Journal of AOAC International最新文献

{"title":"Evaluating Substitution of Hazardous Solvents in USP Monograph HPLC Methods.","authors":"Weidong Zhao, Koushik Mondal, Praveen Thakur, David Mande, Nagaraju Katepally, Parise Naga Malleswari, Lakshmi Kanth Juluru, Suresh Kumar Sheik, Yvs Veerendra, Arunima Pola, Greg Winter, Paolo Lecchi, Mrunal A Jaywant, Michael Ambrose","doi":"10.1093/jaoacint/qsag071","DOIUrl":"https://doi.org/10.1093/jaoacint/qsag071","url":null,"abstract":"<p><strong>Background: </strong>Hazardous solvents, such as dichloromethane (DCM), n-hexane, and acetonitrile (ACN), are widely used in HPLC methods, posing significant health and environmental risks.</p><p><strong>Objective: </strong>To evaluate the feasibility and impact of substituting hazardous solvents with greener alternatives in USP monograph methods.</p><p><strong>Methods: </strong>Six high-impact solvents were identified from USP-NF monographs. Two representative monographs per solvent were selected. Substitution strategies were assessed, and performance was compared using system suitability and sample acceptance criteria. Greenness improvement was evaluated using the Analytical GREEnness (AGREE) metric.</p><p><strong>Results: </strong>Performance remained equivalent across all twelve substitution cases. In almost every instance, only the mobile phase required modification, either by direct substitution or by adjusting the solvent-to-buffer ratio, except for one case that required a minor adjustment in column temperature. The AGREE Greenness metric increased by 18-65% in ten out of twelve cases; for n-hexane, improvements were modest at just 6% when replaced with n-heptane but exceeded 40% when substituted with supercritical CO₂.</p><p><strong>Conclusions: </strong>Greener solvents are highly likely to replace hazardous solvents used in compendial chromatography methods without loss of performance.</p><p><strong>Highlights: </strong>Demonstrated performance equivalency for greener solvent substitutions; Quantified greenness improvements using AGREE; Discussed strategies to implement greener solvents in USP monograph methods.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-09-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148932233","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":"STRATUM-Structured Framework for Reporting, Assessment, and Translational Utility of Metagenomics.","authors":"Joseph A Russell, Ishi Keenum, Karen Jarvis, Haley Sanderson, Michael D Sussman, Kamil Khanipov, Joe Lacirignola, Amy Xiao, Jonathan M Phillips, Malcolm Johns, Bala Ganesan, Cameron Parsons, Benjamin Davis, Shanmuga Sozhamannan","doi":"10.1093/jaoacint/qsag085","DOIUrl":"https://doi.org/10.1093/jaoacint/qsag085","url":null,"abstract":"<p><strong>Background: </strong>Metagenomic next-generation sequencing (mNGS) enables broad, untargeted detection of pathogens and microbial signals across complex sample types. However, the diversity of operational contexts, from regulatory enforcement to exploratory discovery, challenges the defining of analytical or interpretive standards appropriate across all applications. Variability in laboratory practices, bioinformatic methods, and reporting conventions continues to limit consistency and decision-maker confidence in mNGS results.</p><p><strong>Objectives: </strong>We introduce STRATUM (Structured Framework for Reporting, Assessment, and Translational Utility of Metagenomics), a use-case-stratified framework that aligns quality assurance, metadata reporting, and interpretive standards with the consequence and intended use of metagenomic sequencing outputs.</p><p><strong>Methods: </strong>STRATUM is organized around five representative biosurveillance use cases spanning public health, food safety, environmental monitoring, synthetic biology detection, and national security. A three-tier interpretive model calibrates analytical rigor, validation expectations, and reporting requirements to decision consequence; from high-consequence regulatory and clinical determinations (Tier 1), through operational surveillance (Tier 2), to exploratory and hypothesis-generating contexts (Tier 3).</p><p><strong>Results: </strong>The framework provides graduated guidance across key domains including sample preparation, sequencing design, controls and contamination governance, reference database curation, bioinformatics reproducibility, and multi-factor signal validation. Cross-cutting principles include explicit documentation of evidentiary bases, transparency in database and pipeline provenance, and defined escalation pathways when results transition between interpretive tiers.</p><p><strong>Conclusion: </strong>Realizing the operational potential of mNGS requires evidentiary standards responsive to decision context rather than fixed across applications. STRATUM offers a consequence-tiered model for quality and reporting in applied metagenomics, supporting reproducible, transparent, and defensible sequencing-based surveillance across public health and biodefense domains.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148914682","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":"Validation of a QuEChERS-UHPLC-MS/MS method for the determination of aflatoxins and ochratoxin A in cannabis flowers: Application to regulated and non-regulated products.","authors":"Mónica Pereira, Florencia Tissot, Ignacio Machado","doi":"10.1093/jaoacint/qsag086","DOIUrl":"https://doi.org/10.1093/jaoacint/qsag086","url":null,"abstract":"<p><strong>Background: </strong>Cannabis sativa flowers are a complex plant matrix that poses significant analytical challenges due to their chemical composition and the low regulatory limits established for consumer safety.</p><p><strong>Objective: </strong>To optimize and validate a QuEChERS-UHPLC-MS/MS method for the simultaneous determination of aflatoxins B1, B2, G1, G2, and ochratoxin A in Cannabis sativa flowers.</p><p><strong>Methods: </strong>Critical parameters influencing extraction efficiency were systematically evaluated through a 3³ factorial design, including solvent acidification, extraction time, and evaporation temperature. Optimal conditions were achieved using acetonitrile acidified with 0.1% v/v formic acid, 15 min vortex extraction, and evaporation below 50 °C.</p><p><strong>Results: </strong>Under these conditions, recoveries ranged between 90-109%, with precision (RSD 2.5-8.3%) and trueness demonstrating satisfactory method performance. Linearity was confirmed with R² > 0.99, and LOQs of 1.0 µg/kg for aflatoxins and 5.0 µg/kg for ochratoxin A, consistent with European Pharmacopoeia requirements. Application to 30 cannabis flower samples revealed that all commercial products complied with international maximum residue limits (MRLs), whereas some non-regulated samples exceeded the total aflatoxin limit (4 µg/kg), mainly due to elevated aflatoxin B2.</p><p><strong>Conclusion: </strong>These findings provide the first data on mycotoxin occurrence in cannabis flowers from Uruguay and highlight the importance of monitoring non-regulated products, emphasizing the need for appropriate quality-control strategies.</p><p><strong>Highlights: </strong>The proposed method provides a simple, robust, and high-throughput approach for routine quality control of cannabis flowers.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-09-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148889792","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":"Simplified Method to Test Decontamination of Bovine Spongiform Encephalopathy Agent Dried on Steel Surfaces.","authors":"Oksana Yakovleva, Teresa Pilant, Juraj Cervenak, Cyrus Bett, Terry O Woods, Kitty L Pomeroy, Luisa Gregori, David M Asher","doi":"10.1093/jaoacint/qsag083","DOIUrl":"https://doi.org/10.1093/jaoacint/qsag083","url":null,"abstract":"<p><strong>Background: </strong>Transmissible spongiform encephalopathy (TSE) agents are lethal unconventional pathogens that have infected both humans and animals. Bovine spongiform encephalopathy (BSE) is a TSE. TSE agents are unusually resistant to inactivation. In-use tests conducted to investigate those products involve intentionally contaminating carrier objects with TSE agents, exposing them to decontaminating regimens, and then surgically implanting treated carriers into TSE-susceptible rodents to assay for TSE infectivity.</p><p><strong>Objective: </strong>To adapt a simple in-use carrier test to decontaminate TSE agents based on methods employed for decades to test for bacteria, fungi and viruses remaining on surfaces treated with disinfectants, known as \"use-dilution tests.\"</p><p><strong>Methods: </strong>We serially diluted 10% BSE brain homogenate in a normal bovine-brain-tissue paste and contaminated 60 stainless-steel pins mounted in disposable heat-resistant plastic holders with the lowest dilution and five or six pins with each successive dilution. We investigated 2N NaOH-known to inactivate TSE agents-with and without autoclaving (121 °C and 134 °C) and autoclaving without exposure to NaOH. Each pin was briefly introduced into the brain of an anesthetized mouse. We monitored animals for 24 months. At the end of the study, the brains of all mice (except six mice that died early post inoculation) were tested for the presence of abnormal prion protein, a marker of TSE infections. Next, we calculated the level of inactivation provided by each method.</p><p><strong>Results: </strong>Our results indicated that none of the 60 animals inoculated with pins decontaminated with NaOH (with or without autoclaving) developed BSE while steam autoclaving alone at both conventional and elevated temperatures was not effective. This inactivation corresponded to ≥ 1.1 log10 reduction of infectivity.</p><p><strong>Conclusion: </strong>Using our relatively simple and quick pin method with brief intracerebral punctures without surgical implantation, we tested many more replicate treated carriers than in studies previously reported while yielding similar results.</p><p><strong>Highlights: </strong>The proposed pin method was proven effective to evaluate inactivation regimens for BSE agents.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-09-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148882901","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":"Determination of Per- and Polyfluoroalkyl Substances in Food and Feed by Enhanced Matrix Removal LC-MS/MS Method, AOAC Official Method 2025.11, First Action.","authors":"Limian Zhao, Matthew Giardina, Emily Parry, M Lorna De Leoz","doi":"10.1093/jaoacint/qsag029","DOIUrl":"10.1093/jaoacint/qsag029","url":null,"abstract":"<p><strong>Background: </strong>AOAC INTERNATIONAL Standard Method Performance Requirement (SMPR)® 2023.003 outlines method performance requirements for the determination of per- and polyfluoroalkyl substances (PFAS) across a broad range of food and feed matrixes.</p><p><strong>Objective: </strong>The objective of this study was to develop and validate the EMR LC-MS/MS method in accordance with AOAC INTERNATIONAL SMPR 2023.003 using a single-laboratory approach.</p><p><strong>Methods: </strong>The method features QuEChERS extraction followed by a novel enhanced matrix removal (EMR) mixed-mode passthrough cleanup, an online injection program, sensitive LC-MS/MS detection, and accurate, precise quantitation using neat calibration curves with isotopically labeled internal standards.</p><p><strong>Results: </strong>Method performance was evaluated for suitability and selectivity, calibration linearity, limit of quantitation (LOQ), recovery, and repeatability, and the method was successfully validated in a single-laboratory validation (SLV) across 16 diverse food matrixes, encompassing all 11 required food categories. Acceptable PFAS background cleanliness was demonstrated, supporting accurate and reliable quantitation in all food matrixes. Validated or calculated LOQs for all analytes across all food matrixes were equal or below the required LOQs, with an exception rate of <1%. Recovery and single-laboratory repeatability also satisfied the acceptance criteria specified in the AOAC SMPR guideline, again with an exception rate of <1%. Method selectivity was confirmed through baseline separation of cholic acid interferences from PFOS isomers and through secondary confirmation of PFBA and PFPeA using LC-QTOF analysis.</p><p><strong>Conclusions: </strong>The EMR LC-MS/MS method met all performance criteria, supporting its advancement as a First Action AOAC Official Method of AnalysisSM  2025.11.</p><p><strong>Highlights: </strong>A novel EMR LC-MS/MS method was developed and successfully validated for the determination of 30 PFAS analytes across a wide range of food and feed matrixes, fulfilling the requirements of AOAC SMPR 2023.003.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"720-740"},"PeriodicalIF":1.7,"publicationDate":"2026-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147679742","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":"Microbial Community Composition and Quality Characteristics of a Tea and Jujube Blend Kombucha Beverage.","authors":"Qian Wang, Yu Zhao, Haorui Ma, Zhulin Wang","doi":"10.1093/jaoacint/qsag031","DOIUrl":"10.1093/jaoacint/qsag031","url":null,"abstract":"<p><strong>Background: </strong>Despite the high nutritional value of jujubes, their product diversification remains limited. Developing a new functional fermented beverage is a promising strategy for enhancing their economic value and expanding their market appeal.</p><p><strong>Objective: </strong>To enhance the value-added processing of jujubes, this study developed a novel co-fermentation process for producing kombucha using both jujubes and tea. Furthermore, the individual and synergistic impacts of these substrates on the microbial, sensory, and physicochemical properties of the final beverage were systematically evaluated.</p><p><strong>Methods: </strong>Three kombucha types were prepared: traditional (C), pure jujube (Z), and tea-jujube blend (CZ). They were comprehensively characterized by evaluating their physicochemical profiles, microbial compositions, and sensory attributes.</p><p><strong>Results: </strong>Group CZ displayed significantly higher contents of total flavonoids and reduced sugars after fermentation. The addition of jujubes also restructured the microbial community, introducing Saccharomyces and significantly increasing the relative abundance of Lactobacillus. Group CZ achieved the highest sensory acceptance scores. The ethanol content of group CZ conformed to the commercial standard for nonalcoholic beverages.</p><p><strong>Conclusions: </strong>Co-fermentation with jujubes and tea significantly enhances both the functional properties and the palatability of kombucha, presenting a promising strategy for creating high-value fermented products.</p><p><strong>Highlights: </strong>The synergistic fermentation of tea and jujubes significantly enhances the functional properties and nutritional value of the product; jujubes optimize the microbial community structure during kombucha fermentation.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"819-827"},"PeriodicalIF":1.7,"publicationDate":"2026-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147793057","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":"Chromatographic Considerations and Maltitol Interference in Dietary Fiber Analysis.","authors":"Tadas Kargelis, Zhen K Lam, David Mangan","doi":"10.1093/jaoacint/qsag017","DOIUrl":"10.1093/jaoacint/qsag017","url":null,"abstract":"<p><strong>Background: </strong>AOAC 2017.16 and AOAC 2022.01 are CODEX Type I methods for total dietary fiber (TDF) that integrate enzymatic-gravimetric steps with high-performance liquid chromatography (HPLC) quantification of low molecular weight soluble dietary fiber (SDFS). As implementation expands, chromatography-related limitations and matrix-specific interferences can affect SDFS determination.</p><p><strong>Objective: </strong>To evaluate performance of AOAC-recommended and alternative HPLC columns for DP2/DP3 boundary assignment across a broad carbohydrate set, and to investigate maltitol-associated interference leading to apparent SDFS overestimation in starch-containing matrixes.</p><p><strong>Methods: </strong>Seventy-four carbohydrate standards (including oligosaccharides, polyols, and sugar alcohols) were analyzed in duplicate across five HPLC column configurations under AOAC 2017.16/2022.01 and AOAC 2009.01/2011.25 conditions. Column performance was scored by correct peak-area assignment relative to the maltose demarcation. Maltitol interference was assessed using food products formulated with/without maltitol and mixtures of maltitol (and other polyols) with wheat starch or wheat flour using scaled AOAC 2017.16 and AOAC 2001.03 procedures.</p><p><strong>Results: </strong>Across 74 analytes, SugarPak (Waters) provided the highest overall assignment accuracy, with a two-column series configuration scoring highest. Maltitol alone could be excluded by adjusting the DP2/DP3 demarcation; however, maltitol combined with glucose-based polymers produced an additional peak area in the SDFS region, yielding up to ∼8% apparent SDFS overestimation in wheat starch mixtures.</p><p><strong>Conclusions: </strong>Chromatographic selection materially affects DP2/DP3 assignment for SDFS quantification. Maltitol can cause matrix-dependent artifactual SDFS in starch-containing test materials, suggesting formation of low-molecular-weight species during enzymatic processing. Guidance on column equivalency would strengthen AOAC dietary fiber methodology, and further work is warranted to further investigate maltitol interaction with glucose-based polymers during TDF analysis.</p><p><strong>Highlights: </strong>SugarPak showed best DP2/DP3 peak-area assignment across 74 standards. Several analytes elute at/near the demarcation depending on column configuration. Maltitol + starch matrixes can generate artifactual SDFS and inflate TDF.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"741-751"},"PeriodicalIF":1.7,"publicationDate":"2026-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13553113/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147322668","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Correction to: Determination of Alkaloids in Mitragyna speciosa (Kratom) Raw Materials and Dietary Supplements by HPLC-UV: Single-Laboratory Validation, First Action 2017.14.","authors":"","doi":"10.1093/jaoacint/qsag052","DOIUrl":"10.1093/jaoacint/qsag052","url":null,"abstract":"","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"861"},"PeriodicalIF":1.7,"publicationDate":"2026-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148392753","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":"Validation of Methods for Determination of Vitamins B1, D2, and D3 in Commercial Animal Feed Matrixes by LC-MS/MS.","authors":"Alvaro G Garcia, Carlos Tamez, Nassifatou Koko Tittikpina, Jason C White, Christian O Dimkpa","doi":"10.1093/jaoacint/qsag027","DOIUrl":"10.1093/jaoacint/qsag027","url":null,"abstract":"<p><strong>Background: </strong>Vitamin B1 (thiamine), D2 (ergocalciferol), and D3 (cholecalciferol) are essential nutrients in animal diets, critical for health and the maintenance of physiological processes. Deficiencies or excesses can lead to severe health issues, necessitating reliable quantification methods for QC, label claim compliance, and safety assurance in the pet food industry.</p><p><strong>Objective: </strong>The aim of this study was to extend and validate AOAC Official Methods  2015.14 (for vitamin B1) and 2016.05 (for vitamins D2 and D3) to animal feed matrixes using LC-MS/MS in a single-laboratory study.</p><p><strong>Methods: </strong>Vitamin B1 was extracted via enzymatic digestion with acid phosphatase, while vitamins D2 and D3 were extracted using saponification, followed by liquid-liquid extraction.</p><p><strong>Results: </strong>The methods were validated for cat kibble, dog kibble, and wet dog feed, demonstrating high sensitivity (LODs: 0.018 ng/mL for B1 and 0.005 ng/mL for D2 and D3. LOQs: 0.06 ng/mL for B1, 0.016 ng/mL for D2, and 0.018 ng/mL for D3), excellent linearity (R2 = 0.997-0.999), and acceptable recoveries (88-115%). Quantification revealed vitamin B1 concentrations exceeding the Association of American Feed Control Officials minimum recommendations, with the lowest at 8.99 mg/kg on a dry matter basis (DMB) in wet dog food. Vitamin D levels were within recommended ranges, with the lowest in cat kibble at 18.13 μg/kg DMB for vitamin D3, while vitamin D2 contributed minimally to total vitamin D, at 0.27 μg/kg DMB.</p><p><strong>Conclusion: </strong>LC-MS/MS methods based AOAC 2015.14 and 2016.05 were single-laboratory validated and applied to the analysis of vitamin B1 and vitamins D2 and D3, respectively, in cat kibble, dog kibble, and wet dog food.</p><p><strong>Highlights: </strong>These results support the utility of the methods for routine analysis of animal feeds to verify label claims, nutritional adequacy, and safety.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"657-664"},"PeriodicalIF":1.7,"publicationDate":"2026-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147597281","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":"Optimization of Supercritical CO2 Extraction of Phenolic Compounds from Tomato (Solanum lycopersicum L.) Seeds Using Response Surface Methodology.","authors":"Abderrahmane Tighrine, Anna Montefusco, Monica De Caroli, Marcello Salvatore Lenucci","doi":"10.1093/jaoacint/qsag033","DOIUrl":"10.1093/jaoacint/qsag033","url":null,"abstract":"<p><strong>Background: </strong>Tomato seeds, a byproduct of the tomato-processing industry, are a rich source of bioactive compounds with promising nutritional and functional potential.</p><p><strong>Objective: </strong>This study aimed to optimize the supercritical CO2 (SC-CO2) extraction of phenolic compounds from Solanum lycopersicum L. seeds using a full factorial design (FFD) within the framework of response surface methodology (RSM).</p><p><strong>Method: </strong>The effects of extraction pressure (100-500 bar) and temperature (40-80°C) were evaluated, with oil extraction yield and total phenolic content (TPC) as response variables. A one-factor-at-a-time (OFAT) approach assessed the effect of ethanol (0.25-1.0 mL) as a co-solvent under constant optimal extraction conditions. Derringer's desirability function was applied to identify simultaneous optimal conditions to maximize both responses. The main phenolic compounds were putatively annotated via HPLC coupled with a diode array detector and time-of-flight mass spectrometry (HPLC-DAD-TOF).</p><p><strong>Results: </strong>Extraction pressure and co-solvent volume significantly affected both oil extraction yield and TPC, while temperature primarily influenced yield. Multi-response optimization achieved an overall desirability value of 1.0 at 425 bar and 78°C with 1 mL ethanol, resulting in the highest oil extraction yield and phenolic recovery.</p><p><strong>Conclusion: </strong>SC-CO2 extraction combined with desirability-based RSM is an efficient, green technique for valorizing tomato-processing residues, supporting circular bioeconomy principles through the sustainable recovery of high-value bioactives.</p><p><strong>Highlights: </strong>Optimized SC-CO2 extraction using RSM revealed that the factors most influencing oil extraction yield and the recovery of phenolic compounds were pressure and the quantity of co-solvents used. HPLC-DAD-TOF analysis putatively annotated the main phenolic compounds, thus emphasizing the sustainable valorization of byproducts from tomato processing.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"804-812"},"PeriodicalIF":1.7,"publicationDate":"2026-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147793127","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}