Pub Date : 2025-01-25DOI: 10.1016/j.chroma.2025.465722
Mikhail S Karbyshev, Irina V Kalashnikova, Viktoriya V Dubrovskaya, Kristina O Baskakova, Pavel K Kuzmichev, Volker Sandig
Bispecific antibodies (bsAbs) represent a rapidly growing field of therapeutic agents. More bsAbs are being approved worldwide and are in various stages of clinical trials. However, the discovery and production of novel bsAbs presents significant challenges due to their complex structure. Thus, precise control of assembly and stability is required, given the many formats developed. This review examines recent trends in bsAb production, focusing on advancements in engineering platforms, production strategies, and challenges in large-scale manufacturing. Key developments include improvements in modular antibody design, novel expression systems, and optimization of bioprocessing techniques to enhance stability, yield, and efficacy. Additionally, the article explores the future potential of bsAbs as next-generation therapeutics, underscoring the growing impact of these innovations on expanding treatment options for patients with unmet medical needs.
{"title":"Trends and challenges in bispecific antibody production.","authors":"Mikhail S Karbyshev, Irina V Kalashnikova, Viktoriya V Dubrovskaya, Kristina O Baskakova, Pavel K Kuzmichev, Volker Sandig","doi":"10.1016/j.chroma.2025.465722","DOIUrl":"https://doi.org/10.1016/j.chroma.2025.465722","url":null,"abstract":"<p><p>Bispecific antibodies (bsAbs) represent a rapidly growing field of therapeutic agents. More bsAbs are being approved worldwide and are in various stages of clinical trials. However, the discovery and production of novel bsAbs presents significant challenges due to their complex structure. Thus, precise control of assembly and stability is required, given the many formats developed. This review examines recent trends in bsAb production, focusing on advancements in engineering platforms, production strategies, and challenges in large-scale manufacturing. Key developments include improvements in modular antibody design, novel expression systems, and optimization of bioprocessing techniques to enhance stability, yield, and efficacy. Additionally, the article explores the future potential of bsAbs as next-generation therapeutics, underscoring the growing impact of these innovations on expanding treatment options for patients with unmet medical needs.</p>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1744 ","pages":"465722"},"PeriodicalIF":3.8,"publicationDate":"2025-01-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143063035","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}
Pub Date : 2025-01-25Epub Date: 2024-12-16DOI: 10.1016/j.chroma.2024.465602
Yu-Cheng Chen, Xue-Zhao Zhong, Ce Shi, Ran Chen, Mattia Sponchioni, Shan-Jing Yao, Dong-Qiang Lin
Development of a next-generation chromatographic model, capable of simultaneously meeting academic demands for thermodynamic consistency and industrial requirements in everyday project work, has become a focal point of research. In this study, anti-Langmuirian to Langmuirian (AL-L) elution behavior was observed in cation-exchange chromatographic separation of charge variants of industrial Fc-fusion proteins. To characterize this behavior, the multi-protein Mollerup activity model was integrated into the steric mass action (SMA) model, resulting in a new model named the generalized ion-exchange (nGIEX) isotherm for multi-protein systems. An R2 exceeding 0.95 calibrated by three elution experiments indicates an effective description of the AL-L behavior (dynamic adsorption). Using isotherm sampling, the nGIEX model exhibited sigmoidal AL-L isotherms (static adsorption). Finally, the model's extrapolation capability was externally validated through process optimization, resulting in an optimal two-step elution condition and a yield improvement of the main variant from 25.9 % to 89.1 % within purity specifications (>70 %).
{"title":"Mechanistic modeling of anti-Langmuirian to Langmuirian behavior of Fc-fusion proteins in cation exchange chromatography.","authors":"Yu-Cheng Chen, Xue-Zhao Zhong, Ce Shi, Ran Chen, Mattia Sponchioni, Shan-Jing Yao, Dong-Qiang Lin","doi":"10.1016/j.chroma.2024.465602","DOIUrl":"10.1016/j.chroma.2024.465602","url":null,"abstract":"<p><p>Development of a next-generation chromatographic model, capable of simultaneously meeting academic demands for thermodynamic consistency and industrial requirements in everyday project work, has become a focal point of research. In this study, anti-Langmuirian to Langmuirian (AL-L) elution behavior was observed in cation-exchange chromatographic separation of charge variants of industrial Fc-fusion proteins. To characterize this behavior, the multi-protein Mollerup activity model was integrated into the steric mass action (SMA) model, resulting in a new model named the generalized ion-exchange (nGIEX) isotherm for multi-protein systems. An R<sup>2</sup> exceeding 0.95 calibrated by three elution experiments indicates an effective description of the AL-L behavior (dynamic adsorption). Using isotherm sampling, the nGIEX model exhibited sigmoidal AL-L isotherms (static adsorption). Finally, the model's extrapolation capability was externally validated through process optimization, resulting in an optimal two-step elution condition and a yield improvement of the main variant from 25.9 % to 89.1 % within purity specifications (>70 %).</p>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1741 ","pages":"465602"},"PeriodicalIF":3.8,"publicationDate":"2025-01-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142908929","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}
Pub Date : 2025-01-25DOI: 10.1016/j.chroma.2025.465728
Victor Castro-Alves, Anh Hoang Nguyen, João Marcos G Barbosa, Matej Orešič, Tuulia Hyötyläinen
Mass spectrometry-based methods have become fundamental to exposome research, providing the capability to explore a broad spectrum of chemical exposures. Liquid and gas chromatography coupled with low/high-resolution mass spectrometry (MS) are among the most frequently employed platforms due to their sensitivity and accuracy. However, these approaches present challenges, such as the inherent complexity of MS data and the expertise of biologists, chemists, clinicians, and data analysts to integrate and interpret MS data with other datasets effectively. The "omics" era advances rapidly, driven by developments of AI-based algorithms and an increase in accessible data; nevertheless, further efforts are necessary to ensure that exposomics outputs are comparable and reproducible, thus enhancing research findings. This review outlines the principles of MS-based methods for the exposome analytical pipeline, from sample collection to data analysis. We summarize and review both standard and cutting-edge strategies in exposome research, covering sample preparation, focusing on MS-based platforms, data acquisition strategies, and data annotation. The ultimate goal of this review is to highlight applications that enable the simultaneous analysis of endogenous metabolites and xenobiotics, which can help enhance our understanding of the impact of human exposure on health and disease and support personalized healthcare.
{"title":"Liquid and gas-chromatography-mass spectrometry methods for exposome analysis.","authors":"Victor Castro-Alves, Anh Hoang Nguyen, João Marcos G Barbosa, Matej Orešič, Tuulia Hyötyläinen","doi":"10.1016/j.chroma.2025.465728","DOIUrl":"https://doi.org/10.1016/j.chroma.2025.465728","url":null,"abstract":"<p><p>Mass spectrometry-based methods have become fundamental to exposome research, providing the capability to explore a broad spectrum of chemical exposures. Liquid and gas chromatography coupled with low/high-resolution mass spectrometry (MS) are among the most frequently employed platforms due to their sensitivity and accuracy. However, these approaches present challenges, such as the inherent complexity of MS data and the expertise of biologists, chemists, clinicians, and data analysts to integrate and interpret MS data with other datasets effectively. The \"omics\" era advances rapidly, driven by developments of AI-based algorithms and an increase in accessible data; nevertheless, further efforts are necessary to ensure that exposomics outputs are comparable and reproducible, thus enhancing research findings. This review outlines the principles of MS-based methods for the exposome analytical pipeline, from sample collection to data analysis. We summarize and review both standard and cutting-edge strategies in exposome research, covering sample preparation, focusing on MS-based platforms, data acquisition strategies, and data annotation. The ultimate goal of this review is to highlight applications that enable the simultaneous analysis of endogenous metabolites and xenobiotics, which can help enhance our understanding of the impact of human exposure on health and disease and support personalized healthcare.</p>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1744 ","pages":"465728"},"PeriodicalIF":3.8,"publicationDate":"2025-01-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143078298","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}
Pub Date : 2025-01-23DOI: 10.1016/j.chroma.2025.465702
Cong Liu , Weihua Liu , Qianqian Wang , Chun Wang , Qiuhua Wu
To effectively control food safety risks caused by nitroimidazoles (NDZs), a sensitive detection method was established on the basis of a newly-developed solid-phase extraction (SPE) sorbent named as Phl-TBM that is a porous polymer prepared by crosslinking natural phloretin with (2,4,6-tris(bromomethyl)mesitylene. The Phl-TBM presented outstanding NDZs adsorption capacity, which can be ascribed to its well-developed porosity and multiple hydrogen bonding sites. With Phl-TBM as SPE sorbent, NDZs were successfully isolated and enriched from lake water, Basa fish, and beef before being assayed by high-performance liquid chromatography-diode array detector. This Phl-TBM based method has a detection limit of 0.02–0.06 ng mL−1 in lake water, 0.60–1.50 ng g−1 in Basa fish, and 0.70–1.20 ng g−1 in beef. The method recoveries are 80.0–120 % with relative standard deviations less than 8.1 %. This study presents an effective and feasible approach for detection of NDZs residues at trace level.
{"title":"Construction of novel hyper-crosslinked polymers with adjustable hydrophilicity for efficient extraction of nitroimidazoles","authors":"Cong Liu , Weihua Liu , Qianqian Wang , Chun Wang , Qiuhua Wu","doi":"10.1016/j.chroma.2025.465702","DOIUrl":"10.1016/j.chroma.2025.465702","url":null,"abstract":"<div><div>To effectively control food safety risks caused by nitroimidazoles (NDZs), a sensitive detection method was established on the basis of a newly-developed solid-phase extraction (SPE) sorbent named as Phl-TBM that is a porous polymer prepared by crosslinking natural phloretin with (2,4,6-<em>tris</em>(bromomethyl)mesitylene. The Phl-TBM presented outstanding NDZs adsorption capacity, which can be ascribed to its well-developed porosity and multiple hydrogen bonding sites. With Phl-TBM as SPE sorbent, NDZs were successfully isolated and enriched from lake water, Basa fish, and beef before being assayed by high-performance liquid chromatography-diode array detector. This Phl-TBM based method has a detection limit of 0.02–0.06 ng mL<sup>−1</sup> in lake water, 0.60–1.50 ng g<sup>−1</sup> in Basa fish, and 0.70–1.20 ng g<sup>−1</sup> in beef. The method recoveries are 80.0–120 % with relative standard deviations less than 8.1 %. This study presents an effective and feasible approach for detection of NDZs residues at trace level.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1743 ","pages":"Article 465702"},"PeriodicalIF":3.8,"publicationDate":"2025-01-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143035643","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}
Pub Date : 2025-01-22DOI: 10.1016/j.chroma.2025.465716
Yang Li , Peng Zhan , Shu-Ya Xue , Lin-Han Xiang , Meng-Ge Feng , Li-Qing Wang , Zi-Kang Cheng , Yang Lv , Zhi-Gao Zhao , Wen Ma , Li-Zhi Chen , Guang-Xue Liu , Ming-Ying Shang , Shao-Qing Cai , Feng Xu
Identification of constitutive herbs in an herbal product is critical for ensuring its quality and efficacy. However, current identification methods often lack universality, entail long durations, and involve complex procedures. Therefore, there is an urgent need to develop innovative methods for identifying constitutive herbs. This paper aims to propose a more refined, universal, simple, rapid, and eco-friendly method for identifying more constitutive herbs in herbal products, significantly enhancing the precision and efficiency of quality control method of herbal products. Leveraging UHPLC‒Q‒TOF‒MS (ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry) data of herbs and the R language, we devised algorithms to find exclusive ions and diagnostic ions of each herb. An open platform named IdenHerb for identifying constitutive herbs of herbal products was established. Using IdenHerb, exclusive ions of 94 herbs were found, and from these exclusive ions, their diagnostic ions were screened out. These diagnostic ions were successfully applied to identify constitutive herbs of two mixtures of herbal powders and eight Chinese patent medicines. Furthermore, this methodology was evaluated using three commonly encountered adulterants as test cases. After incorporating the LC‒MS data of these adulterants into the comprehensive LC‒MS database of all herbs, this approach demonstrated excellent discriminatory capabilities. Compared to the Chinese Pharmacopoeia (2020 edition), IdenHerb is capable of identifying a greater number of constituent herbs, thereby enhancing the level of quality control for the herbal products. This strategy deserves further research and wide application.
{"title":"IdenHerb: A strategy for identifying constitutive herbs of herbal products by screening exclusive ions of each herb from large-scale multi-group LC–MS data","authors":"Yang Li , Peng Zhan , Shu-Ya Xue , Lin-Han Xiang , Meng-Ge Feng , Li-Qing Wang , Zi-Kang Cheng , Yang Lv , Zhi-Gao Zhao , Wen Ma , Li-Zhi Chen , Guang-Xue Liu , Ming-Ying Shang , Shao-Qing Cai , Feng Xu","doi":"10.1016/j.chroma.2025.465716","DOIUrl":"10.1016/j.chroma.2025.465716","url":null,"abstract":"<div><div>Identification of constitutive herbs in an herbal product is critical for ensuring its quality and efficacy. However, current identification methods often lack universality, entail long durations, and involve complex procedures. Therefore, there is an urgent need to develop innovative methods for identifying constitutive herbs. This paper aims to propose a more refined, universal, simple, rapid, and eco-friendly method for identifying more constitutive herbs in herbal products, significantly enhancing the precision and efficiency of quality control method of herbal products. Leveraging UHPLC‒Q‒TOF‒MS (ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry) data of herbs and the R language, we devised algorithms to find exclusive ions and diagnostic ions of each herb. An open platform named IdenHerb for identifying constitutive herbs of herbal products was established. Using IdenHerb, exclusive ions of 94 herbs were found, and from these exclusive ions, their diagnostic ions were screened out. These diagnostic ions were successfully applied to identify constitutive herbs of two mixtures of herbal powders and eight Chinese patent medicines. Furthermore, this methodology was evaluated using three commonly encountered adulterants as test cases. After incorporating the LC‒MS data of these adulterants into the comprehensive LC‒MS database of all herbs, this approach demonstrated excellent discriminatory capabilities. Compared to the Chinese Pharmacopoeia (2020 edition), IdenHerb is capable of identifying a greater number of constituent herbs, thereby enhancing the level of quality control for the herbal products. This strategy deserves further research and wide application.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1743 ","pages":"Article 465716"},"PeriodicalIF":3.8,"publicationDate":"2025-01-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143035652","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}
Pub Date : 2025-01-22DOI: 10.1016/j.chroma.2025.465715
Monica V. Falla , Ivo Lebrun , Marcos A. Pudenzi , Laudiceia A. Oliveira , Heloisa F. Almeida , Nathalia G. Santos , Mariana S. Rodrigues , Patrick J. Spencer , Marisa M. Rocha , Daniel C. Pimenta , Guilherme R. Coelho
Although proteins in snake venoms have been extensively studied and characterized, low-mass molecules remain relatively unexplored, mainly due to their low abundance, secondary role in envenomation, and some analytical technique limitations. However, these small molecules can provide new important data related to venom toxins' molecular structure, functions, and evolutionary relationships. This research aimed to characterize molecules below 10 kDa in the venoms of snakes from the Viperidae families (Bothrops, Agkistrodon, and Bitis) and compare two chromatographic approaches: reverse-phase chromatography (RP), a classic technique, and hydrophilic interaction liquid chromatography (HILIC), an alternative technique, both coupled with high-resolution mass spectrometry (HRMS). The results showed that the separation of the HILIC column provided a more efficient evenly distributed ion profile than RP, contributing to a 25.6% increase in the sequences identified. Homologous sequences for Bradykinin-potentiating peptides (BPPs) and fragments of major venom proteins, possibly cryptids, were found. In addition, BPP 13a, peptides rich in histidine and glycine (pHpG), and spacer sequences were identified in all snakes analyzed, especially with HILIC separation, suggesting that these sequences may be conserved within Viperidae. These findings indicate that the use of the HILIC column, compared to RP, is a promising approach for characterizing peptides in snake venom obtained by the ultrafiltration process. It contributes to the study of these still poorly understood molecules and is also a good option for studying other complex protein/peptide mixtures.
{"title":"Hydrophilic interaction chromatography coupled to high resolution mass spectrometry (HILIC-LC-HRMS): An approach to study natural peptides in Viperidae snake venom","authors":"Monica V. Falla , Ivo Lebrun , Marcos A. Pudenzi , Laudiceia A. Oliveira , Heloisa F. Almeida , Nathalia G. Santos , Mariana S. Rodrigues , Patrick J. Spencer , Marisa M. Rocha , Daniel C. Pimenta , Guilherme R. Coelho","doi":"10.1016/j.chroma.2025.465715","DOIUrl":"10.1016/j.chroma.2025.465715","url":null,"abstract":"<div><div>Although proteins in snake venoms have been extensively studied and characterized, low-mass molecules remain relatively unexplored, mainly due to their low abundance, secondary role in envenomation, and some analytical technique limitations. However, these small molecules can provide new important data related to venom toxins' molecular structure, functions, and evolutionary relationships. This research aimed to characterize molecules below 10 kDa in the venoms of snakes from the <em>Viperidae</em> families (<em>Bothrops, Agkistrodon</em>, and <em>Bitis</em>) and compare two chromatographic approaches: reverse-phase chromatography (RP), a classic technique, and hydrophilic interaction liquid chromatography (HILIC), an alternative technique, both coupled with high-resolution mass spectrometry (HRMS). The results showed that the separation of the HILIC column provided a more efficient evenly distributed ion profile than RP, contributing to a 25.6% increase in the sequences identified. Homologous sequences for Bradykinin-potentiating peptides (BPPs) and fragments of major venom proteins, possibly cryptids, were found. In addition, BPP 13a, peptides rich in histidine and glycine (pHpG), and spacer sequences were identified in all snakes analyzed, especially with HILIC separation, suggesting that these sequences may be conserved within <em>Viperidae</em>. These findings indicate that the use of the HILIC column, compared to RP, is a promising approach for characterizing peptides in snake venom obtained by the ultrafiltration process. It contributes to the study of these still poorly understood molecules and is also a good option for studying other complex protein/peptide mixtures.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1743 ","pages":"Article 465715"},"PeriodicalIF":3.8,"publicationDate":"2025-01-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143045275","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-01-22DOI: 10.1016/j.chroma.2025.465714
Tao Yang , Xinling Li , Jianhua Tan , Wenyao Liang , Xianzhi Peng
Sulfate and sulfonate compounds are extensively used as anionic surfactants in personal care products (PCPs), which might pose adverse potential to human health. However, available research mostly identified certain subsets of sulfated and sulfonated surfactants based on target analysis. In this study, we developed a comprehensive nontarget strategy for identification of sulfated and sulfonated surfactants in PCPs using UHPLCHRMS supplemented by an in-lab R script based on characteristic fragment ions and sulfur isotope patterns. A total of 20 sulfate and 12 sulfonate surfactants of confidence level 3 and above were identified in the range of alkyl chain length from C12 to C26 with 0–7 ethoxy groups and molecular weights of 200–600 Da in the PCP samples. The sulfates included 4 alkyl sulfates and 16 alkyl ether sulfates. In addition to commonly reported 4 alkyl benzene sulfonates, this study identified eight sulfonate surfactants for the first time, which were 3 alkyl sulfonates, 3 methyl ammonium sulfonates, and 2 bis-sulfonate sulfonates in the PCPs. Interestingly, 22 sulfate and sulfonate compounds were identified in the negatively labeled PCP samples which were not supposed to contain sulfate and sulfonate surfactants. The results demonstrated robustness of the developed nontarget analyzing strategy in identifying and characterizing sulfate and sulfonate surfactants and consequently providing guidance for management and regulation of chemical addition in PCPs to ensure safe use.
{"title":"Nontarget screen and identify sulfate and sulfonate surfactants in personal care products using UHPLC-Q-Orbitrap-HRMS based on fragmentation characteristics and sulfur isotopologue pattern","authors":"Tao Yang , Xinling Li , Jianhua Tan , Wenyao Liang , Xianzhi Peng","doi":"10.1016/j.chroma.2025.465714","DOIUrl":"10.1016/j.chroma.2025.465714","url":null,"abstract":"<div><div>Sulfate and sulfonate compounds are extensively used as anionic surfactants in personal care products (PCPs), which might pose adverse potential to human health. However, available research mostly identified certain subsets of sulfated and sulfonated surfactants based on target analysis. In this study, we developed a comprehensive nontarget strategy for identification of sulfated and sulfonated surfactants in PCPs using UHPLC<img>HRMS supplemented by an in-lab R script based on characteristic fragment ions and sulfur isotope patterns. A total of 20 sulfate and 12 sulfonate surfactants of confidence level 3 and above were identified in the range of alkyl chain length from C12 to C26 with 0–7 ethoxy groups and molecular weights of 200–600 Da in the PCP samples. The sulfates included 4 alkyl sulfates and 16 alkyl ether sulfates. In addition to commonly reported 4 alkyl benzene sulfonates, this study identified eight sulfonate surfactants for the first time, which were 3 alkyl sulfonates, 3 methyl ammonium sulfonates, and 2 bis-sulfonate sulfonates in the PCPs. Interestingly, 22 sulfate and sulfonate compounds were identified in the negatively labeled PCP samples which were not supposed to contain sulfate and sulfonate surfactants. The results demonstrated robustness of the developed nontarget analyzing strategy in identifying and characterizing sulfate and sulfonate surfactants and consequently providing guidance for management and regulation of chemical addition in PCPs to ensure safe use.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1743 ","pages":"Article 465714"},"PeriodicalIF":3.8,"publicationDate":"2025-01-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143035695","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}
Pub Date : 2025-01-21DOI: 10.1016/j.chroma.2025.465701
Jia-Mei Kang , Yuan-Yuan Cui , Abdukader Abdukayum , Cheng-Xiong Yang
Considering the widespreadly use, large consumption, and serious environmental and health threats of phenylpyrazole insecticides (PPIs), development of a selective and sensitive method for accurate detection of their residuals in food samples is of great significance and challenging. Herein, depending on the hydrophobic and F-containing characteristics of PPIs, a novel fluorinated magnetic microporous organic network (FMMON) was designed and prepared for efficient and selective magnetic solid-phase extraction (MSPE) of two typical PPIs (fipronil and ethiprole) from milk and egg samples before the HPLC-UV determination. FMMON owned large specific surface area, multiple interaction sites, excellent magnetic separation performance and stability and exhibited good extraction and selectivity for fipronil and ethiprole through the specific F-F, hydrogen bonding, hydrophobic, and π-π interactions. Under optimal extraction conditions, the established FMMON-MSPE-HPLC-UV method provided wide linear ranges (0.1–1000 µg L-1), low limits of detection (0.03–0.05 µg L-1), large enrichment factors (96.2–99.7), low adsorbent consumption (4 mg), and short extraction time (6 min) for fipronil and ethiprole. This work revealed the bright future of fluorinated MONs in sample pretreatment of fluorinated contaminants in complex substrates.
{"title":"Synthesis of a fluorophilic magnetic microporous organic network for selective enrichment of fipronil and ethiprole in milk and egg samples","authors":"Jia-Mei Kang , Yuan-Yuan Cui , Abdukader Abdukayum , Cheng-Xiong Yang","doi":"10.1016/j.chroma.2025.465701","DOIUrl":"10.1016/j.chroma.2025.465701","url":null,"abstract":"<div><div>Considering the widespreadly use, large consumption, and serious environmental and health threats of phenylpyrazole insecticides (PPIs), development of a selective and sensitive method for accurate detection of their residuals in food samples is of great significance and challenging. Herein, depending on the hydrophobic and F-containing characteristics of PPIs, a novel fluorinated magnetic microporous organic network (FMMON) was designed and prepared for efficient and selective magnetic solid-phase extraction (MSPE) of two typical PPIs (fipronil and ethiprole) from milk and egg samples before the HPLC-UV determination. FMMON owned large specific surface area, multiple interaction sites, excellent magnetic separation performance and stability and exhibited good extraction and selectivity for fipronil and ethiprole through the specific F-F, hydrogen bonding, hydrophobic, and π-π interactions. Under optimal extraction conditions, the established FMMON-MSPE-HPLC-UV method provided wide linear ranges (0.1–1000 µg L<sup>-1</sup>), low limits of detection (0.03–0.05 µg L<sup>-1</sup>), large enrichment factors (96.2–99.7), low adsorbent consumption (4 mg), and short extraction time (6 min) for fipronil and ethiprole. This work revealed the bright future of fluorinated MONs in sample pretreatment of fluorinated contaminants in complex substrates.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1743 ","pages":"Article 465701"},"PeriodicalIF":3.8,"publicationDate":"2025-01-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143035714","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}
Pub Date : 2025-01-21DOI: 10.1016/j.chroma.2025.465711
Ana Castiñeira-Landeira , Samantha Sasse , Melissa Broeren , Saskia S. Sterk , Ane Arrizabalaga-Larrañaga
The recent unauthorization of antiviral drugs in food-producing animals according to Commission Delegated Regulation (EU) 2022/1644 have increased the need for food control laboratories to develop analytical methods and perform official controls. In this work, a simple and fast analytical methodology was developed for the simultaneous determination of 21 antiviral drugs in chicken muscle and liver by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). Chromatographic separation was achieved by an HILIC BEH amide column; followed by detection with a electrospray ionization source in positive and negative modes. Based on extraction efficiencies, critical parameters affecting sample treatment were optimized including the evaporation and clean up steps to extract the largest number of antiviral drugs and reduce interferences. The method was validated according to Commission Implementing Regulation (EU) 2021/808 in chicken muscle and liver. Most compounds showed a linearity of R2>0.9800, while decision limits were between 0.18 and 7.05 μg kg−1 and 0.19 and 36 μg kg−1 for chicken muscle and liver, respectively. Trueness and within-lab reproducibility were determined at three levels (n = 7) and the results showed values ranging from 81 to 133 % and 4.2–57 % for chicken muscle, and 71–136 % and 4.6–106 % for chicken liver, respectively. The applicability of the developed method was demonstrated by the analysis real samples. 20 samples from the National Residue Control Plan in the Netherlands were analyzed and although none of targeted compounds were detected it is important to continue the analysis of larger set of samples to address any possible food safety risks.
{"title":"Method development and validation for the simultaneous determination of 21 antiviral drugs by ultra-high performance liquid chromatography-tandem mass spectrometry in chicken muscle and liver","authors":"Ana Castiñeira-Landeira , Samantha Sasse , Melissa Broeren , Saskia S. Sterk , Ane Arrizabalaga-Larrañaga","doi":"10.1016/j.chroma.2025.465711","DOIUrl":"10.1016/j.chroma.2025.465711","url":null,"abstract":"<div><div>The recent unauthorization of antiviral drugs in food-producing animals according to Commission Delegated Regulation (EU) 2022/1644 have increased the need for food control laboratories to develop analytical methods and perform official controls. In this work, a simple and fast analytical methodology was developed for the simultaneous determination of 21 antiviral drugs in chicken muscle and liver by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). Chromatographic separation was achieved by an HILIC BEH amide column; followed by detection with a electrospray ionization source in positive and negative modes. Based on extraction efficiencies, critical parameters affecting sample treatment were optimized including the evaporation and clean up steps to extract the largest number of antiviral drugs and reduce interferences. The method was validated according to Commission Implementing Regulation (EU) 2021/808 in chicken muscle and liver. Most compounds showed a linearity of R<sup>2</sup>>0.9800, while decision limits were between 0.18 and 7.05 μg kg<sup>−1</sup> and 0.19 and 36 μg kg<sup>−1</sup> for chicken muscle and liver, respectively. Trueness and within-lab reproducibility were determined at three levels (<em>n</em> = 7) and the results showed values ranging from 81 to 133 % and 4.2–57 % for chicken muscle, and 71–136 % and 4.6–106 % for chicken liver, respectively. The applicability of the developed method was demonstrated by the analysis real samples. 20 samples from the National Residue Control Plan in the Netherlands were analyzed and although none of targeted compounds were detected it is important to continue the analysis of larger set of samples to address any possible food safety risks.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1743 ","pages":"Article 465711"},"PeriodicalIF":3.8,"publicationDate":"2025-01-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143045277","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-01-21DOI: 10.1016/j.chroma.2025.465688
Dumidu Perera , Valeriia Lishchuk , Amin Hedayati Moghaddam , Juha Mylläri , Susanne K. Wiedmer
This study was conducted to investigate possible differences in the interactions of some selected steroids based on their distribution coefficients with cholesterol- or ergosterol-rich liposomes. Structurally cholesterol and ergosterol have very close resemblance to each other and generally it is thought that they behave in a similar manner. In this work we will show that this is not the case. Liposome electrokinetic chromatography (LEKC) was selected as the methodology for estimating the interactions between the steroids and the liposomes and for calculating the distribution coefficients. Apart from the distribution coefficients, the interactions were also studied with a response surface methodology and exploratory regression analysis. Both graphical and statistical analysis confirmed that there is an obvious difference in the interactions between the studies steroids and the cholesterol- or ergosterol-rich liposomes, and even a minute change in the sterol content had a significant impact on the interactions. The study demonstrates the flexibility and efficacy of LEKC for studying analyte-lipid membrane interactions, and for investigating taylor-made liposome systems.
{"title":"Differences in the distribution of steroids in sterol-containing liposomes: A study by liposome electrokinetic chromatography","authors":"Dumidu Perera , Valeriia Lishchuk , Amin Hedayati Moghaddam , Juha Mylläri , Susanne K. Wiedmer","doi":"10.1016/j.chroma.2025.465688","DOIUrl":"10.1016/j.chroma.2025.465688","url":null,"abstract":"<div><div>This study was conducted to investigate possible differences in the interactions of some selected steroids based on their distribution coefficients with cholesterol- or ergosterol-rich liposomes. Structurally cholesterol and ergosterol have very close resemblance to each other and generally it is thought that they behave in a similar manner. In this work we will show that this is not the case. Liposome electrokinetic chromatography (LEKC) was selected as the methodology for estimating the interactions between the steroids and the liposomes and for calculating the distribution coefficients. Apart from the distribution coefficients, the interactions were also studied with a response surface methodology and exploratory regression analysis. Both graphical and statistical analysis confirmed that there is an obvious difference in the interactions between the studies steroids and the cholesterol- or ergosterol-rich liposomes, and even a minute change in the sterol content had a significant impact on the interactions. The study demonstrates the flexibility and efficacy of LEKC for studying analyte-lipid membrane interactions, and for investigating taylor-made liposome systems.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1743 ","pages":"Article 465688"},"PeriodicalIF":3.8,"publicationDate":"2025-01-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142997673","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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