Journal of separation science最新文献

{"title":"A Protocol for Determination of Proteinogenic Amino Acids in Biological Fluids by the High-Speed UHPLC-MS Method: Application on Transgenic Spontaneously Hypertensive Rat-24 Plasma and Cerebrospinal Fluid Samples","authors":"Juraj Piestansky,&nbsp;Dominika Olesova,&nbsp;Petra Majerova,&nbsp;Petra Chalova,&nbsp;Andrej Kovac","doi":"10.1002/jssc.70089","DOIUrl":"https://doi.org/10.1002/jssc.70089","url":null,"abstract":"<div>\u0000 \u0000 <p>Recently, proteinogenic amino acids have become very interesting molecules, accompanied by a large variety of metabolic processes in humans and are associated with various diseases. In the era of system biology, including a broad spectrum of associated disciplines (e.g., metabolomics, lipidomics, proteomics, etc.), the possibility of identifying trustworthy biomarkers of diseases becomes much more likely. Changes in amino acid levels in plasma, serum, or cerebrospinal fluid reflect physiological or pathological conditions and, therefore, their regular monitoring can lead to early detection of the occurrence of a disease. Therefore, the exact determination of amino acids in biological fluids is of great importance. However, it is necessary to dispose with an effective, accurate, precise, selective, and robust analytical method. This protocol describes the complex procedure of amino acid analysis based on a combination of UHPLC with single quadrupole MS. The protocol presents a highly reproducible and robust methodology that has already been established in the quality control of biopharmaceuticals and determination of proteinogenic amino acids in urine in our laboratory. Here, the application potential is extended to the most frequently investigated biological fluid, that is, plasma and to the cerebrospinal fluid, which is investigated in many neurological conditions.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 2","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-02-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143248429","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}

{"title":"A Protocol for Determination of Proteinogenic Amino Acids in Biological Fluids by the High-Speed UHPLC-MS Method: Application on Transgenic Spontaneously Hypertensive Rat-24 Plasma and Cerebrospinal Fluid Samples","authors":"Juraj Piestansky,&nbsp;Dominika Olesova,&nbsp;Petra Majerova,&nbsp;Petra Chalova,&nbsp;Andrej Kovac","doi":"10.1002/jssc.70089","DOIUrl":"https://doi.org/10.1002/jssc.70089","url":null,"abstract":"<div>\u0000 \u0000 <p>Recently, proteinogenic amino acids have become very interesting molecules, accompanied by a large variety of metabolic processes in humans and are associated with various diseases. In the era of system biology, including a broad spectrum of associated disciplines (e.g., metabolomics, lipidomics, proteomics, etc.), the possibility of identifying trustworthy biomarkers of diseases becomes much more likely. Changes in amino acid levels in plasma, serum, or cerebrospinal fluid reflect physiological or pathological conditions and, therefore, their regular monitoring can lead to early detection of the occurrence of a disease. Therefore, the exact determination of amino acids in biological fluids is of great importance. However, it is necessary to dispose with an effective, accurate, precise, selective, and robust analytical method. This protocol describes the complex procedure of amino acid analysis based on a combination of UHPLC with single quadrupole MS. The protocol presents a highly reproducible and robust methodology that has already been established in the quality control of biopharmaceuticals and determination of proteinogenic amino acids in urine in our laboratory. Here, the application potential is extended to the most frequently investigated biological fluid, that is, plasma and to the cerebrospinal fluid, which is investigated in many neurological conditions.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 2","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-02-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143248640","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}

{"title":"Dual-Template Imprinted Polyaniline Designed by Response Surface Methodology","authors":"V. D. Gorlo,&nbsp;P. S. Pidenko,&nbsp;N. A. Burmistrova","doi":"10.1002/jssc.70091","DOIUrl":"https://doi.org/10.1002/jssc.70091","url":null,"abstract":"<div>\u0000 \u0000 <p>In this work, we investigated the possibility of using response surface methodology to optimize the conditions for the synthesis of molecularly imprinted polyaniline specific to quercetin and horseradish peroxidase simultaneously. The work also discusses the role of horseradish peroxidase during aniline polymerization. As far as we know, a methodology for the synthesis of dual-template imprinted polyaniline selective to low and high molecular weight compounds simultaneously has not been described previously. The imprinted polyaniline layer was obtained on the surface of a microtitration plate, and response surface methodology was used to predict the optimal synthesis conditions to achieve the highest possible selectivity of polyaniline to quercetin (imprinting factor 2.4). We used the predicted optimal conditions to produce a polyaniline-modified microtitration plate and successfully used it for solid-phase extraction of quercetin and horseradish peroxidase with high selectivity (imprinting factors 2.3 and 24.6, respectively) in model solutions. Sorption capacity was 0.7 and 1.2 mg g⁻¹ for quercetin and horseradish peroxidase, respectively. As we can see, the results of response surface methodology prediction were in good agreement with the experimental values of the quercetin imprinting factor.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 2","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-02-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143111834","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}

{"title":"Efficient and Symmetric Temperature Control in Capillary Electrophoresis I: Tying Cooling Capillaries Around Analytical Capillaries","authors":"Tarso B. Ledur Kist","doi":"10.1002/jssc.70081","DOIUrl":"https://doi.org/10.1002/jssc.70081","url":null,"abstract":"<div>\u0000 \u0000 <p>The heat generated by the Joule effect during capillary electrophoresis (CE) runs creates radial temperature gradients in the separation medium. These temperature gradients cause zone dispersion in addition to molecular diffusion. This severely limits the field strengths that can be applied during the runs, especially when solutions with high ionic conductivity are used. This greatly increases run times, especially when high separation efficiencies are sought. In this work, the author proposes tying cooling capillaries (fused silica microtubes) along the external surface of the analytical capillary, allowing the circulation of coolants to efficiently and symmetrically control temperature in CE. The author deduced, step-by-step, the three <i>master equations</i> that serve as guidelines to produce a good match and tightly secure cooling capillaries along the outer surface of analytical capillaries. Additionally, an automated capillary tying machine was developed and demonstrated. Sets were produced with: four, five, and six cooling capillaries tied around one analytical capillary. The outer diameters of the capillaries used (one analytical and <span></span><math>\u0000 <semantics>\u0000 <mi>n</mi>\u0000 <annotation>$n$</annotation>\u0000 </semantics></math> cooling) and the values of the remaining voids left between the first and last cooling capillary are in good agreement with the predictions of the three <i>master equations</i> deduced in this work. To the author's knowledge, this is the first time that cooling capillaries were tied around analytical capillaries to produce an efficient and symmetric cooling system for CE and toroidal capillary electrophoresis.</p></div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 2","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-02-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143111833","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}

{"title":"Dual-Template Imprinted Polyaniline Designed by Response Surface Methodology","authors":"V. D. Gorlo,&nbsp;P. S. Pidenko,&nbsp;N. A. Burmistrova","doi":"10.1002/jssc.70091","DOIUrl":"https://doi.org/10.1002/jssc.70091","url":null,"abstract":"<div>\u0000 \u0000 <p>In this work, we investigated the possibility of using response surface methodology to optimize the conditions for the synthesis of molecularly imprinted polyaniline specific to quercetin and horseradish peroxidase simultaneously. The work also discusses the role of horseradish peroxidase during aniline polymerization. As far as we know, a methodology for the synthesis of dual-template imprinted polyaniline selective to low and high molecular weight compounds simultaneously has not been described previously. The imprinted polyaniline layer was obtained on the surface of a microtitration plate, and response surface methodology was used to predict the optimal synthesis conditions to achieve the highest possible selectivity of polyaniline to quercetin (imprinting factor 2.4). We used the predicted optimal conditions to produce a polyaniline-modified microtitration plate and successfully used it for solid-phase extraction of quercetin and horseradish peroxidase with high selectivity (imprinting factors 2.3 and 24.6, respectively) in model solutions. Sorption capacity was 0.7 and 1.2 mg g⁻¹ for quercetin and horseradish peroxidase, respectively. As we can see, the results of response surface methodology prediction were in good agreement with the experimental values of the quercetin imprinting factor.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 2","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-02-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143111567","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}

{"title":"Efficient and Symmetric Temperature Control in Capillary Electrophoresis I: Tying Cooling Capillaries Around Analytical Capillaries","authors":"Tarso B. Ledur Kist","doi":"10.1002/jssc.70081","DOIUrl":"https://doi.org/10.1002/jssc.70081","url":null,"abstract":"<div>\u0000 \u0000 <p>The heat generated by the Joule effect during capillary electrophoresis (CE) runs creates radial temperature gradients in the separation medium. These temperature gradients cause zone dispersion in addition to molecular diffusion. This severely limits the field strengths that can be applied during the runs, especially when solutions with high ionic conductivity are used. This greatly increases run times, especially when high separation efficiencies are sought. In this work, the author proposes tying cooling capillaries (fused silica microtubes) along the external surface of the analytical capillary, allowing the circulation of coolants to efficiently and symmetrically control temperature in CE. The author deduced, step-by-step, the three <i>master equations</i> that serve as guidelines to produce a good match and tightly secure cooling capillaries along the outer surface of analytical capillaries. Additionally, an automated capillary tying machine was developed and demonstrated. Sets were produced with: four, five, and six cooling capillaries tied around one analytical capillary. The outer diameters of the capillaries used (one analytical and <span></span><math>\u0000 <semantics>\u0000 <mi>n</mi>\u0000 <annotation>$n$</annotation>\u0000 </semantics></math> cooling) and the values of the remaining voids left between the first and last cooling capillary are in good agreement with the predictions of the three <i>master equations</i> deduced in this work. To the author's knowledge, this is the first time that cooling capillaries were tied around analytical capillaries to produce an efficient and symmetric cooling system for CE and toroidal capillary electrophoresis.</p></div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 2","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-02-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143111566","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}

{"title":"Pharmaceuticals, Pesticides, and PFAS: Quantifying Endocrine Disrupting Compounds in Plastics and Fish Tissues Using Solvent Extraction and LC-MS/MS","authors":"Sophie Dolling,&nbsp;Patrick Reis-Santos,&nbsp;Mike Williams,&nbsp;Bronwyn M. Gillanders","doi":"10.1002/jssc.70084","DOIUrl":"https://doi.org/10.1002/jssc.70084","url":null,"abstract":"<p>The rise of plastic pollution in marine environments has been heavily documented, with particular focus on the physical impacts the plastics can have on biota. But, plastics also sorb a range of hydrophobic chemical pollutants, acting as vectors for the transportation of these compounds throughout marine environments. Therefore, an analytical method that can target both marine biota and plastic matrices will be key to advance our understanding of the link between chemicals in the environment, plastic pollution, and effects on biota. Here, an efficient method for the detection and quantification of a broad suite of compounds in marine samples was developed. Five extraction methods were trialed for the analysis of 21 pesticides, PFAS, and pharmaceuticals in biota and plastics. This included three ultrasonic extraction methods and two QuEChERS methods. Ultrasonic extraction in acetonitrile with a microcentrifuge step then concentration by Bond Elut Carbon SPE resulted in best recovery across most compounds. Of the 21 compounds trialed, 16 were efficiently quantified. Method limits of quantification and detection were between 0.02 and 4.81 ppb (mLODs) and between 0.06 and 14.60 ppb (mLOQs). This method is widely applicable to a range of marine environments and supports routine evaluations of environmental safety and monitoring protocols.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 2","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-02-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70084","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143111180","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}

{"title":"Pharmaceuticals, Pesticides, and PFAS: Quantifying Endocrine Disrupting Compounds in Plastics and Fish Tissues Using Solvent Extraction and LC-MS/MS","authors":"Sophie Dolling,&nbsp;Patrick Reis-Santos,&nbsp;Mike Williams,&nbsp;Bronwyn M. Gillanders","doi":"10.1002/jssc.70084","DOIUrl":"https://doi.org/10.1002/jssc.70084","url":null,"abstract":"<p>The rise of plastic pollution in marine environments has been heavily documented, with particular focus on the physical impacts the plastics can have on biota. But, plastics also sorb a range of hydrophobic chemical pollutants, acting as vectors for the transportation of these compounds throughout marine environments. Therefore, an analytical method that can target both marine biota and plastic matrices will be key to advance our understanding of the link between chemicals in the environment, plastic pollution, and effects on biota. Here, an efficient method for the detection and quantification of a broad suite of compounds in marine samples was developed. Five extraction methods were trialed for the analysis of 21 pesticides, PFAS, and pharmaceuticals in biota and plastics. This included three ultrasonic extraction methods and two QuEChERS methods. Ultrasonic extraction in acetonitrile with a microcentrifuge step then concentration by Bond Elut Carbon SPE resulted in best recovery across most compounds. Of the 21 compounds trialed, 16 were efficiently quantified. Method limits of quantification and detection were between 0.02 and 4.81 ppb (mLODs) and between 0.06 and 14.60 ppb (mLOQs). This method is widely applicable to a range of marine environments and supports routine evaluations of environmental safety and monitoring protocols.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 2","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-02-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70084","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143111335","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}

{"title":"Targeting the Antibody Fab Region Using Light-Induced Indole-3-Butyric Acid Functionalized Magnetic Microspheres","authors":"Yu Yi,&nbsp;Yao Li,&nbsp;Sa Wang,&nbsp;Yuting Liang,&nbsp;Jianfeng Mei,&nbsp;Guoqing Ying","doi":"10.1002/jssc.70086","DOIUrl":"https://doi.org/10.1002/jssc.70086","url":null,"abstract":"<div>\u0000 \u0000 <p>A novel light-controlled adsorption system for direct targeting of antibody Fab fragments was developed by utilizing indole-3-butyric acid functionalized magnetic microspheres. Indole-3-butyric acid, serving as a specific small molecule ligand, was successfully conjugated to amine-functionalized magnetic microspheres via a 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide/<i>N</i>-hydroxysuccinimide activation strategy. Under illumination at a particular wavelength, the indole-3-butyric acid ligand generated reactive radicals that interacted with the nucleotide-binding sites of antibody Fab fragments, enabling effective affinity adsorption. Static adsorption experiments demonstrated that the system's adsorption behavior obeys the Langmuir model (<i>K</i>_F = 0.122, <i>R</i>² = 0.996), indicating a homogeneous adsorption process. Kinetic studies further revealed that the adsorption process follows a second-order kinetic model (<i>k</i>₂ = 0.0257, <i>R</i>² = 0.989). When compared with conventional antibody adsorption systems, this new system exhibited specific targeting of Fab fragments, enhanced selectivity, and adjustable properties. In particular, at pH 7.0, effective elution was achieved by increasing the salt concentration, with the eluted product retaining antigen-binding activity. The purification recovery rate exceeded 98%, and the system maintained effective adsorption and elution of Fab fragments across various pH conditions. Besides, even after 10 reuse cycles, the system retained more than 96% of its efficiency, thus presenting excellent regenerability and reusability. In summary, the developed light-controlled antibody Fab region adsorption system offers a highly efficient, stable, and cost-effective approach. It is also expected to become one of the most effective methods for antibody Fab purification in the future.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 2","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-02-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143111338","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}

{"title":"Separation and Purification of Ginsenosides and Flavonoids in From the Leaves and Stems of Panax quinquefolium by High-Speed Countercurrent Chromatography and Online-Storage Inner-Recycling Countercurrent Chromatography","authors":"Chuangchuang Wang,&nbsp;Jinqian Yu,&nbsp;Yingjian Guo,&nbsp;Min Jiang,&nbsp;Kai Zhong,&nbsp;Xiao Wang","doi":"10.1002/jssc.70073","DOIUrl":"https://doi.org/10.1002/jssc.70073","url":null,"abstract":"<div>\u0000 \u0000 <p>Study aimed to isolate and purify compounds from the stems and leaves of <i>Panax quinquefolius</i>. By employing a highly innovative separation technique that combined multistage countercurrent chromatography (MRCC), high-speed countercurrent chromatography (HSCCC), and an advanced online-storage inner-recycling countercurrent chromatography (OS-IRCCC) mode for the first time, 12 compounds were successfully isolated, including 10 ginsenosides and 2 flavonoids. First, the crude extract was fractionated into five parts using D101 MRCC, with HPLC analysis revealing that 40% and 60% ethanol eluate contained the highest compound diversity. Overall, 40% ethanol eluate was separated using the solvent system of EtOAc/<i>n</i>-BuOH/H₂O (2:1:3, v/v), whereas 60% ethanol eluate underwent traditional countercurrent chromatography coupled with OS-IRCCC separation using the solvent system of methyl tert-butyl ether (MTBE)/<i>n</i>-BuOH/ACN/H₂O (4:2:3:8, v/v). Ultimately, various compounds were obtained, including kaempferol 3-<i>O</i>-<i>β</i>-<span>d</span>-glucopyranosyl-(1 → 2)-<i>β</i>-<span>d</span>-galactopyranosyl-7-<i>O</i>-<i>α</i>-<span>l</span>-rhamnopyranoside (13.2 mg), ginsenoside Rc (7.4 mg), 20(R)-ginsenoside Rh₁ (7.2 mg), ginsenoside Re (12.3 mg), kaempferol 3-<i>O</i>-<i>β</i>-<span>d</span>-glucopyranosyl-(1 → 2)-<i>β</i>-<span>d</span>-galactopyranoside (14.1 mg), ginsenoside Rb₁ (8.2 mg), ginsenoside Rb₂ (17.5 mg), ginsenoside Rb₃ (27.3 mg), ginsenoside Rg₁ (13.3 mg), ginsenoside Rg₂ (9.7 mg), ginsenoside Rd (11.4 mg), and pseudo-ginsenoside F₁₁ (16.7 mg). This research highlights the efficacy of the novel separation technique in isolating and purifying valuable compounds from <i>P. quinquefolius</i> stems and leaves.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 2","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-02-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143111078","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}