Kristine Joy Camacho, Oksana Tchoul, Yuehong Xu, Abraham Finny, Lavelay Kizekai, Justin McLaughlin, Steven Byrd, Balasubrahmanyam Addepalli, MingCheng Xu, Matthew Lauber
{"title":"Bridged Ethylene Polyethylene Oxide Surfaces to Improve Packing Materials for Widepore Size Exclusion Chromatography","authors":"Kristine Joy Camacho, Oksana Tchoul, Yuehong Xu, Abraham Finny, Lavelay Kizekai, Justin McLaughlin, Steven Byrd, Balasubrahmanyam Addepalli, MingCheng Xu, Matthew Lauber","doi":"10.1002/jssc.202400541","DOIUrl":"10.1002/jssc.202400541","url":null,"abstract":"<p>Here, we describe the preparation of bridged ethylene polyethylene oxide (BE-PEO) surface-modified silica packing materials for size exclusion chromatography. BE-PEO surface-modified silica was hydrolyzed and subsequent <sup>1</sup>H nuclear magnetic resonance analysis of hydrolysis products confirmed the successful formation of BE-PEO bonded surface. Silica particles exhibiting 3 µm diameters and 1000 Å nominal pore diameters were selected as a base material for this work out of the critical need to improve analytical capabilities for the testing of cell and gene therapy drug products. Accelerated high pH aging study revealed significant enhancement in column stability. Multi-angle light scattering noise measurements showed inordinately lower baseline noise. Moreover, we evaluated the chromatographic performance of BE-PEO silica-packed columns through separations of a protein test mixture, DNA ladder, monoclonal antibody-based therapeutics, and adeno-associated viruses. BE-PEO silica columns demonstrated high resolution, high recovery separations that were confirmed to be reproducible and capable of extended column lifetimes and exhibited low ionic and hydrophobic secondary interactions. In summary, BE-PEO silica particles have yielded a new level of performance, improved base stability, and inherently lower baseline noise. These novel widepore particles will facilitate more sensitive size-based detection and characterization of large biologics in the form of advanced gene therapy products.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"47 20","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-10-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.202400541","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142451773","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}
Zuzana Kilianova, Ivana Cizmarova, Miroslava Spaglova, Juraj Piestansky
{"title":"Recent Trends in Therapeutic Drug Monitoring of Peptide Antibiotics","authors":"Zuzana Kilianova, Ivana Cizmarova, Miroslava Spaglova, Juraj Piestansky","doi":"10.1002/jssc.202400583","DOIUrl":"https://doi.org/10.1002/jssc.202400583","url":null,"abstract":"<div>\u0000 \u0000 <p>Antimicrobial peptides take a specific position in the field of antibiotics (ATBs), however, from a large number of available molecules only a few of them were approved and are used in clinics. These therapeutic modalities play a crucial role in the management of diseases caused by multidrug-resistant bacterial pathogens and represent the last-line therapy for bacterial infections. Therefore, there is a demand for a rationale use of such ATBs based on optimization of the dosing strategy to minimize the risk of resistance and ensure the sustainable efficacy of the drug in real clinical practice. Therapeutic drug monitoring, as a measurement of drug concentration in the body fluids or tissues, results in the optimization of the patient´s medication and therapy outcome. This strategy is beneficial and could result in tailored therapy for different types of infection and the prolongation of the use and efficacy of ATBs in hospitals. This review paper provides an actual overview of approved antimicrobial peptides used in clinical practice and covers current trends in their analysis by convenient and advanced methodologies used for their identification and/or quantitation in biological matrices for therapeutic drug monitoring purposes. Special emphasis is given to the methods with perspective clinical outcomes.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"47 19","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-10-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142435449","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}
Enas Yousef, Charles Phillip Shelor, Seth A. Horn, Purnendu K. Dasgupta
{"title":"Functionalization of High-Density Polyethylene Capillaries for Open Tubular Ion Chromatography","authors":"Enas Yousef, Charles Phillip Shelor, Seth A. Horn, Purnendu K. Dasgupta","doi":"10.1002/jssc.202400455","DOIUrl":"10.1002/jssc.202400455","url":null,"abstract":"<div>\u0000 \u0000 <p>Ion chromatography is the anion analysis benchmark. A miniature form, Open Tubular Ion Chromatography (OTIC), has attractive attributes for efficient ion separations. Here, we fabricate and characterize high-density polyethylene (HDPE) open tubular anion exchange columns (OTCs). We attach positively charged latex particles onto negatively charged capillary surfaces. For efficient OTIC, column diameters need to be < ∼20 µm; functionalizing the bore is challenging. Methods to introduce acid groups to an HDPE capillary bore, e.g., sulfonation using chlorosulfonic or sulfuric acid solutions, with or without grafting of an aromatic ring through photo- or chemical grafting first, are explored. Following quaternary ammonium latex attachment, the ion exchange capacity and separating abilities of each OTC were measured as an index of OTC performance. Gradual loss of capacity was observed for many of these; high-resolution mass spectrometry confirmed the leaching of detached oxidized/sulfonated oligomeric fragments and consequent poisoning of the latex sites. Ways to ameliorate this and/or to rejuvenate the columns are also described.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"47 19","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142391450","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}
Nguyen Minh Luan, Vo Thi Kim Khuyen, Nguyen Duc Tuan
{"title":"High-Performance Liquid Chromatography–Tandem Mass Spectrometry Method Development and Validation for Simultaneous Determination of Seven Nitrosamine and Azidomethyl-Biphenyl-Tetrazole Impurities in Losartan","authors":"Nguyen Minh Luan, Vo Thi Kim Khuyen, Nguyen Duc Tuan","doi":"10.1002/jssc.202400277","DOIUrl":"10.1002/jssc.202400277","url":null,"abstract":"<div>\u0000 \u0000 <p>Nitrosamine-related impurities (<i>N</i>-nitrosomethylamino butyric acid [NMBA], <i>N</i>-nitrosodiethylamine [NDEA], <i>N</i>-nitrosodiisopropylamine [NDIPA], <i>N</i>-nitrosomethylphenylamine [NMPA], <i>N</i>-nitrosodibutylamine [NDBA], <i>N</i>-nitrosodimethylamine [NDMA], and <i>N</i>-nitrosoethylisopropylamine [NEIPA]) and 5-[4'-(azidomethyl)-[1,1'-biphenyl]-2-yl]-2H-tetrazole (AZBT) formed during the manufacture of sartan medicines have been classified into human mutagens and carcinogens after long-term treatment. The study developed a simple, economical but highly sensitive procedure for the simultaneous quantification of seven nitrosamines and AZBT impurities in sartan pharmaceuticals. After extraction with methanol (MeOH) 50%, the compounds were analyzed with a reversed-phase liquid chromatography–tandem mass spectroscopy with atmospheric-pressure chemical ionization (APCI) mode (APCI[+] for nitrosamines and APCI[−] for AZBT), selected reaction monitoring, C18 column, gradient elution with 0.1% formic acid in water and in MeOH, respectively. The validated procedure obtained high extraction efficiency (>90%), wide linear range (0.2–50.0 ng/mL NMBA, NDEA, NDIPA, NMPA, and NDBA; 0.5–50.0 ng/mL NDMA and NEIPA; 2.0–100 ng/mL AZBT), limit of quantification < 10% of the acceptance level, recovery range of 85%–115% with relative standard deviation < 15% and minimum matrix effects for all impurities. The procedure was applied to test 16 commercial losartan samples. As a result, eight samples contained AZBT within the current regulatory limits, but no nitrosamine impurities were detected in all samples.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"47 19","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142391452","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":"Stimuli-Responsive Molecularly Imprinted Polymers: Mechanism and Applications","authors":"Zheng Li, Jiaming Deng, Peirong Ma, Haoran Bai, Yuting Jin, Yanling Zhang, Alideertu Dong, Munkhjargal Burenjargal","doi":"10.1002/jssc.202400441","DOIUrl":"10.1002/jssc.202400441","url":null,"abstract":"<div>\u0000 \u0000 <p>Molecularly imprinted polymers (MIPs) are very suitable for extraction, drug delivery systems, and sensors due to their good selective adsorption ability, but the difficulty of eluting templates during synthesis and the limitation of application scenarios put higher demands on MIPs. Stimuli-responsive MIPs (SR-MIPs) can actively respond to changes in external conditions to realize various functions, which provides new ideas for the further development of MIPs. This paper reviews the multiple response modes of MIPs, including the common temperature, pH, photo, magnetic, redox-responsive and rare gas, biomolecule, ion, and solvent-responsive MIPs, and explains the mechanism, composition, and applications of such SR-MIPs. These SR-MIPs and the resulting dual/multiple-responsive MIPs have good selectivity, and controllability, and are very promising for isolation and extraction, targeted drug delivery, and electro-sensor.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"47 19","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142391454","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}
Haixia Li, KaiLin Li, Wenhui Cheng, Mingjuan Liu, Linwen Wen, Zexu Zhang, Wendan Zhang, Jin Su, Wei Cai
{"title":"Rapid Characterization of the Potential Active of Sinomenine in Rats by Ultra-High-Performance Liquid Chromatography-Quadrupole-Exactive Orbitrap Mass Spectrometry and Molecular Docking","authors":"Haixia Li, KaiLin Li, Wenhui Cheng, Mingjuan Liu, Linwen Wen, Zexu Zhang, Wendan Zhang, Jin Su, Wei Cai","doi":"10.1002/jssc.202400486","DOIUrl":"10.1002/jssc.202400486","url":null,"abstract":"<div>\u0000 \u0000 <p><i>Sinomenium acutum</i> (Thunb.) Rehd. et Wils is widely used in the treatment of rheumatoid arthritis, with its alkaloid compound sinomenine (SIN) being renowned for its significant anti-inflammatory properties. However, despite its widespread application, the in vivo anti-inflammatory mechanisms and metabolic pathways of SIN remain incompletely understood. This study established a rapid and reliable method based on an ultra-high-performance liquid chromatography method coupled with Quadrupole-Exactive Orbitrap mass spectrometry and molecular docking to identify and characterize SIN and 69 metabolites in rat plasma, urine, and feces, revealing primary metabolic pathways of hydroxylation, demethylation, sulfation, and glucuronidation. Molecular docking results revealed that phase I reactions, including dedimethylation, demethylation, dehydrogenation, and dihydroxylation, along with their composite reactions, were pivotal in influencing SIN's in vivo anti-inflammatory activity. M28, M36, and M59 are potentially the most anti-inflammatory active metabolites of SIN in vivo. This comprehensive analysis unveils SIN's metabolic pathways, offering insights into its biological processes and suggesting a novel approach for exploring active drug constituents. These findings pave the way for further understanding SIN's anti-inflammatory mechanisms, contributing significantly to the development of new therapeutic strategies.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"47 19","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-10-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142391453","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":"Greening Separation and Purification of Proteins and Peptides","authors":"Katarína Maráková","doi":"10.1002/jssc.202400554","DOIUrl":"10.1002/jssc.202400554","url":null,"abstract":"<div>\u0000 \u0000 <p>The increasing awareness of environmental issues and the transition to green analytical chemistry (GAC) have gained popularity among academia and industry in recent years. One of the principles of GAC is the reduction and replacement of toxic solvents with more sustainable and environmentally friendly ones. This review gives an overview of the advances in applying green solvents as an alternative to the traditional organic solvents for peptide and protein purification and analysis by liquid chromatography (LC) and capillary electrophoresis (CE) methods. The feasibility of using greener LC and CE methods is demonstrated through several application examples; however, there is still plenty of room for new developments to fully realize their potential and to address existing challenges. Thanks to the tunable properties of designer solvents, such as ionic liquids and deep eutectic solvents, and almost infinite possible mixtures of components for their production, it is possible that some new designer solvents could potentially surpass the traditional harmful solvents in the future. Therefore, future research should focus mainly on developing new solvent combinations and enhancing analytical instruments to be able to effectively work with green solvents.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"47 19","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-10-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142391451","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}
Ahlem Eddehech, Alessia Tropea, Francesca Rigano, Danilo Donnarumma, Emna Ben Abdallah, Francesco Cacciola, Luigi Mondello, Zied Zarai
{"title":"Evaluation of Microbial Phospholipase and Lipase Activity Through the Chromatographic Analysis of Crude, Degummed, and Transesterified Soybean Oil for Biodiesel Production","authors":"Ahlem Eddehech, Alessia Tropea, Francesca Rigano, Danilo Donnarumma, Emna Ben Abdallah, Francesco Cacciola, Luigi Mondello, Zied Zarai","doi":"10.1002/jssc.202400325","DOIUrl":"10.1002/jssc.202400325","url":null,"abstract":"<p>The present study aimed at synthesizing fatty acid methyl esters in a combined enzymatic method by applying degumming and transesterification of soybean oil. A soluble lipase from <i>Serratia</i> sp. W3 and a recombinant phosphatidylcholine-preferring phospholipase C (PC-PLC) from <i>Bacillus thuringiensis</i> were used in a consecutive manner for phosphorus removal and conversion into methyl esters. By applying 1% of recombinant PC-PLC almost 83% of phosphorus was removed (final content of 21.01 mg/kg). Moreover, a sensitive and selective high-performance liquid chromatography method coupled to tandem mass spectrometry was applied to obtain a comprehensive lipid profile for the simultaneous evaluation of phospholipids removal and diacylglycerol (DAG) increase. A significant increase for all the monitored DAG species, up to 138.42%, was observed by using the enzymatic degumming, in comparison to the crude sample, resulting in an increased oil yield. <i>Serratia</i> sp. W3 lipase was identified as a suitable biocatalyst for biodiesel production, converting efficiently the acylglycerols. The results regarding the physical-chemical characteristics show that the cetane level, density and pour point of the obtained biodiesel are close to current regulation requirements. These findings highlight the potential of a two-step process implementation, based on the combination of lipase and phospholipase, as a suitable alternative for biodiesel production.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"47 19","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-10-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.202400325","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142391449","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}
Lea Böckstiegel, Theresa Schaumann, Björn Egert, Sabine E. Kulling, Christoph H. Weinert
{"title":"Development of an Untargeted Method for the Analysis of the Volatile Profile of Onions via Solid-Phase Microextraction Arrow-Headspace-Gas Chromatography-Mass Spectrometry Using Design of Experiments","authors":"Lea Böckstiegel, Theresa Schaumann, Björn Egert, Sabine E. Kulling, Christoph H. Weinert","doi":"10.1002/jssc.202400305","DOIUrl":"10.1002/jssc.202400305","url":null,"abstract":"<p>The distinctive aroma of onions, consisting primarily of sulfur-containing compounds, is one of the reasons for the popularity of the vegetable. The rapid enzymatic and chemical reactions that occur after the destruction of onion bulb tissue render the analysis of the volatile profile challenging. Therefore, sample preparation is a crucial step in the analysis of the onion volatilome, but it often does not receive the necessary attention in the literature. In this work, we focused on two aspects: Firstly, we compared different sample preparation approaches to maximize the volatile yield and to enable the description of the onion volatile profile as it would emerge after a solid-phase microextraction (SPME) Arrow sampling procedure. For headspace (HS)-gas chromatography-mass spectrometry analysis, onion juice with the addition of an ammonium sulfate solution proved to be the best option. Secondly, we optimized the HS sampling and desorption parameters (enrichment time, enrichment temperature, agitator speed, desorption time) for onion volatiles using the efficient design of experiments (DoE) approach. The optimal conditions for the analysis with HS-SPME Arrow were an enrichment time of 75 min at 60°C with an agitator speed of 713 rpm and a desorption time of 120 s.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"47 19","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-10-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.202400305","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142372148","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}
Qian Li, Li-mei Wang, Shu-mei Zhang, Guang-bin Zhang, Shuang Hu
{"title":"Preconcentration of Cinnamic Acid Derivatives in Traditional Chinese Medicines by an Effective Dispersive Liquid-Liquid Microextraction Based on a Hydrophobic Deep Eutectic Solvent","authors":"Qian Li, Li-mei Wang, Shu-mei Zhang, Guang-bin Zhang, Shuang Hu","doi":"10.1002/jssc.202400363","DOIUrl":"10.1002/jssc.202400363","url":null,"abstract":"<div>\u0000 \u0000 <p>A dispersive liquid-liquid microextraction based on hydrophobic deep eutectic solvent (hDES) was developed for the extraction and quantification of four cinnamic acid derivatives in traditional Chinese medicines coupled with high-performance liquid chromatography-ultraviolet detection. In this method, a hDES (tetrabutylammonium chloride-hexanoic acid, molar ratio of 1:2) was prepared as the extractant. It only took 15 s to handle multiple samples simultaneously by hand-assisted dispersion. The use of a narrow-bore tube reduced the amount of the hydrophobic extractant with easier recovery. The approach was influenced by several key parameters, including the composition and consumption of the DES, sample phase pH, salt amount, extraction time, and centrifugation time, all of which had been investigated and optimized. Moreover, the formation of the DES was characterized by Fourier-transform infrared spectroscopy and differential scanning calorimetry. Under the optimal conditions, enrichment factors of the target analytes ranged from 135 to 220. Satisfactory linearities (<i>r</i> ≥ 0.9977), detection limits (0.2–0.4 ng/mL), precision (<8.5%), and accuracy (recoveries: 90.0%–104.6%) were obtained. The method has been successfully applied to the simultaneous extraction and preconcentration of four cinnamic acid derivatives in Chinese medicinal samples with rapidness, high efficiency, and convenience.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"47 19","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142349013","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}