Green Analytical Chemistry最新文献

{"title":"Green sampling of gas-phase volatile organic compounds using time-weighted average solid phase microextraction and gas chromatography - mass spectrometry: A critical review","authors":"Shokouh Haddadi ,&nbsp;Jacek A. Koziel ,&nbsp;Bulat Kenessov","doi":"10.1016/j.greeac.2025.100302","DOIUrl":"10.1016/j.greeac.2025.100302","url":null,"abstract":"<div><div>Time-weighted average solid-phase microextraction (TWA-SPME) is a solvent-free passive sampling technique increasingly applied to volatile organic compounds (VOCs) monitoring in air. This review critically examines the theoretical foundations of TWA-SPME based on Fick’s laws of diffusion, highlights optimization of SPME coating, diffusion path length, and sampling duration, and compares quantification strategies based on both theoretical modeling and empirical calibration. Applications across ambient and indoor air, vehicle exhaust, industrial emissions, and clinical environments demonstrate their versatility and sensitivity relative to conventional sorbent-based methods. A greenness evaluation using the AGREEprep tool confirmed strong TWA-SPME alignment with green sampling preparation principles, particularly through elimination of solvents, low waste, and high operator safety. Challenges such as adsorption on metallic components and coating saturation are discussed alongside mitigation strategies and device refinements. Emerging designs and simulation-based models improve performance predictability and sampling efficiency under diverse environmental conditions. Comparisons with emerging alternatives such as thin-film SPME and needle trap devices highlight the unique advantages of TWA-SPME in robustness, simplicity, and reproducibility. Overall, TWA-SPME represents an environmentally friendly, accurate, and practical approach to VOC sampling, with growing relevance in environmental monitoring and occupational exposure assessments.</div></div>","PeriodicalId":100594,"journal":{"name":"Green Analytical Chemistry","volume":"15 ","pages":"Article 100302"},"PeriodicalIF":6.2,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145266964","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":"Hydrogen vs. Helium as carrier gases in GC-MS/MS for pesticide residue analysis: a comparative evaluation","authors":"Víctor Cutillas,&nbsp;José Antonio Martínez-Martínez,&nbsp;Carmen Ferrer,&nbsp;Amadeo R. Fernández-Alba","doi":"10.1016/j.greeac.2025.100300","DOIUrl":"10.1016/j.greeac.2025.100300","url":null,"abstract":"<div><div>This study presents a comprehensive comparison between helium and hydrogen as carrier gases in gas chromatography coupled with tandem mass spectrometry (GC-MS/MS) for multiresidue pesticide analysis. Using a shared instrumental platform, method parameters were carefully adapted for each carrier gas to maintain equivalent chromatographic efficiency, including adjustments to column dimensions, flow rates, and oven temperature programs. Method performance was evaluated in terms of chromatographic resolution, sensitivity, matrix effects, and regulatory reliability across tomato, pepper, and zucchini matrices. Hydrogen demonstrated faster analysis times and improved resolution in several cases, particularly in separating matrix interferences. However, helium consistently offered higher sensitivity, especially at lower concentrations. At 2 µg/kg, helium enabled the identification of over 90 % of compounds in most matrices, while hydrogen remained below 55 %. Matrix effect evaluations showed slightly better results with helium, though both gases provided acceptable performance, with most compounds falling within the negligible effect range. A proficiency test sample further validated the method, confirming that both gases produced results within acceptable z-score limits. Overall, hydrogen proved to be a viable and sustainable alternative for routine applications, though helium remains preferable when ultra-trace sensitivity or method robustness under stricter regulatory conditions is required.</div></div>","PeriodicalId":100594,"journal":{"name":"Green Analytical Chemistry","volume":"15 ","pages":"Article 100300"},"PeriodicalIF":6.2,"publicationDate":"2025-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145220951","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":"Identification and quantification of microplastics in a wide range of aqueous matrices using pyrolysis-gas chromatography-mass spectrometry: method’s performance, greenness evaluation, and analysis of real samples","authors":"Giulia Bonaccorso ,&nbsp;Simone Bonari ,&nbsp;Paolo Bini ,&nbsp;Christine Savorgianaki ,&nbsp;Lapo Renai ,&nbsp;Michelangelo Fichera ,&nbsp;Donatella Fibbi ,&nbsp;Daniela Santianni ,&nbsp;Claudia Bello ,&nbsp;Anna Maria Papini ,&nbsp;Massimo Del Bubba","doi":"10.1016/j.greeac.2025.100301","DOIUrl":"10.1016/j.greeac.2025.100301","url":null,"abstract":"<div><div>This study describes the analysis of microplastics in aqueous matrices of varying complexity using pyrolysis coupled with gas chromatography-mass spectrometry (Py-GC–MS). Depending on the filtration rate of the analysed matrix, sample treatment prior to Py-GC–MS consisted of filtration on 0.7 µm glass fibre membranes (low-complexity matrices), or microwave-assisted digestion of samples with hydrogen peroxide, followed by filtration as above-mentioned (high-complexity matrices). Low-complexity matrices included demineralised water (DMW), mineral water in polyethylene terephthalate (PET) bottles (BMW), drinking water from a public aqueduct (DW), and DW further treated with activated carbon and distributed in public fountains (FOW). High-complexity matrices included effluent wastewater from primary sedimentation (WW-PS), biological oxidation (WW-BO), clariflocculation (WW-CL), and quaternary treatment (WW-QT). Sample digestion significantly accelerated the filtration process of high-complexity matrices. In most cases, absolute value of matrix effect was &lt;40 %, except for PET in WW-PS (-54 %) and WW-CL (-56 %), and polystyrene in WW-PS (75 %). Apparent recovery, studied in DMW, DW, and WW-BO matrices, was 90±24, 87±25, and 67±19, respectively. The methods were evaluated for their greenness, achieving scores higher than or comparable to those of previously published Py-GC–MS procedures. Poly(methyl methacrylate) and PET were never detected, while different levels of contamination were found for polystyrene, polyethylene, polypropylene, polycarbonate, polyamide, and polyvinyl chloride, depending on the sample type. The lowest contaminations were determined in BMW and DMW. FOW was more contaminated than DW (five microplastics detected at 2.7–138 µg/L vs. two microplastics detected at &lt;0.62–23 µg/L) and concentrations in WWs were in the order WW-QT&lt;WW-CL&lt;WW-PS&lt;&lt;WW-BO.</div></div>","PeriodicalId":100594,"journal":{"name":"Green Analytical Chemistry","volume":"15 ","pages":"Article 100301"},"PeriodicalIF":6.2,"publicationDate":"2025-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145266966","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":"Greenness-assessed RP-HPLC method for budesonide quantification in layer-by-layer polymeric nanoparticles: Validation, stability, and controlled release in colonic delivery","authors":"Giriprasath Ramanathan ,&nbsp;Masroora Hassan ,&nbsp;Yury Rochev","doi":"10.1016/j.greeac.2025.100299","DOIUrl":"10.1016/j.greeac.2025.100299","url":null,"abstract":"<div><div>Robust and sustainable analytical tools are essential for the design, manufacture, and evaluation of advanced drug delivery systems. This study reports the first validated reversed-phase high-performance liquid chromatography (RP-HPLC) method for quantifying budesonide encapsulated within poly(lactic-co-glycolic acid) (PLGA)-based, layer-by-layer (LbL) coated nanoparticles intended for colonic delivery in inflammatory bowel disease (IBD). Using response surface methodology with a central composite design, optimal conditions were identified as acetonitrile:water (80:20, v/v) under isocratic mode, achieving complete separation within 5 min at a flow rate of 0.34 mL min^-1 and detection at 242 nm. The method is buffer-free, rapid, and solvent-efficient, resulting in a favorable greenness profile, further confirmed by GAPI and NEMI assessments. Validation in line with ICH Q2(R2) demonstrated excellent linearity (R² &gt; 0.999), precision (% RSD &lt; 2 %), accuracy, specificity, and sensitivity (LOD: 0.04 µg mL^-1; LOQ: 1.2 µg mL^-1). Forced degradation studies under acidic, alkaline, oxidative, thermal, photolytic, and photostatic conditions showed that the LbL coating markedly enhanced drug stability, particularly against thermal and photostatic stress, while &gt;75 % degradation occurred in alkaline and oxidative environments. In vitro release profiling under simulated gastrointestinal conditions demonstrated sustained, pH-responsive release (20.6 % over 48 h), consistent with colonic targeting. This validated, green, and stability-indicating method integrates controlled release assessment with comprehensive performance evaluation, providing a versatile platform for quality control of nanoparticulate drug delivery systems and supporting their progression from formulation development to clinical translation.</div></div>","PeriodicalId":100594,"journal":{"name":"Green Analytical Chemistry","volume":"15 ","pages":"Article 100299"},"PeriodicalIF":6.2,"publicationDate":"2025-09-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145096805","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":"Agri-food waste biochar-based green vial wall sorptive extraction: Downscaled portable device for steroids in fresh and brackish water samples","authors":"Francesca Merlo,&nbsp;Lorenzo Tassi,&nbsp;Chiara Milanese,&nbsp;Antonella Profumo,&nbsp;Andrea Speltini","doi":"10.1016/j.greeac.2025.100298","DOIUrl":"10.1016/j.greeac.2025.100298","url":null,"abstract":"<div><div>A biochar-based vial wall sorptive extraction (VWSE) was developed for multiclass steroid determination in waters. Coupling biochar with this user-friendly but still undervalued extraction technique provided a green sample preparation functional to HPLC-MS/MS quantification. Among the biochar samples prepared from different vegetal wastes, the most promising in terms of sorption affinity was obtained by pyrolysis of pumpkin peels under optimized conditions (650 °C, 4 h), which yielded a sorbent endowed with polar groups. After immobilization on the inner wall of small sampling tubes, the uptake of steroids was first investigated in potable water. The coated vial provided good extraction efficiency (90 min orbital shaking) not only for sex steroids but also for glucocorticoids (logP 1.9–2.5) possibly due to interaction with biochar oxygenated groups. The uptake of the 17 targets joined to pre-concentration allowed determination of these contaminants at environment-relevant concentrations, using only 10 mL samples. The possibility of sampling and extraction on-site in the same container coupled with the good sorption behaviour followed by quick (10 min) and exhaustive elution in 2.5 mL ethanol, a safe and green solvent, make the procedure green, with a streamlined workflow showing good throughput (15 samples treated simultaneously). Recoveries in the range ∼65 %-120 % (40 %-108 % for glucocorticoids) were obtained in tap, lake, river, lagoon water and wastewater treatment plant effluent samples, with inter-day inter-batch device-to-device RSD &lt; 19 % (<em>n</em> <em>=</em> <em>3</em>). The coated-vial was reusable for at least 20 samples contributing to the positive greenness scores obtained through specific metrics.</div></div>","PeriodicalId":100594,"journal":{"name":"Green Analytical Chemistry","volume":"15 ","pages":"Article 100298"},"PeriodicalIF":6.2,"publicationDate":"2025-09-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145096804","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":"Portable HS-SPME-GC-MS combined with machine learning for onsite detection of huanglongbing-infected navel orange leaves at high-altitude environments","authors":"Jiafan Yang ,&nbsp;Jianfeng Zhang ,&nbsp;Wenqi Mo ,&nbsp;Ximeng Liu ,&nbsp;Xuan Liu ,&nbsp;Yang Yang ,&nbsp;Bin Hu","doi":"10.1016/j.greeac.2025.100297","DOIUrl":"10.1016/j.greeac.2025.100297","url":null,"abstract":"<div><div>Huanglongbing (HLB) remains one of the most destructive diseases threatening global citrus production, with its impact exacerbated in diverse altitudinal environments where environmental conditions can influence disease progression and diagnostic accuracy. In this study, we applied headspace solid-phase microextraction (HS-SPME) coupled with portable gas chromatography-mass spectrometry (GC–MS) to analyze volatile profiles of orange leaves from healthy and asymptomatic HLB-infected trees at different altitudes. A comprehensive machine learning (ML) framework, comprising random forest, logistic regression, XGBoost, support vector machine, and Ensemble classifier, was then used to achieve accurate discrimination between infection states and to identify altitude-dependent shifts in key metabolites such as limonene, 3-carene, and citronellal. The results revealed that the abundance of HLB-infected metabolites varied with altitude, indicating that environmental factors should be considered when selecting robust biomarkers for disease diagnosis. This portable analytical platform enables rapid and reliable detection of HLB under varying environmental conditions, providing a practical tool for precision agriculture and advancing the understanding of citrus metabolic responses to biotic (HLB) and abiotic (altitude) stresses.</div></div>","PeriodicalId":100594,"journal":{"name":"Green Analytical Chemistry","volume":"15 ","pages":"Article 100297"},"PeriodicalIF":6.2,"publicationDate":"2025-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145049128","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":"Green solvents in microextraction of pharmaceuticals: Application and comparison of deep eutectic solvents and ionic liquids","authors":"Sahar Shokouh ,&nbsp;Seyed Mosayeb Daryanavard ,&nbsp;Foad Mashayekhi Suzaei ,&nbsp;Adrián Fuente-Ballesteros ,&nbsp;Chalermpong Saenjum","doi":"10.1016/j.greeac.2025.100296","DOIUrl":"10.1016/j.greeac.2025.100296","url":null,"abstract":"<div><div>Forward-looking, sustainable, and green approaches in analytical chemistry have become a significant topic worldwide. This has attracted considerable attention from scientists in improving methods for analyzing a broad area of analytes and samples, such as pharmaceuticals in biological matrices. These enhancements generally adhere to principles of Green Chemistry (GC) and Green Analytical Chemistry (GAC). To align with these principles, utilizing green materials and solvents, such as deep eutectic solvents (DESs) and ionic liquids (ILs), has proven to be highly effective in making analytical chemistry approaches more environmentally friendly. Building on these principles, we consider specific applications of green solvents in microextraction techniques by analyzing published studies, which have focused on developing solid-phase and liquid-phase microextraction of pharmaceuticals, using DESs and ILs in biological samples. Here, we explored the applicability of these green solvents in microextraction approaches and examined how the analytical results might be affected. We also focused on the different types of DESs and ILs, their characteristics, their ecotoxicity and biodegradability. Furthermore, we examined the advantages and disadvantages of these solvents, addressing both aspects common to all microextraction methods and those specific to individual approaches. Finally, we highlighted the current challenges in this field and outlined future perspectives to overcome them.</div></div>","PeriodicalId":100594,"journal":{"name":"Green Analytical Chemistry","volume":"15 ","pages":"Article 100296"},"PeriodicalIF":6.2,"publicationDate":"2025-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145027129","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":"Dual mode unity-SPME-GC-MS unlocks the low-volatile flavour profiles of oolong, black, and Pu-erh teas: Revealing aroma diversity shaped by processing techniques","authors":"Yun-Jiao Ma ,&nbsp;Xuan-Peng Wang ,&nbsp;Xian-Bing Xu ,&nbsp;Yi-Feng Fan ,&nbsp;Qi-Yue Zhao ,&nbsp;Jia-Ling He","doi":"10.1016/j.greeac.2025.100295","DOIUrl":"10.1016/j.greeac.2025.100295","url":null,"abstract":"<div><div>The flavour diversity of three types of tea (oolong, black, and Pu-erh teas) processed by different methods was comprehensively analysed using dual mode unity solid-phase microextraction (DMU-SPME) technology combined with gas chromatography-mass spectrometry (GC–MS). The optimal DMU-SPME extraction conditions included an extraction temperature and time of 60 °C and 40 min, respectively, and the addition of 20 % NaCl. DMU-SPME is more efficient than traditional headspace solid-phase microextraction (HS-SPME) in the extraction of low-volatility flavour compounds such as nerolidol (floral aroma), 6-pentyltetrahydro-2H-pyran-2-one (creamy aroma), jasminlactone (floral aroma), and methyl jasmonate (floral aroma). A comparative analysis of the flavour characteristics of the nine tea samples revealed similar flavour compound profiles in tea samples of the same type; however, different types of tea samples exhibited significantly different flavour compound profiles. Additionally, the DMU-SPME extracts more differential aroma compounds than HS-SPME and therefore provides effective support for the identification of tea flavours, offering a new technique with strong prospects for tea quality evaluation and classification.</div></div>","PeriodicalId":100594,"journal":{"name":"Green Analytical Chemistry","volume":"15 ","pages":"Article 100295"},"PeriodicalIF":6.2,"publicationDate":"2025-08-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144989918","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":"Multi-criteria sustainability assessment of deep eutectic solvent-based liquid-liquid microextraction for prostate cancer therapeutics: Green, practical, and innovative approach","authors":"Maha Mohammad Abdel-Monem ,&nbsp;Mohamed I. Walash ,&nbsp;Asmaa Kamal El-Deen","doi":"10.1016/j.greeac.2025.100294","DOIUrl":"10.1016/j.greeac.2025.100294","url":null,"abstract":"<div><div>This study presents the first application of a terpene-based deep eutectic solvent (DES) in liquid-liquid microextraction (LLME) of flutamide (FTM) and finasteride (FSR) prior to HPLC-DAD analysis. The extraction efficacy was optimized through systematic evaluation of key parameters, including DES type and volume, vortex time, ionic strength, and pH. Under the optimal conditions, the method demonstrated acceptable linearity over the concentration range of 0.05–15 and 0.10–10 µg/mL with limits of detection (LODs) of 0.016 and 0.033 µg/mL for FTM and FSR, respectively. The precision, expressed as %RSDs, was &lt;3.5 %, demonstrating high repeatability and reproducibility. Furthermore, the method was successfully applied to spiked human plasma and river water samples, yielding recovery rates between 97 and 102 %, confirming its reliability in complex matrices. Finally, a comprehensive multi-criteria sustainability assessment using eight metrics highlighted the method's outstanding greenness, practicality, performance, and innovation. This study explores the potential of terpene-based DESs as sustainable extraction solvents for enhanced pharmaceutical and environmental analysis.</div></div>","PeriodicalId":100594,"journal":{"name":"Green Analytical Chemistry","volume":"14 ","pages":"Article 100294"},"PeriodicalIF":6.2,"publicationDate":"2025-08-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144914034","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":"Textile microfibers: emissions, quantification and analytical characterization. A household laundry perspective","authors":"Khawla Chouchene ,&nbsp;Ana L. Patrício Silva ,&nbsp;Ana Costa ,&nbsp;Andréa Marinho ,&nbsp;Armando C. Duarte ,&nbsp;Teresa Rocha-Santos ,&nbsp;João P. da Costa","doi":"10.1016/j.greeac.2025.100293","DOIUrl":"10.1016/j.greeac.2025.100293","url":null,"abstract":"<div><div>Textile microfibers are among the most significant emerging pollutants. The textile industry and household (laundry) wastewaters are the primary sources of these microfibers, responsible for up to 90% of fragmented fibers entering the aquatic environment. This review updates current knowledge of the last 20 years on microfiber release associated with laundry and textile processes, with a special emphasis on household laundry, and explores potential removal strategies. Scenarios for reducing synthetic microfiber release through interventions at multiple levels and involving different stakeholders including industry, consumers, and governments are discussed.</div><div>Herein, the key steps for microfiber characterization in effluents and laundry processes are also discussed in detail, underlying the need for monitoring, regulation, and effective measures to minimize the uncontrolled release of microfibers into the environment, thus reducing the prevalence of these environmental contaminants and their suspected impact.</div></div>","PeriodicalId":100594,"journal":{"name":"Green Analytical Chemistry","volume":"14 ","pages":"Article 100293"},"PeriodicalIF":6.2,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144895112","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}