Journal of AOAC International最新文献

{"title":"Simultaneous Determination of Four Per- and Polyfluoroalkyl Substances (PFAS) in DHA Products using LC-MS/MS for Quality Control and Risk Assessment.","authors":"Jiayi Zhang, Yanping Cao, Xuee Xi, Chaoqiang Xiao, Li Zhu","doi":"10.1093/jaoacint/qsag045","DOIUrl":"https://doi.org/10.1093/jaoacint/qsag045","url":null,"abstract":"<p><strong>Background: </strong>Docosahexaenoic acid (DHA) is a critical dietary supplement for vulnerable populations (e.g., infants, pregnant women), but contamination by per- and polyfluoroalkyl substances (PFAS)-persistent \"forever chemicals\"-poses potential health risks. Currently, no standardized methods exist for PFAS detection in DHA products, hindering quality control and risk assessment.</p><p><strong>Objective: </strong>To develop and validate a sensitive LC-MS/MS method for simultaneous determination of four PFAS (PFOA, PFODA, PFOS, and PFBS) in DHA matrices (algal oil and fish oil) and support product safety evaluation.</p><p><strong>Methods: </strong>Samples were extracted with 50% methanol/acetonitrile (v/v) via ultrasonication (40 °C, 20 min), followed by centrifugation and filtration. Chromatographic separation was achieved on a Phenomenex Kinetex F5 column (100 × 3.0 mm, 2.6 μm) with gradient elution (mobile phase: 2 mmol/L ammonium formate aqueous solution-methanol) in 12 min. Detection was performed via negative electrospray ionization (ESI-) in multiple reaction monitoring (MRM) mode. Method validation included linearity, limits of detection (LODs)/quantitation (LOQs), accuracy, precision, matrix effects, and stability. Thirteen commercial DHA products (11 algal oil, 2 fish oil) were analyzed.</p><p><strong>Results: </strong>Linearity (r ≥ 0.99) were achieved for PFAS; LODs/LOQs: 0.02/0.04 ng/mL. Recoveries at three spiking levels (0.1, 0.5, 1.0, 1.5 ng/mL) were ranged from 92.1%-108.4%, with RSDs of 2.8%-5.6%. Matrix effects were effectively corrected via matrix-matched calibration. Trace PFAS were detected in 3/13 samples, all below regulatory limits.</p><p><strong>Conclusions: </strong>The developed method is reliable for routine PFAS detection in DHA matrixes, providing practical technical support for quality control and risk assessment for DHA supplements for vulnerable populations.</p><p><strong>Highlights: </strong>Rapid (12 min), sensitive, and applicable to both algal oil and fish oil matrixes.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-06-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148145901","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":"Comprehensive Analysis of Quality Markers in Speranskia tuberculata based on HPLC Fingerprinting, Chemometrics, and Network Pharmacology.","authors":"Huifang Li, Jin Wang, Chun Yang, Xinshu Wang, Naiyi Wang","doi":"10.1093/jaoacint/qsag043","DOIUrl":"https://doi.org/10.1093/jaoacint/qsag043","url":null,"abstract":"<p><strong>Background: </strong>Speranskia tuberculata is a perennial herbaceous plant that is used in traditional Chinese medicine to dispel wind and dampness, promote blood circulation, and relieve pain. However, quality control markers, mechanisms of action, and systematic screening of quality indicators are still lacking.</p><p><strong>Objective: </strong>The high-performance liquid chromatography (HPLC) fingerprint of Speranskia tuberculata was established, and the quality markers (Q-Markers) of Speranskia tuberculata were analyzed by network pharmacology and molecular docking analysis methods.</p><p><strong>Method: </strong>In this study, HPLC was used to establish fingerprints and conduct similarity evaluation. Principal component analysis and orthogonal partial least squares discriminant analysis were used to suggest the differences among these fingerprints. The \"component-target-pathway\" network relationships of characteristic components of Speranskia tuberculata were constructed by network pharmacology. Molecular docking technology was used to analyze the binding affinity between Q-Markers and core targets, and the potential Q-Markers were predicted.</p><p><strong>Results: </strong>HPLC characteristic fingerprints identified 19 common peaks, among which four were tentatively identified as chlorogenic acid, kaempferol, diosmetin and amentoflavone. Through network pharmacological and molecular docking analysis, it was predicted that kaempferol and diosmetin could serve as the Q-Markers of Speranskia tuberculata.</p><p><strong>Conclusions: </strong>The method established in this study is accurate, reliable, simple, and practical, and can be used as a reference method for Speranskia tuberculata quality detection. Two Q-Markers selected by network pharmacology and molecular docking analysis can provide support and references for Speranskia tuberculata QC.</p><p><strong>Highlights: </strong>This study selected Speranskia tuberculata as the research object and initiated the research based on the concept of \"medicinal material characteristics-chemical quality-activity prediction\" starting from its origin to fill the research gap. The methodologies and strategies presented in this study can be extended to other traditional Chinese medicines, offering novel insights into the quantitative evaluation and identification of Q-Markers.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-05-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148007429","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":"Assessment of Homogeneity of Elemental Mass Fractions in a Castor Leaf (Ricinus communis L.) Reference Material Candidate Using ANOVA and PCA.","authors":"Altemar da Cruz Luciano, Adriana Costa Ferreira, Geovani Cardoso Brandão, Fábio de Souza Dias, Erik Galvão Paranhos da Silva, Walter Nei Lopes Dos Santos, Liz Oliveira Dos Santos","doi":"10.1093/jaoacint/qsag042","DOIUrl":"https://doi.org/10.1093/jaoacint/qsag042","url":null,"abstract":"<p><strong>Background: </strong>Certified reference materials (CRMs) are essential for method validation, quality control, and metrological traceability in analytical chemistry. However, CRMs for plant matrices of regional relevance, such as castor bean (Ricinus communis L.) leaves, remain scarce in tropical and subtropical regions. This study addresses that gap by evaluating the homogeneity of a castor bean leaf RM candidate produced under single-laboratory conditions.</p><p><strong>Objective: </strong>To assess between- and within-unit homogeneity of a Ricinus communis L. leaf RM candidate for seven inorganic elements (Al, Ca, Cu, Fe, Mg, P and Zn), following ISO Guide 35:2017. This study does not aim at certification or replacement of full certification procedures as specified in ISO 17034:2016.</p><p><strong>Methods: </strong>Castor bean leaf samples were collected in Bahia, Brazil. A total of 400 g of dry material was produced, homogenized, and distributed among 20 units. Elemental mass fractions were determined by microwave-induced plasma optical emission spectrometry (MIP OES) after acid digestion. Data were evaluated by one-way ANOVA (ISO Guide 35:2017) and principal component analysis (PCA) as a complementary exploratory tool.</p><p><strong>Results: </strong>A minimum sample mass of 400 mg was established as adequate for reliable homogeneity evaluation. Ten units were randomly selected for between-bottle assessment, with three subsamples per unit for within-bottle evaluation.</p><p><strong>Conclusion: </strong>The RM candidate was considered homogeneous for all seven elements at the 95% confidence level. PCA provided additional exploratory insights, including identification of atypical subsamples not detectable by univariate ANOVA.</p><p><strong>Highlights: </strong>Castor bean RM will be of great use for confirming the accuracy of methods, which will facilitate the validation of analytical methods and verification of quality control of samples of vegetable leaves or similar matrix, in addition to allowing metrological traceability.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-05-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147990607","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":"Advances in Enzymatic Measurement of β-Glucan in Mushrooms, Yeast, Algae, and Dietary Supplements.","authors":"Lucie C Sweeney, Caoilfhionn Walsh, Amaya O'Cochlain, Ruth Ivory, David Mangan","doi":"10.1093/jaoacint/qsag041","DOIUrl":"https://doi.org/10.1093/jaoacint/qsag041","url":null,"abstract":"<p><strong>Background: </strong>The rapid expansion of the functional mushroom, yeast, and algae market has increased the need for enzymatic quantification of 1,3-/1,6-β-glucans. The longstanding indirect approach, which calculates β-glucans by subtracting enzymatically measured α-glucans from total glucans obtained through acid hydrolysis, is increasingly challenged by modern supplement formulations containing resistant starches, trehalose, and sweeteners such as maltitol.</p><p><strong>Objective: </strong>To evaluate the current indirect enzymatic method for β-glucan measurement and to refine the analytical workflow to support reliable β-glucan quantification across the expanding functional mushroom, yeast, and algae market and associated dietary supplement formats.</p><p><strong>Methods: </strong>Key steps of the established indirect β-glucan method were systematically evaluated to identify matrix-dependent limitations related to acid solubilization, glucose stability during hydrolysis, α-glucan specificity, and formulation-derived interferences. Based on these findings, a refined analytical workflow was defined and applied for benchmarking and performance evaluation across mushrooms, yeast, algae, and multiple supplement delivery formats.</p><p><strong>Results: </strong>Targeted refinements increased measured total glucan values, improved α-glucan determination in matrices containing resistant starches, trehalose, and maltitol, and reduced systematic glucose loss associated with acid hydrolysis. Comparative evaluation demonstrated matrix-dependent differences relative to the conventional method, while maintaining consistent analytical performance across complex formulations and reducing total assay time.</p><p><strong>Conclusion: </strong>These advances in enzymatic β-glucan measurement address recognized limitations of the indirect approach and support more consistent β-glucan quantification across diverse natural product matrices and modern supplement formats.</p><p><strong>Highlights: </strong>Advances in enzymatic β-glucan measurement were achieved through targeted refinements to total and α-glucan determination, improving measurement consistency across mushrooms, yeast, algae, and complex supplement formulations and supporting further collaborative evaluation.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-05-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147978136","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":"Effect of different Processing Methods on the reduction of Oxytetracycline residues in Tilapia (Oreochromis niloticus).","authors":"R K Nadella, R Rajisha, K N Sajeena, E K Nanitha Krishna, T Paul Nathaniel, A Abhiram, P K Patil, S K Panda, N S Chatterjee","doi":"10.1093/jaoacint/qsag040","DOIUrl":"https://doi.org/10.1093/jaoacint/qsag040","url":null,"abstract":"<p><strong>Background: </strong>Oxytetracycline (OTC) is used as a therapeutic agent against bacterial pathogens in aquaculture, typically administered via medicated feed. Insufficient withdrawal time following drug treatment will result in antibiotic residue deposition in the tissues. Antibiotic residues are determined from freshly harvested fish tissues or processed fish samples for export purposes. But sufficient data is not available on the effect of different processing methods on the fate of antibiotic residues in fish tissues.</p><p><strong>Objective: </strong>This study is aimed at understanding the effects of various processing/cooking methods on the retention of OTC residues in the edible fillets of OTC-fed tilapia.</p><p><strong>Methods: </strong>Medicated feed was prepared by coating different doses of OTC into commercially available feed pellets and was administered to the fish in all the treatment groups for 10 days, and edible fillet samples were collected for various processing techniques, including boiling, microwave cooking, frying, and drying. The processed samples were analysed for OTC residues using Liquid Chromatography-tandem Mass Spectrometry (LC-MS/MS).</p><p><strong>Results: </strong>A Limits of detection (LOD) of 1.75 µg/kg and quantification (LOQ) of 5.82 µg/kg was achieved by the developed LC-MS/MS method for the quantification of OTC in fish samples. The results revealed a significant reduction of OTC in fish tissues following various processing methods. The maximum degradation was observed towards microwave processing and frying.</p><p><strong>Conclusions: </strong>This study provides insights into the effectiveness of various cooking/processing methods for the efficient reduction of OTC residues in edible fish fillets.</p><p><strong>Highlights: </strong>The present study highlights the effects of different processing methods and demonstrates that even when some levels of drug residues are present in fish tissues, they can be effectively degraded using appropriate processing methods.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-05-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147978142","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":"A highly Sensitive ERA-CRISPR/Cas13a Assay for Detection of Vibrio vulnificus.","authors":"Ye Pan, Xiaojuan Nie, Peng Lü","doi":"10.1093/jaoacint/qsag038","DOIUrl":"https://doi.org/10.1093/jaoacint/qsag038","url":null,"abstract":"<p><strong>Background: </strong>Vibrio vulnificus is a halophilic marine bacterium widely distributed in coastal environments and seafood products and is responsible for severe human infections and foodborne disease outbreaks. Rapid and sensitive detection of V. vulnificus is therefore critical for clinical diagnosis and seafood safety monitoring.</p><p><strong>Objective: </strong>The objective of this study was to develop and evaluate a rapid, sensitive, and specific nucleic acid detection method for V. vulnificus suitable for application in complex biological and food matrices.</p><p><strong>Methods: </strong>An ERA-CRISPR/Cas13a-based nucleic acid detection assay was established by coupling enzymatic recombinase amplification (ERA) with Cas13a-mediated collateral cleavage of fluorescent RNA reporters. The analytical performance of the assay was systematically evaluated using V. vulnificus standard plasmids, artificially contaminated human serum samples, and spiked oyster homogenates.</p><p><strong>Results: </strong>The assay exhibited high specificity for V. vulnificus, with no cross-reactivity observed for other common Vibrio species. The limit of detection (LOD) was 1 × 10-1 copies/μL for standard plasmid templates. In complex matrices, including human serum and oyster samples, the assay achieved an LOD of 1 × 101 CFU/mL. The entire detection process was completed under isothermal conditions within 45 min.</p><p><strong>Conclusions: </strong>A sensitive and specific ERA-CRISPR/Cas13a-based assay for the detection of V. vulnificus was successfully developed and validated. The method demonstrates strong analytical performance in both biological and seafood matrices.</p><p><strong>Highlights: </strong>A rapid isothermal ERA-CRISPR/Cas13a assay for V. vulnificus detection was developed. High specificity was achieved without cross-reactivity to other Vibrio species. The assay enables sensitive detection in serum and oyster samples. The method shows potential for routine seafood safety surveillance and marine pathogen monitoring.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-05-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147876971","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":"Innovative Framework for Blinded Evaluation of Methods: Application to Cannabinoid Quantification in Hemp.","authors":"Andriy Tkachenko, Xiangwei Du, Jake Guag, Manisha Das, Chih-Hao Hsu, Shuping Zhang","doi":"10.1093/jaoacint/qsag039","DOIUrl":"https://doi.org/10.1093/jaoacint/qsag039","url":null,"abstract":"<p><strong>Background: </strong>Regulatory changes and growth of hemp-derived products have increased the need for robust methods to quantify cannabinoids.</p><p><strong>Objective: </strong>To systematically evaluate a liquid chromatography photo-diode array (LC-PDA) method for 11 cannabinoids in hemp using a blinded collaborative framework, with emphasis on both fortified and endogenous analytes.</p><p><strong>Methods: </strong>A previously validated method was set up at a new‑to‑method laboratory (Veterinary Medical Diagnostic Laboratory, VMDL) and verified in-house using fortified samples. Discrepancies between certified and measured values for a hemp reference material raised questions about the method's performance for endogenous cannabinoids. To address this, an independent laboratory conducted a two-round collaborative exercise (Blinded Method Test, BMT) by preparing blind-coded samples using hemp, nettle, and hemp-nettle mixtures with various fortification levels. VMDL quantified cannabinoids by external calibration (EC) in acetonitrile (surrogate solution). Parallelism evaluation and standard-addition calibration were complementarily applied to address matrix effect and accuracy for endogenous analytes.</p><p><strong>Results: </strong>The method showed good linearity and acceptable accuracy and precision for blinded fortified hemp, nettle, and hemp-nettle samples and quality controls using EC. Parallelism results supported the use of solvent-based EC for endogenous cannabinoids in hemp. Standard-addition estimates were directionally consistent with EC but differed by about 15-45% for some analytes. These findings underscore the need for more detailed characterization of extraction efficiency for endogenous cannabinoids to strengthen accuracy assessment for incurred cannabinoids in complex botanical matrices.</p><p><strong>Conclusions: </strong>The two-round BMT demonstrates how collaborative exercises can extend conventional validation by integrating multiple matrices, parallelism testing, and complementary quantification approaches. The evaluated method is suitable for routine hemp testing at VMDL, while the findings emphasize the need to evaluate extraction efficiency for incurred versus fortified analytes in complex biomatrices.</p><p><strong>Highlights: </strong>A collaborative framework with parallelism and standard addition provides enhanced evaluation of method performance for complex botanical matrices.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-05-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147857922","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":"Single-Chain Variable Fragment-Based Dot Blot, Single, and Multiple Assays for Rapid SARS-CoV-2 Diagnostics.","authors":"Dilek Çam Derin, Enes Gültekin, Irmak İçen Taşkın, Muhammed Dündar, Barış Otlu","doi":"10.1093/jaoacint/qsaf105","DOIUrl":"10.1093/jaoacint/qsaf105","url":null,"abstract":"<p><strong>Background: </strong>Antigenic detection is reliably utilized in rapid diagnostic tests and provides a significant time advantage during pandemics and epidemics. Therefore, the rapid detection of viral infections is of great importance and will remain crucial in the future. The SARS-CoV-2 outbreak, which resulted in severe losses, is the most recent example of this necessity. Among rapid diagnostic tests, lateral flow assays (LFAs) are the most practical and do not require specialized equipment, typically being developed using antibody pairs.</p><p><strong>Objective: </strong>This study aimed to recombinantly produce a single-chain variable fragment (scFv) specific to the SARS-CoV-2 spike receptor-binding domain (sRBD) and to employ it in the development of LFAs utilizing both antibody and aptamer pairs and an aptamer cocktail.</p><p><strong>Methods: </strong>Gold nanoparticles were employed as labeling agents, while both the scFv and full length forms of CR3022, along with aptamers specific to the S and N proteins, were utilized in a sandwich assay format.</p><p><strong>Results: </strong>scFv was produced at a higher concentration and biologically active. It demonstrated effective viral detection in single LFA, dot blot assay (DBA), and multiplex LFA. While single LFA successfully detected only the synthetic target, DBA and multiplex LFA selectively identified the virus in nasopharyngeal and oropharyngeal swab samples.</p><p><strong>Conclusion: </strong>Findings highlight the differences and effectiveness of using scFv in combination with other capture agents and different assay principles for the development of cost-effective and rapid diagnostic tests.</p><p><strong>Highlights: </strong>scFvs exhibit variable binding in sandwich assays depending on the combinations employed. When used in combination with an aptamer cocktail, scFvs demonstrate enhanced target binding, which is shown for the first time in this study. The use of multiple testing strategies enables a more effective viral diagnosis.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"415-424"},"PeriodicalIF":1.7,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13148769/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145696467","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":"Evaluation of the Applicability of Modified QuEChERS with Small-Scale SPE for the Analysis of Neonicotinoid Insecticides in Beetroot and Paprika Powder.","authors":"Takamitsu Otake, Kaori Machida, Ayako Kimura","doi":"10.1093/jaoacint/qsaf100","DOIUrl":"10.1093/jaoacint/qsaf100","url":null,"abstract":"<p><strong>Background: </strong>As the demand for natural colorants is expected to increase in the future, it is important to analyze pesticide residues to investigate the relationship between exposure and health risks. A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) analytical method, which uses small-scale solid-phase extraction (SPE) for the cleanup process, is increasingly used in Japan. Since this method has hardly been studied for the analysis of pesticides in natural food colorants, it is necessary to evaluate its performance.</p><p><strong>Objective: </strong>This study aimed to evaluate the applicability of a modified QuEChERS for the analysis of neonicotinoid insecticides (NEOs) in beetroot and paprika selected from natural colorants.</p><p><strong>Methods: </strong>The modified QuEChERS was evaluated by a recovery study using blank beetroot and paprika powder. The matrix effect (ME) was also evaluated in detail for the analysis by the modified QuEChERS and LC coupled with tandem mass spectrometry (LC-MS/MS). These results were compared with those obtained by the Japanese official multiresidue method.</p><p><strong>Results: </strong>The mean recovery, intraday repeatability, and interday reproducibility for the modified QuEChERS were acceptable according to the validation guideline. The MEs for the modified QuEChERS were not particularly strong for the NEOs in the beetroot and paprika even when the isotopically labeled internal standards were not used.</p><p><strong>Conclusion: </strong>The evaluation of the modified QuEChERS was successfully tested and demonstrated the suitability of this method for the analysis of NEOs in beetroot and paprika.</p><p><strong>Highlight: </strong>The modified QuEChERS is not only accurate but is also a fast and environmentally friendly method for analyzing NEOs in beetroot and paprika.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"395-405"},"PeriodicalIF":1.7,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145338371","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 the QuEChERSER Method for 245 Pesticides and Environmental Contaminants in Barley and Hemp by Low-Pressure GC: Comparison of Triple Quadrupole MS/MS and Orbitrap HRMS for Qualitative and Quantitative Analysis.","authors":"Nicolás Michlig, Steven J Lehotay","doi":"10.1093/jaoacint/qsae093","DOIUrl":"10.1093/jaoacint/qsae093","url":null,"abstract":"<p><strong>Background: </strong>Monitoring laboratories are a fundamental link in the food safety chain, and regulatory demands in a competitive economy call for analytical methods that are simpler, faster, more rugged, and broader in scope. The \"quick, easy, cheap, effective, rugged, safe, efficient, and robust\" (QuEChERSER) mega-method introduced in 2021 meets these monitoring needs, which includes high sample throughput, automated cleanup of extracts, and fast low-pressure gas chromatography (LPGC).</p><p><strong>Objective: </strong>The goal of this work was to extend the QuEChERSER method to additional matrixes and more analytes using LPGC, including comparison of the analytical performances of two different mass spectrometric analyzers: triple quadrupole tandem mass spectrometry (MS/MS) and orbital ion trap (orbitrap) high-resolution (HR)MS.</p><p><strong>Methods: </strong>The QuEChERSER mega-method was validated for 245 pesticides and environmental contaminants in barley grains and hemp pellets using automated instrument top sample preparation (ITSP) coupled with LPGC-MS/MS or LPGC-HRMS (orbitrap).</p><p><strong>Results: </strong>Targeted MS/MS detection proved to be more sensitive than orbitrap using full data acquisition, leading to lower LOQs with more analytes yielding acceptable recoveries (70-120%) and repeatabilities (RSDs <20%). In barley, 89% of the compounds met validation criteria in MS/MS and 74% in HRMS, which in hemp were 81 and 66%, respectively. Qualitatively, orbitrap HRMS yielded 1% false positives compared to 3-4% in MS/MS, but due to the higher LOQs, the rates of false negatives were 14-17% in orbitrap versus 6-10% in MS/MS for the different matrixes.</p><p><strong>Conclusion: </strong>The QuEChERSER mega-method including ITSP+LPGC coupled with MS/MS or orbitrap analysis is a robust approach for multiple applications. In the comparison, MS/MS outperformed the orbitrap in terms of sensitivity, but the orbitrap advantages of easier method development, greater selectivity, and the possibility for non-targeted/retrospective analysis permit even broader expansion of analytical scope in the future.</p><p><strong>Highlights: </strong>ITSP+LPGC-MS/MS or -HRMS (orbitrap) analysis as part of the QuEChERSER mega-method is a useful and efficient way to monitor for contaminants in foods.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"281-293"},"PeriodicalIF":1.7,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142683994","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}