{"title":"Critical review on the assessments of green metric tools for Olmesartan medoxomil analytical methods: Case studies","authors":"Shaikh Manirul Haque , Abuzar Kabir","doi":"10.1016/j.jcoa.2025.100242","DOIUrl":"10.1016/j.jcoa.2025.100242","url":null,"abstract":"<div><div>Green chemistry metrics can incorporate features of analytical practices that adhere to the principles of green chemistry. Several metrics are available to evaluate the greenness of the analytical procedure, including the AES, AGREE, and BAGI. The current review article outlines the selected metrics used to determine case studies of Olmesartan, employing various analytical techniques, including UV spectrophotometry, HPLC, HPTLC, UPLC, LC-MS, and UPLC-MS, based on specific criteria. These criteria also include the advantages, disadvantages, and limitations of each technique. The analytical eco–scale, AGREE and BAGI values were in the range 79–86, 72–84, 66–68, 77, 75–89, 67–75; 0.6–0.71, 0.55–0.65, 0.58–0.65, 0.62, 0.65–0.66, 0.68–0.69; 77.5–82.5, 72.5–82.5; 75–77.5, 80, 75 – 80 and 80 respectively for UV spectrophotometry, HPLC, HPTLC, UPLC, LC-MS and UPLC-MS. The results are well-organised according to the criteria and have produced an excellent greener methodology. The new researchers could understand and use all the assessment tools for different purposes. Additionally, they can utilise it to develop new procedures, which could demonstrate a greener methodology for quantifying Olmesartan in various matrices.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100242"},"PeriodicalIF":0.0,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144686445","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Allan Polidoro , Valentina Costa , Monica Romagnoli , Elena Sarti , Claudia Stevanin , Cinzia Fabbro , Luisa Pasti , Flavio A. Franchina
{"title":"Multitargeted analysis for the simultaneous determination of organochlorine pesticides and polychlorinated biphenyls in sediments exploiting comprehensive two-dimensional gas chromatography coupled to mass spectrometry","authors":"Allan Polidoro , Valentina Costa , Monica Romagnoli , Elena Sarti , Claudia Stevanin , Cinzia Fabbro , Luisa Pasti , Flavio A. Franchina","doi":"10.1016/j.jcoa.2025.100245","DOIUrl":"10.1016/j.jcoa.2025.100245","url":null,"abstract":"<div><div>Persistent organic pollutants (POPs), including organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs), remain a significant environmental concern due to their persistence, bioaccumulation, and toxicity. Accurate quantification of these contaminants in sediment matrices remains analytically challenging due to the complexity of the matrix and the need for detection at trace levels to meet regulatory standards. This research focused on the development and application of an analytical protocol for the simultaneous determination of OCPs and PCBs in sediments using solid-phase extraction (SPE) followed by comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC×GC-TOFMS). The developed method was validated, achieving low limits of detection (0.4 to 14 ng kg<sup>-1</sup>) and quantification (1.1 to 41 ng kg<sup>-1</sup>), with satisfactory linearity (r² > 0.99), accuracy (90–110%), and precision (RSD < 5%) for all target analytes. Validation with certified reference material confirmed the agreement between experimental and certified concentrations for most compounds. The protocol was applied to environmental sediment samples, detecting multiple PCBs and DDT-related compounds at concentrations below international guideline values. These results confirm the method’s suitability for trace-level determination of OCPs and PCBs in sediments, addressing the analytical demands of environmental monitoring and regulatory compliance. The established protocol enables sensitive and reliable assessment of sediment contamination, supporting a simultaneous ongoing surveillance and risk assessment of such classes of persistent organic pollutants in the same analytical run.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100245"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144842201","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Susanna Della Posta, Vittoria Terrigno, Maria Chiara Frondaroli, Laura De Gara, Chiara Fanali
{"title":"Use of a deep eutectic solvent-assisted matrix solid-phase dispersion extraction for phenolic compounds determination from pigmented wheat","authors":"Susanna Della Posta, Vittoria Terrigno, Maria Chiara Frondaroli, Laura De Gara, Chiara Fanali","doi":"10.1016/j.jcoa.2025.100282","DOIUrl":"10.1016/j.jcoa.2025.100282","url":null,"abstract":"<div><div>In this study, an innovative extraction method for the determination of phenolic compounds in pigmented wheat was developed and optimized. Using deep eutectic solvents (DESs), a greener alternative extraction procedure is offered to the conventional ones based on organic solvents. A matrix solid-phase dispersion (MSPD) extraction was performed and enhanced by the addition of DES in the homogenization step. In comparison with an ultrasound-assisted solid liquid extraction, the MSPD-DES technique allowed to obtain a higher extraction efficiency reducing organic solvent consumption and environmental impact. Although different DESs were tested, the one based on choline chloride and glycerol (1:2 molar ratio) showed the best extraction yield of phenolic compounds. A three-level four-factor Box-Behnken design optimization was performed: sample-to-dispersing material ratio, DES volume, extraction solvent volume, and number of cycles were evaluated. Under the optimal conditions a total phenolic content (TPC) of 3.562 ± 0.005 mg GAE/g was achieved. The AGREEprep, BAGI, and ComplexMoGAPI indicators confirmed the environmental sustainability of the proposed methodology. The qualitative profile of the extracted phenolic compounds was determined using high-performance liquid chromatography-photodiode array detector.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100282"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145473941","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Şeyda Yayla , Ahmet Cetinkaya , M․Mesud Hurkul , Sibel A. Ozkan
{"title":"Recent advances in green chromatography techniques for natural product analysis","authors":"Şeyda Yayla , Ahmet Cetinkaya , M․Mesud Hurkul , Sibel A. Ozkan","doi":"10.1016/j.jcoa.2025.100284","DOIUrl":"10.1016/j.jcoa.2025.100284","url":null,"abstract":"<div><div>New developments in green chromatography (GrCh) techniques have helped scientists to study natural products. These developments have done two important things. First, they have made it possible to align analytical methods with sustainability and environmental safety principles. At the same time, accurate and reliable traditional chromatography methods are often heavily reliant on toxic organic solvents and energy-intensive procedures, with ecological and health risks being posed as a result. To address these concerns, researchers have developed various environmentally friendly approaches that reduce solvent consumption, waste generation, and energy demand. One of the most significant advancements is Supercritical Fluid Chromatography (SFC), which utilises carbon dioxide as a non-toxic and reusable mobile phase, greatly minimising the use of harmful solvents. The popularity of Micellar Liquid Chromatography (MLC) and High-Performance Thin Layer Chromatography (HPTLC) has grown thanks to their ability to minimise solvent use and provide miniaturised and efficient separations. Natural Deep Eutectic Solvents (NADES) are emerging as green alternatives for extraction and sample preparation, offering biodegradability and low toxicity.</div><div>Additionally, microextraction techniques are being used to reduce both solvent and sample volume requirements. Examples of microextraction techniques include Solid Phase Microextraction (SPME) and Liquid Phase Microextraction (LPME). The combination of online extraction and real-time detection systems increases the amount of analysis done while protecting the environment. These GrCh strategies hold great promise. They are suitable for the qualitative and quantitative analysis of plant-derived compounds. Examples of these compounds include flavonoids, alkaloids, terpenes, and phenolics. These methods provide high analytical performance with a lower ecological footprint when used in conjunction with advanced detection systems such as LC-MS/MS and GC–MS under optimised, environmentally friendly conditions. Overall, the way is paved for more responsible and sustainable practices in natural product research by GrCh.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100284"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145528215","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Vacuum-assisted headspace solid-phase microextraction for volatile profiling of avocado puree: Application to post-harvest ripening","authors":"Angeliki Pateraki , Breno Jorge Pollo , Fabio Augusto , Elefteria Psillakis","doi":"10.1016/j.jcoa.2025.100274","DOIUrl":"10.1016/j.jcoa.2025.100274","url":null,"abstract":"<div><div>Vacuum-assisted headspace solid-phase microextraction (Vac-HS-SPME) was developed and applied for the first time to monitor free volatile emissions during post-harvest ripening of Hass and Fuerte avocados. The parameters of extraction time and temperature were optimized using 24 analytes identified in unripe Hass puree. Through this optimization, the advantages of vacuum conditions were confirmed by comparing Vac-HS-SPME with conventional headspace solid-phase microextraction (HS-SPME). Vacuum conditions improved the extraction of sesquiterpenes and enabled the unique detection of octanal and (Z)-2-octen-1-ol under milder conditions. Under optimal conditions (30 min at 40 °C), Vac-HS-SPME successfully revealed cultivar-specific and ripening-related changes in volatile profiles. At the unripe stage, Fuerte showed higher relative abundances of sesquiterpenes compared to Hass, while (E)-2-heptenal, hexyl acetate and β-bisabolene were detected exclusively in unripe Hass. Ripening was associated with a marked reduction in sesquiterpenes, alcohols, and higher molecular weight aldehydes. The decline of sesquiterpenes is likely driven by the increasing oil content of the mesocarp during ripening, as lipophilic compounds preferentially remain in the lipid matrix rather than partitioning into the headspace. Aldehydes such as hexanal and (E)-2-hexenal became dominant at the ripe stage, and both cultivars displayed similar profiles. Overall, this study demonstrates that Vac-HS-SPME is a powerful and robust method for monitoring volatile changes in avocado ripening, with potential applications in harvest, storage, and quality management.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100274"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145361930","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Editorial on “Tutorial 2024” virtual special issue","authors":"Sanka N. Atapattu","doi":"10.1016/j.jcoa.2025.100237","DOIUrl":"10.1016/j.jcoa.2025.100237","url":null,"abstract":"","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100237"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145693500","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Bin Yang , Myriam Taverna , Cédric Y. Montanier , Zhengjin Jiang , N. Thuy Tran
{"title":"Rapid O-glycan release from glycoproteins using a monolith-based glycosidase microreactor","authors":"Bin Yang , Myriam Taverna , Cédric Y. Montanier , Zhengjin Jiang , N. Thuy Tran","doi":"10.1016/j.jcoa.2025.100269","DOIUrl":"10.1016/j.jcoa.2025.100269","url":null,"abstract":"<div><div>Fast, efficient and simple selective <em>O</em>-glycan release methods are urgently needed for accurately analyzing <em>O</em>-glycans of therapeutic proteins or glycosylation-based biomarkers. In this study, a polymeric monolith-based microreactor with immobilized <em>O</em>-glycosidase inside a capillary has been developed. The photopolymerization of a poly (glycidyl methacrylate-<em>co</em>-poly (ethylene glycol) diacrylate) monolith in a capillary with tens of nanoliters volume (50 μm I.D. × 1 cm) was optimized. It exhibited a relatively high permeability (2.29 × 10<sup>–13</sup> m<sup>2</sup>), and good mechanical and chemical stabilities. Two different immobilization chemistries to attach <em>O</em>-glycosidase and several digestion protocols were tested and compared. We showed that Shiff base and Epoxy chemistries for <em>O</em>-glycosidase immobilization led to similar digestion efficiencies regarding the quantity of released <em>O</em>-glycans. The performance of the immobilized enzyme reactor (IMER) was assessed on asialofetuin used as a substrate for the release of <em>O</em>-glycans. In-IMER digestion was able to release 56 % of <em>O</em>-glycans in <3 s, while the enzyme in-solution digestion required at least one hour to achieve the same release efficiency. The capillary format monolith proves the route to fulfil on-line coupling between <em>O</em>-glycan release and glycan separation analysis.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100269"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145264956","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Carmela Maria Montone , Nina Felli , Massimo Giuseppe De Cesaris , Lorenzo Antonelli , Tecla Gasperi , Maria Bianchi , Patrizia Papacci , Luciana Teofili , Salvatore Fanali , Alessandra Gentili
{"title":"An analytical methodology for the quantitative profiling of fat-soluble antioxidants in maternal blood, umbilical cord blood and meconium","authors":"Carmela Maria Montone , Nina Felli , Massimo Giuseppe De Cesaris , Lorenzo Antonelli , Tecla Gasperi , Maria Bianchi , Patrizia Papacci , Luciana Teofili , Salvatore Fanali , Alessandra Gentili","doi":"10.1016/j.jcoa.2025.100253","DOIUrl":"10.1016/j.jcoa.2025.100253","url":null,"abstract":"<div><div>The determination of fat-soluble antioxidants represents a significant analytical challenge, particularly when dealing with biological matrices available only in limited quantities, such as those collected from preterm infants. This paper presents the development, validation, and application of a multianalyte high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for the determination of 21 fat-soluble antioxidants (including vitamins and carotenoids) in meconium, cord plasma, and maternal plasma samples. All the analytes were separated by non-aqueous reversed phase chromatography, detected by atmospheric pressure chemical ionization, acquiring in Scheduled/Multiple Reaction Monitoring mode to improve sensitivity. Their extraction was performed with hexane, after protein precipitation with cold ethanol, followed by a “lipid freezing” clean-up. Recoveries ranged between 63 and 100 % with relative standard deviations ≤ 18 %. For all matrices, limits of detection and lower limits of quantitation were in the ppb and ppm-ppb range, respectively. The developed approach enabled the study of the distribution of 21 fat-soluble antioxidants, which play a protective role against oxidative stress at various levels within the human body. To better interpret the data obtained from an unconventional matrix such as meconium, the results were compared with those from cord plasma and maternal plasma, revealing, in most cases, a common trend across the 24 cases under study.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100253"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145010210","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Y Jin , A Thomas , S Gochard , P Delahaut , M Thevis
{"title":"Metabolite patterns of the carbonic anhydrase inhibitors brinzolamide and dorzolamide: potential markers for the route of application","authors":"Y Jin , A Thomas , S Gochard , P Delahaut , M Thevis","doi":"10.1016/j.jcoa.2025.100236","DOIUrl":"10.1016/j.jcoa.2025.100236","url":null,"abstract":"<div><div>Brinzolamide (BA) and dorzolamide (DA) are carbonic anhydrase inhibitors (CAIs), and are commonly used therapeutics for glaucoma treatment via topical application. According to the regulations of the World Anti-Doping Agency (WADA), both drugs are classified under \"Diuretics and Masking Agents\", prohibiting their use in- and out-of-competition, except for ophthalmic application. Despite ophthalmic use being permitted, systemic absorption occurs, enabling BA and DA detection in blood and urine samples after topical administration. Thus, distinguishing between legitimate (e.g. topical) and prohibited (e.g. oral) drug application routes is critical for sports drug testing result management.</div><div>This study investigated the elimination and metabolic profiles of BA and DA following topical and systemic administration in male piglets. Three piglets received BA or DA ophthalmic suspensions, while another three received an oral dose. Urine and blood samples were collected over one week, and all samples were analysed using liquid chromatography-high-resolution tandem mass spectrometry (LC<img>HRMS MS). In vitro experiments yielded five phase I metabolites for DA and BA. After method validation, the approach was confirmed to detect DA and BA, with Limits of Detection (LODs) of 55 pg/mL and 75 pg/mL in urine, 110 pg/mL and 180 pg/mL in red blood cells, and 380 pg/mL and 910 pg/mL in plasma. BA and DA metabolites were primarily found in the red blood cell fraction, with only trace amounts detectable in plasma. N-desethylation was observed as the main metabolic reaction for both drugs, and metabolite-to-parent drug ratios were determined in all collected post-administration samples alongside drug concentration levels. The combined consideration of analyte ratios and drug concentrations appears to be indicative of time and dose of drug use (under the chosen routes of administration), which might assist in sports drug testing result management.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100236"},"PeriodicalIF":0.0,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144563681","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}