Journal of Chromatography A最新文献_第10页

Chromatographic-based 103Ru/103mRh generator for Auger therapy 基于色谱的103Ru/103mRh发生器用于俄歇治疗

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-06-14 DOI: 10.1016/j.chroma.2025.466149

Marie Thery , Anne-Cécile Bonraisin , Cyrille Alliot , Sandrine Huclier-Markai

{"title":"Chromatographic-based 103Ru/103mRh generator for Auger therapy","authors":"Marie Thery , Anne-Cécile Bonraisin , Cyrille Alliot , Sandrine Huclier-Markai","doi":"10.1016/j.chroma.2025.466149","DOIUrl":"10.1016/j.chroma.2025.466149","url":null,"abstract":"<div><div>Conversion and Auger electrons are promising for vectorized internal radiotherapy for cancer treatment, in addition to α and β<sup>-</sup> particles. Rhodium-103 m (t<sub>1/2</sub> = 56.11 min) is an interesting candidate for Auger Therapy and can be produced from Ruthenium-103. The development of a <sup>103</sup>Ru/<sup>103m</sup>Rh generator would provide the possibility of regular supply of <sup>103m</sup>Rh to evaluate its therapeutic potential. In this study, chromatographic separation system allowing Ru retention and Rh elution in chlorinated environment was investigated. A resin based on trioctylphosphine oxide functional groups (TK200) showed promising results. Results with dynamic separations revealed high Rh elution. In addition, Ru partial elution was visible and estimated to 4–8 % of initial amount of Ru. The hypothesis that Ru partial elution was due to Ru(III) presence, not retained by TK200 resin, was suggested and verified. Generator concept has also been tested with <sup>97+103</sup>Ru radioactive isotopes. A reduction in Ru partial elution was observed compared to results obtained with stable Ru isotopes. ¹⁰³Ru/¹⁰³ᵐRh generator developed in this study is operational, even if further improvements are necessary.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1757 ","pages":"Article 466149"},"PeriodicalIF":3.8,"publicationDate":"2025-06-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144307886","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Gravity stop-flow electrophoresis: A high-power technique for size-based separation of graphene oxide nanosheets 重力停止流动电泳：一种基于尺寸的氧化石墨烯纳米片分离的高功率技术

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-06-14 DOI: 10.1016/j.chroma.2025.466145

Masoud Shayegan, Hossein Ahmadzadeh

{"title":"Gravity stop-flow electrophoresis: A high-power technique for size-based separation of graphene oxide nanosheets","authors":"Masoud Shayegan, Hossein Ahmadzadeh","doi":"10.1016/j.chroma.2025.466145","DOIUrl":"10.1016/j.chroma.2025.466145","url":null,"abstract":"<div><div>Graphene oxide (GO) exhibits size-dependent properties that enable its use in a range of applications. Current techniques for size-based separation of GO face several notable limitations and challenges. The gravity stop-flow electrophoresis (GSFE) technique is introduced here, for the first time, which addresses a large part of the stated limitations. Characterization methods were applied to each collected fractions for further correlation between size of each fraction and their corresponding properties. Characterization experiments including, a) the UV–Vis spectroscopy (Stokes shift from 195.4 nm for the smallest particle to 200.7 nm for the largest particle), b) capillary electrophoresis (migration time changed from 6.8 min for the smallest particle to 5 min for the largest particle), c) zeta potential measurement (changed from 23.3 mV for the largest particle to 37.7 mV for the smallest particle), d) electrophoretic mobility (determined by dynamic light scattering, changed from 2.9 × 10–8 m2V-1s-1 for the smallest particle to 1.8 × 10–8 m2V-1s-1 for the largest particle) and e) transmission electron microscopy for the smallest and the largest particles were performed. Furthermore, the results demonstrated that this technique has a high resolution with less limitations when compared to most classical separation methods. Finally, the most important limitation of capillary electrophoresis was resolved by significantly improving the throughput of separation.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1757 ","pages":"Article 466145"},"PeriodicalIF":3.8,"publicationDate":"2025-06-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144298148","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Determination of per- and polyfluoroalkyl substances in tissue using QuEChERS extraction followed by novel enhanced matrix removal mixed-mode passthrough cleanup with LC-MS/MS detection 采用QuEChERS萃取法测定组织中的全氟烷基和多氟烷基物质，然后采用LC-MS/MS检测的新型增强基质去除混合模式穿透清理

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-06-14 DOI: 10.1016/j.chroma.2025.466150

Limian Zhao , Carrie Xu , Emily Parry , Matthew Giardina

{"title":"Determination of per- and polyfluoroalkyl substances in tissue using QuEChERS extraction followed by novel enhanced matrix removal mixed-mode passthrough cleanup with LC-MS/MS detection","authors":"Limian Zhao , Carrie Xu , Emily Parry , Matthew Giardina","doi":"10.1016/j.chroma.2025.466150","DOIUrl":"10.1016/j.chroma.2025.466150","url":null,"abstract":"<div><div>A novel multiresidue method was developed and validated for the quantification of 40 per- and polyfluoroalkyl substances (PFAS) in fish, poultry and terrestrial animal muscle tissues. The method integrates QuEChERS extraction with an enhanced matrix removal (EMR) mixed-mode passthrough cleanup, followed by LC-MS/MS analysis. Validation was performed using tilapia, chicken, and pork matrices, assessing method suitability, selectivity, method detection limits (MDLs), limits of quantitation (LOQs), quantitation accuracy, intra- and inter- batch precision, internal standard recovery and repeatability (both extracted and non-extracted). The method was further cross-validated in cod, canned tuna, beef, and turkey, evaluating suitability and selectivity, MDLs, LOQ, and accuracy and precision at LOQ level.</div><div>The new approach met all acceptance criteria outlined in EPA Method 1633 for tissue matrices, as well as the requirements of relevant EU regulations and AOAC SMPR guidelines. Target quantitation accuracy (apparent recovery) ranged from 72 – 151 % with over 95 % of analytes achieving accuracy within 80 – 120 % range. Precision, expressed as relative standard deviation (RSD), was below 20 % for all compounds across all tested tissue matrices. Internal standard recoveries, both extracted and non-extracted ranged, ranged from 57 to 202 %, with RSD below 9.4 %. Validated LOQs ranged from 0.05 – 1.25 ng/g, while calculated MDLs spanned 0.003 to 0.185 ng/g across the various tissue matrices.</div><div>Compared to the conventional solvent extraction and solid phase extraction (SPE) approach outlined in EPA Method 1633, this method demonstrated enhanced accuracy, precision, and operational efficiency, resulting in significant time and cost savings.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1758 ","pages":"Article 466150"},"PeriodicalIF":3.8,"publicationDate":"2025-06-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144579609","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

On-line preconcentration and analysis of neutral propiconazole and atrazine in wheat flour by micelle to cyclodextrin stacking-micellar electrokinetic chromatography 胶束-环糊精堆积-胶束电动色谱在线富集分析小麦粉中中性丙环康唑和阿特拉津

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-06-13 DOI: 10.1016/j.chroma.2025.466148

Aemi Syazwani Abdul Keyon , Michael Charles Breadmore

{"title":"On-line preconcentration and analysis of neutral propiconazole and atrazine in wheat flour by micelle to cyclodextrin stacking-micellar electrokinetic chromatography","authors":"Aemi Syazwani Abdul Keyon , Michael Charles Breadmore","doi":"10.1016/j.chroma.2025.466148","DOIUrl":"10.1016/j.chroma.2025.466148","url":null,"abstract":"<div><div>Online micelle to cyclodextrin stacking (MCDS) was demonstrated to preconcentrate neutral propiconazole enantiomers and atrazine, followed by separation under suppressed EOF MEKC. Stacking occurred at the boundary between SDS micelle-bound analytes and neutral alpha-cyclodextrin (α-CD), where the analytes were released upon formation of inclusion complexes between SDS micelles and α-CD. The SDS concentration in the sample matrix, the ratio of α-CD and sample solution injection time, and the electrokinetic sample injection voltage during MCDS were optimized. The LODs obtained using MCDS-MEKC were 0.12 µg/mL for propiconazole enantiomeric peak 1, 0.096 µg/mL for propiconazole enantiomeric peak 2 and 0.0018 µg/mL for atrazine. When compared with electrokinetic injection (EKI) in MEKC, the sensitivity enhancement factor (SEFs) of MCDS-MEKC were 59 to 79-fold. Linearity was 20-fold (0.34–6.8 µg/mL) for propiconazole and 200-fold (0.022–4.3 µg/mL) for atrazine; an indication that MCDS-MEKC could be applied for both trace and concentrated analyses. The feasibility of MCDS in a complex sample was demonstrated using spiked wheat flour, where the solid sample was only prepared with an organic solvent, redissolved in the micellar diluent and directly analyzed. The MCDS-MEKC showed the potential in simplicity with good online preconcentration ability without utilizing extensive off-line sample treatment.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1757 ","pages":"Article 466148"},"PeriodicalIF":3.8,"publicationDate":"2025-06-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144307887","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Deep eutectic solvents modified carbon nanotubes as additives for enhanced enantioseparation in capillary electrophoresis 深共晶溶剂修饰碳纳米管作为毛细管电泳中增强对映体分离的添加剂

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-06-12 DOI: 10.1016/j.chroma.2025.466143

Qin Wang, Tianyi Sheng, Ying Lu, Liangliang Cai, Xiaofei Ma

{"title":"Deep eutectic solvents modified carbon nanotubes as additives for enhanced enantioseparation in capillary electrophoresis","authors":"Qin Wang, Tianyi Sheng, Ying Lu, Liangliang Cai, Xiaofei Ma","doi":"10.1016/j.chroma.2025.466143","DOIUrl":"10.1016/j.chroma.2025.466143","url":null,"abstract":"<div><div>Carbon nanotubes (CNTs) possess many excellent properties; however, their strong hydrophobicity makes it difficult for them to disperse in aqueous solutions, leading to aggregation. Although they are considered to have great potential in capillary electrophoresis (CE) for enantioseparation, this issue still limits their widespread application. In this work, we modified the surface of carboxylated multi-walled CNTs with hydrophilic deep eutectic solvents (DESs) via physical adsorption, preparing DESs@CNTs functional materials as buffer additives in CE. Compared to the single maltodextrin (MD) separation system, the DESs@CNTs modified system exhibited significant advantages in chiral separation. Not only was the resolution of the model drugs increased, but the amount of chiral selectors was reduced. We conducted detailed characterization of DESs@CNTs using several methods such as infrared spectroscopy, nuclear magnetic resonance, X-ray diffraction, and transmission electron microscopy. To achieve better separation, a systematic investigation of several key factors affecting the separation was performed. Additionally, we discussed the potential mechanisms of DESs@CNTs on improving separation by ultraviolet spectroscopy. This study is the first application of DESs@CNTs functional materials in CE chiral separation, laying a solid foundation for the development of novel chiral recognition materials.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1757 ","pages":"Article 466143"},"PeriodicalIF":3.8,"publicationDate":"2025-06-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144298147","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Mechanistic multi-objective optimization of ion-pair reversed-phase liquid chromatography for oligonucleotide purification 离子对反相液相色谱法纯化寡核苷酸的机理多目标优化

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-06-12 DOI: 10.1016/j.chroma.2025.466147

Marek Leśko , Martin Enmark , Krzysztof Kaczmarski , Jörgen Samuelsson , Torgny Fornstedt

{"title":"Mechanistic multi-objective optimization of ion-pair reversed-phase liquid chromatography for oligonucleotide purification","authors":"Marek Leśko , Martin Enmark , Krzysztof Kaczmarski , Jörgen Samuelsson , Torgny Fornstedt","doi":"10.1016/j.chroma.2025.466147","DOIUrl":"10.1016/j.chroma.2025.466147","url":null,"abstract":"<div><div>Oligonucleotides (ONs) play a vital role in diagnostics and therapeutics, with ion-pair reversed-phase liquid chromatography (IP-RPLC) being a key method for their purification. This study presents a numerical approach to optimize ON purification using both single-objective (productivity) and multi-objective (productivity and yield) optimization. A transport–dispersive column model incorporating a gradient-modified Langmuir kinetic adsorption–desorption isotherm was employed to describe the separation dynamics. The model was validated against experimental elution profiles of a 20-mer ON and its six most abundant shortmer impurities, and then used to optimize injection volume and gradient slope under varying purity constraints. A hybrid optimization strategy combining simulated annealing (stochastic) with the simplex algorithm (deterministic) was applied.</div><div>The results showed that productivity was maximized at the highest injection volume, while higher purity constraints required shallower gradient slopes. Multi-objective optimization yielded Pareto fronts with unexpected shapes, including inflection points or local minima. We hypothesize that slow adsorption–desorption kinetics limited the model’s ability to accurately describe separations across a broad range of gradient slopes. To test this, two new models were calibrated using only shallow or steep gradient data. The resulting Pareto fronts displayed no inflection points or local minima, supporting our hypothesis.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1757 ","pages":"Article 466147"},"PeriodicalIF":3.8,"publicationDate":"2025-06-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144307890","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Integrated centrifugal microfluidic device with three-dimensional molecular concentrator for plasma separation and biomarker enrichment 带三维分子浓缩器的一体化离心微流控装置用于血浆分离和生物标志物富集

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-06-12 DOI: 10.1016/j.chroma.2025.466146

Wei-Chen Xu , Jun-Yan Lu , Chung-Yu Chen , Ju-Nan Kuo

{"title":"Integrated centrifugal microfluidic device with three-dimensional molecular concentrator for plasma separation and biomarker enrichment","authors":"Wei-Chen Xu , Jun-Yan Lu , Chung-Yu Chen , Ju-Nan Kuo","doi":"10.1016/j.chroma.2025.466146","DOIUrl":"10.1016/j.chroma.2025.466146","url":null,"abstract":"<div><div>Microfluidic-based liquid biopsy allows for sensitive and non-invasive detection of circulating biomarkers such as circulating free DNA (cfDNA), circulating tumor cells (CTCs), and extracellular vesicles (EVs), serving as a valuable tool for early cancer diagnosis, monitoring, and precision medicine. The clinical application of the prostate-specific antigen (PSA) has significantly improved prostate cancer screening. The integration of microfluidics with PSA detection enables ultra-sensitive analysis at low concentrations, crucial for early diagnosis, prompt treatment, and reduced metastasis and mortality. In this research, a novel centrifugal microfluidic device combined with a three-dimensional molecular concentrator was created to separate and quantitatively decant blood plasma from whole blood samples and concentrate PSA biomarker molecules. The volume of plasma entering the molecular concentrator was precisely regulated by adjusting the rotational speed. The electrokinetic behavior of the molecular concentrator was studied through numerical modeling and experimental validation. The incorporation of a microconstriction structure significantly improved electric field localization, enhancing the field-focusing factor by approximately 30,000-fold. This intensified field facilitated rapid molecular accumulation, resulting in a 10<sup>6</sup>-fold increase in PSA within 55 s. This device allows for quick and highly sensitive biomarker detection from minimally processed blood, providing a scalable and cost-effective platform for early cancer diagnosis and precision medicine.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1757 ","pages":"Article 466146"},"PeriodicalIF":3.8,"publicationDate":"2025-06-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144298149","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

A Multi-omics approach combining GC-MS, LC-MS, and FT-NIR with chemometrics and machine learning for metabolites systematic profiling and geographical origin tracing of Artemisia argyi Folium 结合GC-MS、LC-MS、FT-NIR、化学计量学和机器学习的多组学方法在艾叶代谢产物系统分析和地理起源溯源中的应用

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-06-11 DOI: 10.1016/j.chroma.2025.466138

Wennan Nie , Shamukaer Alimujiang , Yao Zhang , Shule Zhang , Wenlong Li

{"title":"A Multi-omics approach combining GC-MS, LC-MS, and FT-NIR with chemometrics and machine learning for metabolites systematic profiling and geographical origin tracing of Artemisia argyi Folium","authors":"Wennan Nie , Shamukaer Alimujiang , Yao Zhang , Shule Zhang , Wenlong Li","doi":"10.1016/j.chroma.2025.466138","DOIUrl":"10.1016/j.chroma.2025.466138","url":null,"abstract":"<div><div><em>Artemisia argyi Folium</em> (AAF) is a widely used functional aromatic medicinal plant with significant health, culinary, and therapeutic value. However, geographical variations in environmental factors notably affect its metabolite production, making comprehensive analysis of AAF quality essential. This study aims to systematically characterize AAF from different geographical regions in China using a multi-omics analysis platform. By employing chemometrics and machine learning, we identify differentiated compounds in AAF and develop rapid, non-destructive models to determine its geographic origin. Comprehensive characterization of AAF samples from seven provinces in China was conducted using HS-SPME-GC–MS, UHPLC-Q-TOF-MS, and FT-NIR. Potential quality markers for volatile and non-volatile compounds were identified through mass spectrometry and chemometrics. Utilizing robust machine learning techniques, XGBoost and Stacking models were constructed for geographic tracing of AAF based on spectral data. Results revealed the identification of 66 volatile and 32 non-volatile compounds via HS-SPME-GC–MS and UHPLC-Q-TOF-MS. Chemometric analysis, including PCA and PLS-DA, highlighted 12 volatile and 12 non-volatile compounds as key quality markers. The combination of FT-NIR with machine learning demonstrated distinct spectral bands for AAF samples from different origins, achieving an accuracy of 94 % through the comparison of 130 spectral preprocessing techniques and three feature selection methods. This study indicates significant metabolomic differences in AAF based on geographic origin, emphasizing the potential of multidimensional metabolomics and machine learning in natural product quality assessment, thereby supporting germplasm development, marketing, and quality control of AAF.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1757 ","pages":"Article 466138"},"PeriodicalIF":3.8,"publicationDate":"2025-06-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144298146","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

A contemporary gas chromatography-electron capture detection (GC-ECD) method for regulatory analysis of polybrominated diphenyl ethers (PBDEs) in unfiltered secondary-treated wastewater 当代气相色谱-电子捕获检测（GC-ECD）方法用于未过滤二级处理废水中多溴联苯醚（PBDEs）的调控分析

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-06-11 DOI: 10.1016/j.chroma.2025.466141

Khoi Phan , Lila Mouakkad , Tom Juma , Ochan Otim

{"title":"A contemporary gas chromatography-electron capture detection (GC-ECD) method for regulatory analysis of polybrominated diphenyl ethers (PBDEs) in unfiltered secondary-treated wastewater","authors":"Khoi Phan , Lila Mouakkad , Tom Juma , Ochan Otim","doi":"10.1016/j.chroma.2025.466141","DOIUrl":"10.1016/j.chroma.2025.466141","url":null,"abstract":"<div><div>Polybrominated diphenyl ethers (PBDEs), a class of flame retardants used extensively in consumer products, have become ecological and public health hazards. Monitoring exposure to them has therefore become a priority as well. At the request of a regulating body, a cost-effective GC-ECD method that exploits advances in gas chromatography was developed in this study to monitor particularly PBDE-28, 47, 99, 100, 153, 154, 183 and 209 in treated municipal wastewater. The proposed method utilizes a programmable injector, an injection volume splitter, and two short open capillary columns (DB-5XLB and DB-5MS) in additoin to a pair of <sup>63</sup>Ni-based halogen-specific electron capture detectors to analyze the PBDEs. All eight PBDEs and PCB-209 surrogate are baseline resolved within a 0.02 min retention time window. The analytes were also recovered quantitatively from single injections of fortified wastewater extracts (range: 76.2–101 % with relative percent deviation range: 2.4–11.7 %). The method detection limits were 1.0–3.4 ng/L for smaller PBDEs and 40 ng/L for PBDE-209. For quantitation, 16 six-point concentration calibration curves, eight for each column, were generated. The relative standard deviations range associated with the curves was 1.6–12 % (<em>r</em><sup>2</sup> > 0.998) for smaller PBDEs and 26–45 % (<em>r</em><sup>2</sup>: 0.984–0.994) for PBDE-209. Additionally, DB-5MS retention times (<em>t</em><sub>R</sub> range: 6.85–18.40 min) were found to relate strongly with DB-XLB retention times (<em>t</em><sub>R</sub>: 7.03–23.32 min) by the polynomial <em>t</em><sub>R(DB-5MS)</sub> =-0.02[<em>t</em><sub>R(DB-XLB)</sub>]<sup>2</sup> + 1.33[<em>t</em><sub>R(DB-XLB)</sub>]-1.94 (<em>r</em>² =0.9997). The relationship suggests that the 182 congeners larger than PBDE-27, but not included here, could be detected and quantified by the proposed method.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1757 ","pages":"Article 466141"},"PeriodicalIF":3.8,"publicationDate":"2025-06-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144291323","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

TLC plate micro-extractor versus TLC-MS Interface: A comparative study on the extraction of non-steroidal anti-inflammatory drugs from milk as a model of a complex matrix TLC平板微萃取器与TLC- ms界面：以复杂基质为模型，从牛奶中提取非甾体类抗炎药的比较研究

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-06-11 DOI: 10.1016/j.chroma.2025.466144

Rafał Gajos, Anna Klimek-Turek, Kamila Trawińska, Tadeusz H. Dzido

{"title":"TLC plate micro-extractor versus TLC-MS Interface: A comparative study on the extraction of non-steroidal anti-inflammatory drugs from milk as a model of a complex matrix","authors":"Rafał Gajos, Anna Klimek-Turek, Kamila Trawińska, Tadeusz H. Dzido","doi":"10.1016/j.chroma.2025.466144","DOIUrl":"10.1016/j.chroma.2025.466144","url":null,"abstract":"<div><div>This study evaluates a new approach for isolating analytes from thin-layer chromatography (TLC) plates, called the TLC plate micro-extraction (TLC-μE) technique, with a focus on non-steroidal anti-inflammatory drugs (NSAIDs). The performance of the TLC-μE device was compared to the commercially available TLC-MS Interface, with both approaches optimised for extraction conditions. Results demonstrate that TLC-μE offers superior extraction efficiency, reduces the risk of cross-contamination, and lowers operational costs. It aligns with green chemistry principles by requiring minimal solvent consumption and operates without electricity or a gas supply, making it suitable for use outside a standard laboratory setting. For methanolic samples, the peak areas for NSAIDs extracted using TLC-μE were more than double those obtained with the TLC-MS Interface under similar conditions. The application of the TLC-μE device for samples with complex matrices was performed by extracting drugs from fortified milk samples. HPLC analysis of the extracts obtained confirmed that TLC-μE demonstrated an average recovery increase of approximately 32.5 % compared to the TLC-MS Interface. These findings suggest that TLC-μE is a promising alternative for integrating TLC with instrumental analysis techniques. Future research will focus on expanding its applicability to a broader range of analytes and matrices.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1757 ","pages":"Article 466144"},"PeriodicalIF":3.8,"publicationDate":"2025-06-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144280348","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0