.99），检出限为0.5 ~ 3.0µg/mL，定量下限为1.0 ~ 5.0µg/mL。日内、日间精密度（RSD < 12.2%）和准确度（回收率：91.5 ~ 110.3%）令人满意。该方法具有显著的富集能力、高选择性、高灵敏度和高可靠性，适用于人血浆中替可planin的检测。

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引用次数: 0

Ultrasensitive detection of triazine herbicides in food via dispersive solid-phase extraction with nanoconfined task-specific ionic liquids in tunable hollow porous carbon spheres 在可调中空多孔碳球中，纳米限定任务特异性离子液体分散固相萃取超灵敏检测食品中三嗪类除草剂。

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2026-01-03 DOI: 10.1016/j.chroma.2026.466672

Xu Xu, Yuanjun Liao, Yuhan Guo, Yi Jiang, Lei Zhang

Triazine herbicides are widely detected in food and pose significant hazards to ecosystems and human health. In this study, a nanoconfined composite of task-specific ionic liquids (TSILs) within hollow porous carbon spheres (HPCS), denoted TSILs@HPCS, was synthesized via post-impregnation for selective enrichment and efficient extraction of triazine herbicides. Hydrophobic TSILs incorporating [NTf₂^-] anion were systematically prepared. Confinement within HPCS tunable pores yielded a 6.0-fold increase in triazine herbicide adsorption capacity relative to pristine HPCS. The TSILs@HPCS composite serves as a multifunctional adsorbent, enabling the simultaneous sorptive removal, highly sensitive detection, and sieving of analytes. A dispersive solid-phase extraction method coupled with high-performance liquid chromatography was developed to quantify trace triazine herbicides in complex food matrices. This approach demonstrated low detection limits (0.06–0.12 μg kg^-1) and high enrichment factors (124–192), confirming its suitability for residue analysis. These results establish TSILs@HPCS as a promising adsorbent for preconcentrating triazine herbicides in food samples.

三嗪类除草剂广泛存在于食品中，对生态系统和人类健康造成重大危害。在本研究中，通过后浸渍法制备了一种中空多孔碳球（HPCS）内的任务特异性离子液体（TSILs）纳米复合材料（表征为TSILs@HPCS），用于选择性富集和高效提取三嗪类除草剂。系统制备了含[NTf2-]阴离子的疏水TSILs。封闭在HPCS可调孔内的三嗪类除草剂的吸附量比原始HPCS增加了6.0倍。TSILs@HPCS复合材料作为多功能吸附剂，可同时进行吸附去除、高灵敏度检测和分析物筛分。建立了分散固相萃取-高效液相色谱法定量测定复杂食品基质中痕量三嗪类除草剂的方法。该方法检出限低（0.06 ~ 0.12 μ kg-1），富集系数高（124 ~ 192），适用于残留分析。这些结果表明TSILs@HPCS是一种很有前途的吸附剂，用于预先浓缩食品样品中的三嗪类除草剂。

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引用次数: 0

Structure-guided design of a minimal epitope tag and nanobody affinity system 最小表位标签和纳米体亲和系统的结构导向设计。

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2026-01-03 DOI: 10.1016/j.chroma.2026.466675

Jiayi Tan , Limin Zhao , Mu Li , Kanglong Yang , Yue Li , Yuqing Ding , Heng Liu , Houjun Xia , Chongyuan Wang , Jiawei Li

The isolation of recombinant proteins commonly relies on affinity-based methods. Nevertheless, widely used tags and solid supports are frequently constrained by insufficient specificity, harsh elution requirements, and cost inefficiency. Here, we developed a robust purification system based on a nanobody that specifically recognizes a short peptide epitope. The nanobody is produced at high yield in a prokaryotic expression system, and the corresponding peptide tag, comprising only 6–7 amino acids, can be fused to either the N- or C-terminus of target proteins. We demonstrate that this system enables one-step purification of diverse soluble and membrane proteins from cell lysates, with high purity and yield. Bound proteins are gently eluted under non-denaturing conditions using a competitive synthetic peptide, achieving a recovery yield of over 90%. Furthermore, the nanobody-conjugated resin maintains consistent binding capacity over at least 10 reuse cycles. Given its high specificity, mild elution, reusability, and simplicity, we propose this system as a versatile and efficient platform for high-quality protein purification, with broad applicability in proteomics, structural biology, and biotherapeutic development.

重组蛋白的分离通常依赖于基于亲和力的方法。然而，广泛使用的标签和固体支架经常受到特异性不足，苛刻的洗脱要求和成本低效率的限制。在这里，我们开发了一种基于纳米体的强大纯化系统，该系统可以特异性识别短肽表位。该纳米体在原核表达系统中高产出，其相应的肽标签仅包含6-7个氨基酸，可以融合到目标蛋白的N端或c端。我们证明了该系统能够一步纯化细胞裂解物中的多种可溶性和膜蛋白，具有高纯度和产量。结合蛋白在非变性条件下使用竞争性合成肽轻轻洗脱，回收率超过90%。此外，纳米体共轭树脂在至少10次重复使用循环中保持一致的结合能力。鉴于其高特异性、温和洗脱、可重复使用和简单性，我们建议该系统作为高质量蛋白质纯化的多功能和高效平台，在蛋白质组学、结构生物学和生物治疗开发中具有广泛的适用性。

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引用次数: 0

Enrichment of pyrethroid insecticides using effervescent-assisted ionic liquid functionalized in melamine sponge for pipette tip micro solid-phase extraction 三聚氰胺海绵微固相萃取泡腾辅助离子液体富集拟除虫菊酯类杀虫剂。

IF 4 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2026-01-03 DOI: 10.1016/j.chroma.2026.466674

Dararat Saenkam , Pirom Suwannasom , Jitlada Vichapong

A preconcentration and detection method using ionic liquid for embedded in melamine sponge for pipette tip micro solid-phase extraction of pyrethroid insecticides coupled to HPLC was developed for trace amount of pyrethroids residue detection. The synthesis of ionic liquid was accomplished by using tributylhexadecylphosphonium bromide ([P₄₄₄₁₂]Br) and potassium hexafluorophosphate (KPF₆), after that effervescent process was carried out by adding sodium carbonate into a centrifuge tube. The as-prepared ionic liquid was then embedded into melamine sponge, and used for pipette tip micro solid-phase extraction of insecticides in fruit juice matrices. After impregnation, the morphological and structural properties of the sorbents were characterized by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR), respectively. Under the selected conditions, the method exhibited wide linear range (2 – 100 μg l^-1) with a coefficient for determination (R²) greater than 0.99. The limit of quantification (LOQ) and limit of detection (LOD) were in the range of 2 – 3 μg l^-1 and 0.7 – 1 μg l^-1, respectively. Good reproducibility (RSD < 4.65%, n = 5) were achieved. Moreover, the proposed method provided high enrichment factors (EF) ranging from 36.50 to 45.52 folds. The sorbent was then applied to extract pyrethroids in fruit juice. Accuracy was excellent and acceptable recoveries were attained. The greenness profiles were evaluated utilizing multiple assessment metrics including the Analytical Eco-Scale, AGREE Assessment, and BAGI.

建立了离子液体包埋在三聚氰胺海绵中进行移管尖端微固相萃取拟除虫菊酯类杀虫剂的预浓缩检测方法，并结合高效液相色谱法对痕量拟除虫菊酯类杀虫剂残留进行检测。以三烷基十六烷基溴化磷（[P44412]Br）和六氟磷酸钾（KPF6）为原料，在离心管中加入碳酸钠进行泡腾制得离子液体。将制备好的离子液体包埋在三聚氰胺海绵中，用于吸管尖微固相萃取果汁基质中的杀虫剂。浸渍后，用扫描电镜（SEM）和傅里叶变换红外光谱（FTIR）分别表征了吸附剂的形态和结构特性。在所选择的条件下，该方法具有较宽的线性范围（2 ~ 100 μg -1），测定系数（R2）大于0.99。定量限和检出限分别在2 ~ 3 μg -1和0.7 ~ 1 μg -1范围内。重现性好（RSD < 4.65%, n = 5）。此外，该方法具有较高的富集因子（EF），范围为36.50 ~ 45.52倍。然后应用该吸附剂提取果汁中的拟除虫菊酯。准确度极好，回收率可接受。利用多种评估指标对绿色概况进行评估，包括分析生态尺度、AGREE评估和BAGI。

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