Journal of separation science最新文献

{"title":"The Last 10 Years of Research in the Enantioseparation of Pharmacologically Relevant Phytocannabinoids: An Updated Review","authors":"Ina Varfaj,&nbsp;Federica Ianni,&nbsp;Ghaid W. A. Abualzulof,&nbsp;Anna Migni,&nbsp;Laura Mercolini,&nbsp;Sandra Furlanetto,&nbsp;Andrea Carotti,&nbsp;Roccaldo Sardella","doi":"10.1002/jssc.70234","DOIUrl":"https://doi.org/10.1002/jssc.70234","url":null,"abstract":"<div>\u0000 \u0000 <p>As research on <i>Cannabis sativa</i> L. and its derivatives expands, an increasing number of novel phytocannabinoids are being identified. Many of these compounds exhibit molecular chirality due to the presence of one or more stereogenic centers in their structures. Given the pharmacological and toxicological relevance of chiral molecules, regulatory authorities are expected to demand more stringent analytical characterization of the enantiomeric composition of phytocannabinoids in <i>C. sativa</i> L. extracts. The growing availability and enhanced performance of advanced analytical technologies, particularly chiral chromatographic systems, have renewed interest in the stereochemical profiling of these natural products. Chiral separation techniques have become central to research efforts aimed at determining enantiomeric purity and understanding stereoisomeric distributions in complex plant matrices. Among the limited studies addressing chiral chromatographic methods for separating phytocannabinoid enantiomers and diastereomers, two techniques are predominant: high-performance liquid chromatography (HPLC) and supercritical fluid chromatography (SFC). Method development in both approaches typically relies on two major classes of chiral stationary phases (CSPs). The first comprises Pirkle-type CSPs, which utilize the “Inverted Chirality Columns Approach” (ICCA) and are based on rational design principles for enantioselective interactions. The second group includes polysaccharide-based CSPs employing cellulose or amylose derivatives, recognized for their broad applicability in resolving diverse phytocannabinoid enantiomers. This work will review a selection of recent, representative studies, highlighting key analytical strategies for chiral separation, methodological challenges, and implications for both scientific research and regulatory frameworks.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 8","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144773925","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":"Development and Validation of a Headspace Gas Chromatography–Mass Spectrometry Method for the Identification and Quantification of Glycol Ethers in Cosmetic Cream Formulations","authors":"Imane Mecheri,&nbsp;Rachid Djafer,&nbsp;Mohamed Dammak,&nbsp;Rahma Ben Slama,&nbsp;Mohamed Habib Belmahi","doi":"10.1002/jssc.70243","DOIUrl":"10.1002/jssc.70243","url":null,"abstract":"<div>\u0000 \u0000 <p>An analytical method was developed and validated for the simultaneous detection of four glycol ethers in cosmetic creams using headspace gas chromatography coupled with mass spectrometry (HS-GC–MS). Samples were extracted with ethanol and then subjected to vortexing and ultrasonic treatment prior to analysis. The analytes showed good linearity within the concentration range of 25–200 µg/mL, with determination coefficients (<i>R</i>²) exceeding 0.995. Limits of detection (LOD) and quantification (LOQ) were determined for each compound. For ethylene glycol dimehyl ether (EGDME), LOD and LOQ were 1.39 and 4.00 µg/mL, respectively. For diethylene glycol monoethyl ether (DEGEE), values were 3.70 and 12.34 µg/mL. Triethylene glycol dimethyl ether (TEGDME) showed LOD and LOQ of 1.61 and 5.38 µg/mL. For phenoxyethanol (EGPhE), these limits were 4.79 and 15.95 µg/mL. Mean recovery rates ranged from 96.72% to 100.40%, and relative standard deviations (RSDs) remained below 15% across all validation procedures. The average method recovery ranged between 100.34% and 102.09%. The validation parameters, including specificity, linearity, precision, trueness, and accuracy, were found to be satisfactory.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 8","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144773627","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":"Identification of Chemical Constituents and Pharmacokinetics of Differential Phytochemicals in Crude and Salt-Processed Plantago asiatica L. by UHPLC-Q-TOF-MS","authors":"Shun Xie,&nbsp;Ying Lu,&nbsp;Weiping He,&nbsp;Weidong Li,&nbsp;Qin Wang,&nbsp;Linwei Chen","doi":"10.1002/jssc.70233","DOIUrl":"10.1002/jssc.70233","url":null,"abstract":"<div>\u0000 \u0000 <p>Plantaginis semen (PS), a traditional herbal medicine extensively utilized in China, contains bioactive compounds that exhibit notable therapeutic effects in promoting diuresis, regulating blood pressure, modulating lipid metabolism, and controlling blood glucose levels. Crude PS (CPS) and salt-processed CPS (SPS) are the two most commonly used decoction pieces of PS. The therapeutic efficacy of PS is further enhanced after salt processing, resulting in the SPS exhibiting superior pharmacological effects compared to the CPS. This study aims to explore the differences in chemical constituents between CPS and SPS in vitro. Additionally, the study seeks to compare the pharmacokinetics (PKs) of bioactive compounds after oral administration of extracts from both crude and salt-processed PS in rats. The identification results showed that there were 45 common components and six unique components between CPS extract and SPS extract. The results of multivariate statistical analysis have identified six differential components. The PK study results demonstrated that the mean plasma concentration–time profile and PK parameters of six representative components were significantly different between CPS extract and SPS extract. This study proved that salt-processed method increased the dissolution of most components and absorption of active components in PS, and revealed the material basis underlying the superior efficacy of SPS compared to CPS to some extent. This study provides a scientific foundation for the enhanced therapeutic efficacy of traditional Chinese medicine (TCM) following salt processing, elucidating how this ancient preparation method amplifies pharmacological activity through modern mechanistic insights.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 8","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144773624","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":"Development of Enhanced Separation Techniques for Oligonucleotides Utilizing Mixed-Mode Chromatography and 2D-LC/UV/MS Analysis","authors":"Jakob Haglöf,&nbsp;Jenny M. Nilsson,&nbsp;Jufang Wu Ludvigsson","doi":"10.1002/jssc.70238","DOIUrl":"https://doi.org/10.1002/jssc.70238","url":null,"abstract":"<p>Oligonucleotides are traditionally analyzed using ion-pair reversed-phase liquid chromatography. In this project, we explored an alternative approach utilizing a reversed phase-weak anion exchange mixed-mode column, which combines separation based on both charge and hydrophobicity. Our findings indicate that the mixed-mode column provided stronger retention and superior separation compared to the C18 column, eliminating the need for ion-pairing reagents. Additionally, selectivity can be adjusted using gradient pH and buffer concentration as well as acetonitrile content. However, the use of a phosphate buffer was necessary to ensure adequate retention and separation, despite its incompatibility with MS detection. To address this issue, a 2DLC-UV-qTOF setup with multiple loops was established, where the second-dimension LC, connected to the MS detector, required only an MS-compatible mobile phase. Using a HILIC-type LUNA Omega Sugar column in the second-dimension LC, the MS intensity of the heart-cut from the first dimension was increased 100-fold, allowing for the characterization of the main peak.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 8","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70238","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144773626","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":"Identification of Chemical Constituents and Pharmacokinetics of Differential Phytochemicals in Crude and Salt-Processed Plantago asiatica L. by UHPLC-Q-TOF-MS","authors":"Shun Xie,&nbsp;Ying Lu,&nbsp;Weiping He,&nbsp;Weidong Li,&nbsp;Qin Wang,&nbsp;Linwei Chen","doi":"10.1002/jssc.70233","DOIUrl":"10.1002/jssc.70233","url":null,"abstract":"<div>\u0000 \u0000 <p>Plantaginis semen (PS), a traditional herbal medicine extensively utilized in China, contains bioactive compounds that exhibit notable therapeutic effects in promoting diuresis, regulating blood pressure, modulating lipid metabolism, and controlling blood glucose levels. Crude PS (CPS) and salt-processed CPS (SPS) are the two most commonly used decoction pieces of PS. The therapeutic efficacy of PS is further enhanced after salt processing, resulting in the SPS exhibiting superior pharmacological effects compared to the CPS. This study aims to explore the differences in chemical constituents between CPS and SPS in vitro. Additionally, the study seeks to compare the pharmacokinetics (PKs) of bioactive compounds after oral administration of extracts from both crude and salt-processed PS in rats. The identification results showed that there were 45 common components and six unique components between CPS extract and SPS extract. The results of multivariate statistical analysis have identified six differential components. The PK study results demonstrated that the mean plasma concentration–time profile and PK parameters of six representative components were significantly different between CPS extract and SPS extract. This study proved that salt-processed method increased the dissolution of most components and absorption of active components in PS, and revealed the material basis underlying the superior efficacy of SPS compared to CPS to some extent. This study provides a scientific foundation for the enhanced therapeutic efficacy of traditional Chinese medicine (TCM) following salt processing, elucidating how this ancient preparation method amplifies pharmacological activity through modern mechanistic insights.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 8","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144774000","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":"Development and Validation of a Headspace Gas Chromatography–Mass Spectrometry Method for the Identification and Quantification of Glycol Ethers in Cosmetic Cream Formulations","authors":"Imane Mecheri,&nbsp;Rachid Djafer,&nbsp;Mohamed Dammak,&nbsp;Rahma Ben Slama,&nbsp;Mohamed Habib Belmahi","doi":"10.1002/jssc.70243","DOIUrl":"10.1002/jssc.70243","url":null,"abstract":"<div>\u0000 \u0000 <p>An analytical method was developed and validated for the simultaneous detection of four glycol ethers in cosmetic creams using headspace gas chromatography coupled with mass spectrometry (HS-GC–MS). Samples were extracted with ethanol and then subjected to vortexing and ultrasonic treatment prior to analysis. The analytes showed good linearity within the concentration range of 25–200 µg/mL, with determination coefficients (<i>R</i>²) exceeding 0.995. Limits of detection (LOD) and quantification (LOQ) were determined for each compound. For ethylene glycol dimehyl ether (EGDME), LOD and LOQ were 1.39 and 4.00 µg/mL, respectively. For diethylene glycol monoethyl ether (DEGEE), values were 3.70 and 12.34 µg/mL. Triethylene glycol dimethyl ether (TEGDME) showed LOD and LOQ of 1.61 and 5.38 µg/mL. For phenoxyethanol (EGPhE), these limits were 4.79 and 15.95 µg/mL. Mean recovery rates ranged from 96.72% to 100.40%, and relative standard deviations (RSDs) remained below 15% across all validation procedures. The average method recovery ranged between 100.34% and 102.09%. The validation parameters, including specificity, linearity, precision, trueness, and accuracy, were found to be satisfactory.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 8","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144773921","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 Universal Strategy for Evaluation and Quantification of Potential Genotoxic Impurities of Hydrazine Derivatives in Isoniazid Injection","authors":"Changhong Li,&nbsp;Jingjing Liu,&nbsp;Piao Liu,&nbsp;Ting Zhou,&nbsp;Guo Yin,&nbsp;Jun Chen,&nbsp;Ran Liu","doi":"10.1002/jssc.70235","DOIUrl":"https://doi.org/10.1002/jssc.70235","url":null,"abstract":"<div>\u0000 \u0000 <p>Isoniazid is an irreplaceable first-line anti-tuberculosis drug. Its synthesis requires hydrazine as a starting material, which is classified as a Class 2 genotoxic impurity according to the ICH M7 guideline. Consequently, there is a risk of introducing potential genotoxic impurities (PGIs) containing hydrazine-related alerting structural during production. This study employed a systematic approach to assess the risks of PGIs in isoniazid and developed a novel LC-MS/MS method for accurate control and quantification of these impurities. First, candidate impurities were preliminarily predicted using quantitative structure–activity relationship (QSAR) systems based on expert rule and statistics. Subsequently, acceptable impurity limits were established based on the prediction results. Finally, an LC-MS/MS method was developed to quantify the selected PGIs. The results indicated that the impurities were classified as Class 3 (3,5-bis(4-pyridyl)-4-amino-1,2,4-triazole), Class 4 (benzohydrazide, picolinohydrazide, and nicotinohydrazide), and Class 5 (3,6-di(4-pyridyl)-1,4-dihydro-1,2,4,5-tetrazine). According to the ICH Q3B guidelines and the threshold of toxicological concern (TTC) based on the duration of administration, the limits of Class 4 and 5 impurities were set at 0.1%, and the limit of Class 3 impurities was set at 0.0066%. The established method demonstrated excellent linearity (<i>r</i> &gt; 0.999) within the range of 0.2-25 ng/mL. And good recoveries were observed in the range of 88.1%–113.0%. The method was successfully applied to quantify impurities in 77 batches of isoniazid injections, all of which complied with the established acceptance limits. This universal strategy enhances quality control of isoniazid formulations, ensuring clinical safety through robust impurity assessment and validated analytical methodology.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 8","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144740517","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 Universal Strategy for Evaluation and Quantification of Potential Genotoxic Impurities of Hydrazine Derivatives in Isoniazid Injection","authors":"Changhong Li,&nbsp;Jingjing Liu,&nbsp;Piao Liu,&nbsp;Ting Zhou,&nbsp;Guo Yin,&nbsp;Jun Chen,&nbsp;Ran Liu","doi":"10.1002/jssc.70235","DOIUrl":"10.1002/jssc.70235","url":null,"abstract":"<div>\u0000 \u0000 <p>Isoniazid is an irreplaceable first-line anti-tuberculosis drug. Its synthesis requires hydrazine as a starting material, which is classified as a Class 2 genotoxic impurity according to the ICH M7 guideline. Consequently, there is a risk of introducing potential genotoxic impurities (PGIs) containing hydrazine-related alerting structural during production. This study employed a systematic approach to assess the risks of PGIs in isoniazid and developed a novel LC-MS/MS method for accurate control and quantification of these impurities. First, candidate impurities were preliminarily predicted using quantitative structure–activity relationship (QSAR) systems based on expert rule and statistics. Subsequently, acceptable impurity limits were established based on the prediction results. Finally, an LC-MS/MS method was developed to quantify the selected PGIs. The results indicated that the impurities were classified as Class 3 (3,5-bis(4-pyridyl)-4-amino-1,2,4-triazole), Class 4 (benzohydrazide, picolinohydrazide, and nicotinohydrazide), and Class 5 (3,6-di(4-pyridyl)-1,4-dihydro-1,2,4,5-tetrazine). According to the ICH Q3B guidelines and the threshold of toxicological concern (TTC) based on the duration of administration, the limits of Class 4 and 5 impurities were set at 0.1%, and the limit of Class 3 impurities was set at 0.0066%. The established method demonstrated excellent linearity (<i>r</i> &gt; 0.999) within the range of 0.2-25 ng/mL. And good recoveries were observed in the range of 88.1%–113.0%. The method was successfully applied to quantify impurities in 77 batches of isoniazid injections, all of which complied with the established acceptance limits. This universal strategy enhances quality control of isoniazid formulations, ensuring clinical safety through robust impurity assessment and validated analytical methodology.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 8","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144740515","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":"Rapid and Preparative Separation of Polyphenols From Pods of Paeonia suffruticosa Andr. By Elution-Extrusion Counter-Current Chromatography Coupled With Inner-Recycling Mode","authors":"Xiuheng Qin,&nbsp;Li Xu,&nbsp;Yufa Zhang,&nbsp;Huijiao Yan,&nbsp;Ammara Sohail,&nbsp;Wenshuang Zhao,&nbsp;Daijie Wang,&nbsp;Chao Ma,&nbsp;Li Cui","doi":"10.1002/jssc.70207","DOIUrl":"10.1002/jssc.70207","url":null,"abstract":"<div>\u0000 \u0000 <p>Pods of <i>Paeonia suffruticosa</i> Andr. are a good source of natural plants and have drawn a lot of interest in order to increase their overall utility value. In this study, elution-extrusion counter-current chromatography coupled with inner-recycling mode was used to successfully extract the polyphenols from <i>Paeonia suffruticosa</i> Andr. pods. Eight compounds, including (1) methyl gallate, (2) 1,2,3,4, 6-trigalloyl-<i>β</i>-<span>d</span>-glucose, (3) methyl digallate (meta- and para- isomers), (4) 4-<i>O</i>-digalloyl-1,2,3,6-tetra-<i>O</i>- galloyl-<i>β</i>-<span>d</span>-glucose, (5) 3-<i>O</i>-digalloyl-1,2,3,6-tetra-<i>O</i>-galloyl-<i>β</i>-<span>d</span>-glucose, (6) (+)-<i>ε</i>-viniferin, (7) amurensin B and (8) gnetin H, were effectively isolated. Structural characterization was performed by nuclear magnetic resonance spectrometry and mass spectrometry. Based on our research, the developed process was a successful way to separate the polyphenols with a broad and similar partition coefficient from pods of <i>Paeonia suffruticosa</i> Andr. It could be used to separate the polyphenols from complicated natural products with the established method.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144647175","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":"Flow Injection Inductively Coupled Plasma-Mass Spectrometry With Ultrasonic Nebulizer for the Quantification of Trace Elements in Seawater: An Innovative Method Targeting Cadmium, Cobalt, Lead, Manganese, Molybdenum, Tin, Uranium, and Vanadium","authors":"Giorgia Mattei,&nbsp;Clara Sette,&nbsp;Luca Lucentini,&nbsp;Enrico Veschetti","doi":"10.1002/jssc.70228","DOIUrl":"https://doi.org/10.1002/jssc.70228","url":null,"abstract":"<p>The accurate determination of trace elements in seawater is essential for environmental monitoring and the study of oceanic biogeochemical processes. However, traditional analytical techniques often face limitations due to the ultra-trace concentrations of metals and the high salinity of seawater, which introduces significant matrix effects. In this study, a novel flow injection—inductively coupled plasma mass spectrometry (FI-ICP-MS) method coupled with an ultrasonic nebulizer was developed and optimized for the direct quantification of cadmium, cobalt, lead, manganese, molybdenum, tin, uranium, and vanadium in seawater samples. The method was optimized by evaluating the effects of eluent concentration (0.05–0.20% HNO3, with 0.05% selected as the minimum effective value to ensure analyte stability, prevent precipitation, and minimize salt-related stress on the FI system), flow rate (0.4–1.0 mL/min), and sodium chloride matrix composition, ensuring minimal spectral interferences while maintaining high sensitivity. The selected operating conditions (0.05% HNO3 eluent at 0.70 mL/min with 103Rhodium and 193Iridium as internal standards) provided a robust analytical performance with low procedural limits of detection and quantification (ranging from 0.003 to 0.2 µg/L for LoDs and from 0.01 to 0.7 µg/L for LoQs) and excellent instrumental repeatability (1.2%–6.6%). The overall method was validated using the IAEA-443 seawater certified reference material, yielding recoveries between 104%–118% and procedural reproducibility ranging from 3.8% to 15%.</p><p>The optimized FI-ICP-MS method was applied to real seawater samples collected from two distinct Mediterranean transects: offshore Livorno, a site influenced by intense maritime and industrial activities, and Montecristo Island, a protected marine reserve with minimal anthropogenic impact. Results indicated no significant differences in trace metal concentrations between the two areas, suggesting that natural geochemical processes predominantly regulate elemental distributions. Most elements followed a conservative vertical distribution, with localized anomalies observed for manganese and cadmium. Furthermore, all measured cadmium and lead concentrations were well below the regulatory thresholds set by Directive 2013/39/EU, confirming compliance with environmental quality standards.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70228","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144647230","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}