Journal of separation science最新文献_第2页

Trends in Stationary Phases and Column Technologies 固定相和色谱技术的发展趋势

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2025-07-15 DOI: 10.1002/jssc.70215

Michael Lämmerhofer

引用次数: 0

Trends in Stationary Phases and Column Technologies 固定相和色谱技术的发展趋势

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2025-07-15 DOI: 10.1002/jssc.70215

Michael Lämmerhofer

引用次数: 0

PolyJet Three-dimensional-Printed Microchip Devices With Integrated Carbon Electrodes for Neurotransmitter Analysis 集成碳电极的PolyJet三维打印微芯片设备用于神经递质分析

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2025-07-14 DOI: 10.1002/jssc.70224

Major A. Selemani, Jason L. Assafeen, R. Scott Martin

{"title":"PolyJet Three-dimensional-Printed Microchip Devices With Integrated Carbon Electrodes for Neurotransmitter Analysis","authors":"Major A. Selemani, Jason L. Assafeen, R. Scott Martin","doi":"10.1002/jssc.70224","DOIUrl":"https://doi.org/10.1002/jssc.70224","url":null,"abstract":"<div>\u0000 \u0000 <p>We present an approach for integrating carbon ink electrodes into PolyJet three-dimensional (3D)-printed microfluidic devices for electrochemical (EC) detection. Devices for both microchip-based electrophoresis (ME) and microchip-based flow injection analysis can be created with this methodology. The fabrication involves printing two separate components, a channel layer and an electrode layer, which are thermally bonded to form the final device. For the electrode layer, carbon electrodes are first patterned onto glass substrates using a micromolding technique. A custom stencil is printed directly onto the PolyJet tray to guide precise alignment; the electrode layer is then printed directly over the glass substrate, transferring and embedding the electrodes accurately within the 3D-printed structure. The channel layer is produced by 3D printing either onto a pre-fabricated mold featuring a T-intersection (for ME) or onto the printer tray along with solid support (for microchip-based flow injection analysis). This method yields devices with reliable electrode-channel alignment and minimal band broadening. For ME experiments, the device effectively separated a mixture of neurotransmitters with theoretical plate counts up to 136 000 plates/m and a limit of detection for dopamine of 170 nM. Additionally, we demonstrate how to use 3D printing to integrate off-chip processes such as microdialysis sampling with ME and EC detection. Lastly, we show how microchip flow-based injection analysis devices featuring single or dual in-channel carbon electrodes can also be produced with this approach.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144624648","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Simultaneous Detection and Quantification of Organic Acids and Furans in Lignocellulosic Biomass Hydrolysate Through High-Performance Liquid Chromatography With Diode Array Detector 高效液相色谱二极管阵列检测器同时检测和定量木质纤维素生物质水解液中的有机酸和呋喃

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2025-07-14 DOI: 10.1002/jssc.70216

Patrizia Casella, Raffaele Loffredo, Maria Antonietta Rao, Federico Liuzzi, Isabella De Bari, Antonio Molino

{"title":"Simultaneous Detection and Quantification of Organic Acids and Furans in Lignocellulosic Biomass Hydrolysate Through High-Performance Liquid Chromatography With Diode Array Detector","authors":"Patrizia Casella, Raffaele Loffredo, Maria Antonietta Rao, Federico Liuzzi, Isabella De Bari, Antonio Molino","doi":"10.1002/jssc.70216","DOIUrl":"https://doi.org/10.1002/jssc.70216","url":null,"abstract":"<p>Lignocellulosic biomass is gaining attention as low-cost renewable resources for sugars for fermentation and as a source of energy. Pretreatments and fermentation of these biomasses can generate organic acids and furans. Many liquid chromatography protocols have been developed for the analysis of these compounds. Organic acids are typically detected and quantified using diode array detector, while furans can be analyzed by using refractive index or ultraviolet detectors. In this work, the identification of succinic, lactic, formic, and acetic acids and two furans (5-hydroxymethylfurfural and furfural) was performed by ultra-high-performance liquid chromatography coupled with diode array detector and ion chromatography columns. Different chromatographic conditions were tested by varying the column temperature and the flow rate of sulfuric acid 5 mM. Calibration curves, peak resolution, limit of detection, and limit of quantification were calculated using analytical standards at known concentrations for each compound. The accuracy was evaluated by the recovery of the compounds in wheat straw hydrolysate. For succinic acid, the best condition was at a flow rate of 0.6 mL/min and a column temperature of 60°C while formic and lactic acids and furans were better recovered at 1.0 mL/min and 60°C.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70216","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144624234","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Simultaneous Detection and Quantification of Organic Acids and Furans in Lignocellulosic Biomass Hydrolysate Through High-Performance Liquid Chromatography With Diode Array Detector 高效液相色谱二极管阵列检测器同时检测和定量木质纤维素生物质水解液中的有机酸和呋喃

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2025-07-14 DOI: 10.1002/jssc.70216

Patrizia Casella, Raffaele Loffredo, Maria Antonietta Rao, Federico Liuzzi, Isabella De Bari, Antonio Molino

{"title":"Simultaneous Detection and Quantification of Organic Acids and Furans in Lignocellulosic Biomass Hydrolysate Through High-Performance Liquid Chromatography With Diode Array Detector","authors":"Patrizia Casella, Raffaele Loffredo, Maria Antonietta Rao, Federico Liuzzi, Isabella De Bari, Antonio Molino","doi":"10.1002/jssc.70216","DOIUrl":"https://doi.org/10.1002/jssc.70216","url":null,"abstract":"<p>Lignocellulosic biomass is gaining attention as low-cost renewable resources for sugars for fermentation and as a source of energy. Pretreatments and fermentation of these biomasses can generate organic acids and furans. Many liquid chromatography protocols have been developed for the analysis of these compounds. Organic acids are typically detected and quantified using diode array detector, while furans can be analyzed by using refractive index or ultraviolet detectors. In this work, the identification of succinic, lactic, formic, and acetic acids and two furans (5-hydroxymethylfurfural and furfural) was performed by ultra-high-performance liquid chromatography coupled with diode array detector and ion chromatography columns. Different chromatographic conditions were tested by varying the column temperature and the flow rate of sulfuric acid 5 mM. Calibration curves, peak resolution, limit of detection, and limit of quantification were calculated using analytical standards at known concentrations for each compound. The accuracy was evaluated by the recovery of the compounds in wheat straw hydrolysate. For succinic acid, the best condition was at a flow rate of 0.6 mL/min and a column temperature of 60°C while formic and lactic acids and furans were better recovered at 1.0 mL/min and 60°C.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70216","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144624231","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

PolyJet Three-dimensional-Printed Microchip Devices With Integrated Carbon Electrodes for Neurotransmitter Analysis 集成碳电极的PolyJet三维打印微芯片设备用于神经递质分析

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2025-07-14 DOI: 10.1002/jssc.70224

Major A. Selemani, Jason L. Assafeen, R. Scott Martin

{"title":"PolyJet Three-dimensional-Printed Microchip Devices With Integrated Carbon Electrodes for Neurotransmitter Analysis","authors":"Major A. Selemani, Jason L. Assafeen, R. Scott Martin","doi":"10.1002/jssc.70224","DOIUrl":"https://doi.org/10.1002/jssc.70224","url":null,"abstract":"<div>\u0000 \u0000 <p>We present an approach for integrating carbon ink electrodes into PolyJet three-dimensional (3D)-printed microfluidic devices for electrochemical (EC) detection. Devices for both microchip-based electrophoresis (ME) and microchip-based flow injection analysis can be created with this methodology. The fabrication involves printing two separate components, a channel layer and an electrode layer, which are thermally bonded to form the final device. For the electrode layer, carbon electrodes are first patterned onto glass substrates using a micromolding technique. A custom stencil is printed directly onto the PolyJet tray to guide precise alignment; the electrode layer is then printed directly over the glass substrate, transferring and embedding the electrodes accurately within the 3D-printed structure. The channel layer is produced by 3D printing either onto a pre-fabricated mold featuring a T-intersection (for ME) or onto the printer tray along with solid support (for microchip-based flow injection analysis). This method yields devices with reliable electrode-channel alignment and minimal band broadening. For ME experiments, the device effectively separated a mixture of neurotransmitters with theoretical plate counts up to 136 000 plates/m and a limit of detection for dopamine of 170 nM. Additionally, we demonstrate how to use 3D printing to integrate off-chip processes such as microdialysis sampling with ME and EC detection. Lastly, we show how microchip flow-based injection analysis devices featuring single or dual in-channel carbon electrodes can also be produced with this approach.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144624232","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Synthesis of Perfluorooctyl-Functionalized Halloysite Nanotubes for Dispersive Solid-Phase Extraction of Antimalarial Inhibitors in Whole Blood 全血抗疟抑制剂分散固相萃取用全氟辛基功能化高岭土纳米管的合成

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2025-07-12 DOI: 10.1002/jssc.70226

Kejie Wang, Bingye Shi, Yihui Chen, Chunyan Hou, Xie Li, Xiaoqiang Qiao, Tingting Wang

{"title":"Synthesis of Perfluorooctyl-Functionalized Halloysite Nanotubes for Dispersive Solid-Phase Extraction of Antimalarial Inhibitors in Whole Blood","authors":"Kejie Wang, Bingye Shi, Yihui Chen, Chunyan Hou, Xie Li, Xiaoqiang Qiao, Tingting Wang","doi":"10.1002/jssc.70226","DOIUrl":"https://doi.org/10.1002/jssc.70226","url":null,"abstract":"<div>\u0000 \u0000 <p>Quinine, chloroquine, and hydroxychloroquine are effective antimalarial drugs that have shown antiviral activity against SARS-CoV-2 in initial in vitro studies. However, their excessive use can lead to adverse effects in humans. Therefore, rapid and accurate analysis of these inhibitors in whole blood samples is crucial for public health, although this presents significant challenges. In this study, perfluorooctyl-functionalized halloysite nanotubes were synthesized and used as sorbents for dispersive solid-phase extraction. The developed sorbents interacted with inhibitors through various mechanisms, including hydrophobic interactions, electrostatic interactions, F–π interactions, and hydrogen bonding. Notably, their adsorption capacity was twice that of unmodified halloysite nanotubes. By combining the perfluorooctyl-functionalized halloysite nanotubes-based dispersive solid-phase extraction method with liquid chromatography-tandem mass spectrometry, an analytical method was developed to determine concentrations of the three inhibitors in whole blood samples. Under optimized conditions, the limits of detection ranged from 1.2 to 2.1 ng/mL. The recoveries achieved 91.9%–101.5% for intra-day and 92.8%–101.2% for inter-day. The inter- and intra-day relative standard deviations were in the range of 0.6%–3.8% and 2.3%–8.1%, respectively. This study introduces a novel approach for developing sorbents to target drugs and presents an innovative analytical method for therapeutic monitoring. These advancements will facilitate the evaluation of the pharmacokinetics of these inhibitors in patients and support ongoing clinical trials.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144606501","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Identification, Isolation and Structural Elucidation of New Inner Salt Impurity in Vildagliptin and Metformin Tablet by Using Supercritical Fluid Chromatography, NMR, HRMS 维格列汀二甲双胍片剂中新的内盐杂质的超临界液相色谱、核磁共振、质谱鉴定、分离及结构解析

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2025-07-12 DOI: 10.1002/jssc.70218

Saravana Kumar Meganathan, Bijaya Ketan Sahoo, Y. Rajender Reddy, K. Rajani, Peedi Rajasekhara Reddy

{"title":"Identification, Isolation and Structural Elucidation of New Inner Salt Impurity in Vildagliptin and Metformin Tablet by Using Supercritical Fluid Chromatography, NMR, HRMS","authors":"Saravana Kumar Meganathan, Bijaya Ketan Sahoo, Y. Rajender Reddy, K. Rajani, Peedi Rajasekhara Reddy","doi":"10.1002/jssc.70218","DOIUrl":"https://doi.org/10.1002/jssc.70218","url":null,"abstract":"<p>Vildagliptin is an orally active antihyperglycemic agent used for the treatment of type 2 diabetes mellitus in adults as monotherapy either alone or in combination with metformin. The presence of impurities in drug substances or drug products could be toxic and unsafe (injurious) to the user, and it should be ensured that drugs must be free of or controlled from any impurities to the specified level as per International Council for Harmonization guidelines before that reaches the user. That is the reason why work on identification, isolation, and characterization of impurities in drug substances and drug products is very important towards ensuring drug safety and efficacy. Further, product-related impurity isolation and characterization is an important aspect of pharmaceutical processes. The aim of the work is to identify a new impurity which was detected in vildagliptin and metformin tablets under stability storage conditions by using high-performance liquid chromatography (HPLC). The new impurity was isolated and characterized by using comprehensive analysis of HPLC, flash chromatography, supercritical fluid chromatography, Fourier transform infrared spectroscopy, high-resolution mass spectrometry, 1D-NMR [<sup>1</sup>H and <sup>13</sup>C], and 2D-NMR (<sup>1</sup>H-<sup>1</sup>H correlated spectroscopy, total correlated spectroscopy, <sup>1</sup>H-<sup>13</sup>C heteronuclear single quantum coherence spectroscopy, <sup>1</sup>H-<sup>13</sup>C and <sup>1</sup>H-<sup>15</sup>N heteronuclear multiple bond coherence spectroscopy) spectroscopic data.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70218","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144606749","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Vortex-Assisted Magnetic Nanofluid-Based Liquid Phase Microextraction of Methylene Blue and Crystal Violet 涡流辅助磁纳米流体液相微萃取亚甲基蓝和结晶紫

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2025-07-12 DOI: 10.1002/jssc.70225

Xiaochun Chen, Wenxu Hu, Yang Yu, Dandan Ge, Zhehui Weng, Yao Huang, Ren Li

{"title":"Vortex-Assisted Magnetic Nanofluid-Based Liquid Phase Microextraction of Methylene Blue and Crystal Violet","authors":"Xiaochun Chen, Wenxu Hu, Yang Yu, Dandan Ge, Zhehui Weng, Yao Huang, Ren Li","doi":"10.1002/jssc.70225","DOIUrl":"https://doi.org/10.1002/jssc.70225","url":null,"abstract":"<div>\u0000 \u0000 <p>In the present study, a new vortex-assisted magnetic solid phase extraction method was developed based on magnetic ZIF-67 (MZIF-67) nanofluid and supramolecular solvents (SUPRASs) for the extraction and preconcentration of synthetic dyes, followed by high performance liquid chromatography-diode array detector detection. MZIF-67 functionalized with sodium dodecyl sulfate and titanium dioxide (MZIF-67/SDS-TiO<sub>2</sub>) were synthesized and used as magnetic materials. SUPRAS prepared from hexafluorobutanol and nerol was employed as the carrier liquid. Finally, FFs were prepared by adding MZIF-67/SDS-TiO<sub>2</sub> to SUPRAS for the first time. The prepared adsorbents were characterized by scanning electron microscopy, x-ray diffraction, and Fourier transform infrared spectroscopy. The extraction efficiency of the developed method was enhanced by optimization of the influencing parameters. Under the optimized conditions, the linearity was in the range of 9–1000 ng mL<sup>−1</sup> with regression coefficients higher than 0.9961. The limits of detection and limits of quantification were in the range of 2.5–2.7–8.4–9.1 ng mL<sup>−1</sup>, respectively. Finally, the developed method was applied to determine synthetic dyes in river water and beverage samples. Extraction recoveries ranged from 91.0% to 105.8% with relative standard deviations between 0.9% and 7.9%. The green character of the developed method was assessed using the AGREEprep tool. The obtained results indicate that the established method has low environmental impact. The developed method is a simple, cheap, green, and fast and can be applied to determine synthetic dyes in sample solutions.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144606463","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

A Facile Hydrophilic Coating to Construct Immobilized Metal Affinity Chromatography for Protein Adsorption 构建固定化金属亲和层析用于蛋白质吸附的易溶亲水涂层

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2025-07-12 DOI: 10.1002/jssc.70219

Xiao-Bei Huang, Yong-Ming Wei, Lin Yu, Zhen-Liang Xu, Hu Yang

{"title":"A Facile Hydrophilic Coating to Construct Immobilized Metal Affinity Chromatography for Protein Adsorption","authors":"Xiao-Bei Huang, Yong-Ming Wei, Lin Yu, Zhen-Liang Xu, Hu Yang","doi":"10.1002/jssc.70219","DOIUrl":"https://doi.org/10.1002/jssc.70219","url":null,"abstract":"<div>\u0000 \u0000 <p>Immobilized metal affinity chromatography is a green method applied to the separation and purification of proteins and biomolecules in downstream processing. With its unique internal pores, the membrane carriers have more active sites than typical magnetic nanoparticles and beads. It also greatly overcomes the mass-transfer resistance brought by traditional column chromatography. In this study, polysulfone was selected as the pristine membrane. Tannic acid and 3-aminopropyltriethoxysilane coatings were employed to construct the secondary reaction platform, which was then covalently coupled with polyethyleneimine and grafted with iminodiacetic acid groups to chelate Cu<sup>2+</sup>. Bovine serum albumin was utilized as the adsorption protein to adjust and optimize the modification parameters. The results demonstrated that the adsorption amount per unit membrane area reached 0.19 mg/cm<sup>2</sup> under the solution condition of pH 8.5. The adsorption thermodynamics followed the Langmuir model, and the corresponding model parameters were obtained.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144606499","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0