Journal of AOAC International最新文献

{"title":"Development and Validation of a Multiresidue Method for Simultaneous Analysis of 451 Multiclass Pesticides in Fodder Crops.","authors":"Sonu Kumar Mahawer, Sachin C Ekatpure, Narendra Kulkarni, Kaushik Banerjee","doi":"10.1093/jaoacint/qsaf084","DOIUrl":"10.1093/jaoacint/qsaf084","url":null,"abstract":"<p><strong>Background: </strong>Fodder crops are widely used as main ingredients of animal feed products. To combat pest infestations, farmers often apply pesticides on farms, the residual content of which may accumulate at or beyond toxic levels in/on the green fodder at the stage of harvest. To safeguard animals and humans (through ecological food chains) from these residual pesticides, both domestic and commercial programs are necessary to monitor the levels of pesticide residues in food and feed. The existing methods exhibit constraints regarding scope, selectivity, and sensitivity. These limitations warrant a high-throughput multiresidue method for monitoring and risk assessment of multiclass pesticides in fodder crops.</p><p><strong>Objective: </strong>The study aimed to develop and validate a multiresidue method for the simultaneous analysis of 451 multiclass pesticides, their isomers, and metabolites of toxicological concern in three widely used fodder crops, namely sorghum, maize, and lucerne.</p><p><strong>Methods: </strong>Well-homogenized samples of sorghum, maize, and lucerne (10 g) were extracted with acetonitrile (10 mL). An aliquot of the extract was cleaned by dispersive solid-phase extraction (dSPE) with graphitized carbon black (GCB, 7.5 mg/mL). The method performance was evaluated for a mixture of multiclass pesticides at 10 and 20 µg/kg using liquid and gas chromatography with tandem mass spectrometry (LC-MS/MS and GC-MS/MS).</p><p><strong>Results: </strong>The GC-MS/MS and LC-MS/MS techniques allowed analyses of the test pesticides within chromatographic run times of 17 and 20 min, respectively. The method's performance using matrix-matched calibration was satisfactory for all compounds (recoveries 70-120%, repeatability-RSD, <20%) at 10 and 20 µg/kg in three studied matrixes.</p><p><strong>Conclusion: </strong>The method successfully determined the residues of all tested compounds in each fodder matrix. It demonstrates satisfactory selectivity, accuracy, and repeatability. Given all of these, it is recommended for regulatory and commercial testing purposes.</p><p><strong>Highlights: </strong>This is a high-throughput residue analysis method targeting 451 compounds in sorghum, maize, and lucerne involved a single multiresidue extraction, followed by dSPE cleanup with analysis using LC-MS/MS and GC-MS/MS. The method sensitivity met the European Union's-Maximum Residue Levels (EU-MRL), and performance complied with the SANTE/11312/2021 QC criteria.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"304-311"},"PeriodicalIF":1.7,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145093052","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":"Manipulating Analytical Bias in GMO Quantification for Processed Foods by Adjusting PCR Amplicon Sizes.","authors":"Kazuki Toyota, Satoshi Noma, Miwa Takahashi, Shinya Kimata, Yosuke Kikuchi, Megumi Satou, Tomoki Tanaka, Toshiyuki Takiya, Reona Takabatake, Kazumi Kitta, Junichi Mano","doi":"10.1093/jaoacint/qsaf098","DOIUrl":"10.1093/jaoacint/qsaf098","url":null,"abstract":"<p><strong>Background: </strong>A wide range of foods containing genetically modified organisms (GMOs) are commercially available. To verify the accuracy of GMO labeling, real-time PCR is used to quantify GMO content in raw materials. However, DNA fragmentation during food processing can introduce analytical bias, making it difficult to accurately assess GMO content in processed foods.</p><p><strong>Objective: </strong>This study aimed to establish a method to accurately evaluate food labeling suitability by inferring the GMO content at the raw material stage from the measurement results of processed foods.</p><p><strong>Methods: </strong>Model processed foods (heat-treated soybeans) containing GM events were prepared and analyzed using a GMO quantification method incorporating taxon-specific real-time PCR with longer amplicons.</p><p><strong>Results: </strong>We observed that the calculated GMO content increased with the length of the amplicon used in the taxon-specific PCR assay. This finding indicates that GMO content can be artificially influenced by modifying the amplicon size. When a longer amplicon was deliberately employed, the GMO content calculated for the processed food always exceeded that of the raw material.</p><p><strong>Conclusions: </strong>The use of longer amplicons in taxon-specific PCR can lead to an overestimation of GMO content at the raw material stage based on the measurements from processed foods. If the overestimated value remains below the labeling threshold, the appropriateness of GMO labeling can still be confirmed. The proposed method offers a simplified and practical approach for use in routine inspections.</p><p><strong>Highlights: </strong>The developed method enables direct analysis of processed foods to assess GMO labeling appropriateness. It eliminates the need to obtain raw materials or conduct multiple analyses. The approach simplifies GMO quantification in inspection laboratories by reducing procedural complexity.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"377-386"},"PeriodicalIF":1.7,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145277094","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 Methylimidazole in Tea by High-Resolution Mass Spectrometry and Investigation of its Source.","authors":"Huijiao Chen, Weidong Xie, Weiping Xie","doi":"10.1093/jaoacint/qsaf106","DOIUrl":"10.1093/jaoacint/qsaf106","url":null,"abstract":"<p><strong>Background: </strong>Methylimidazole (MEI), classified as a Group 2B carcinogen by the World Health Organization (WHO), is formed primarily as a Maillard reaction byproduct in foods. Its recent detection in tea has raised concerns regarding potential food safety risks.</p><p><strong>Objective: </strong>This study aims to establish an ultrahigh-performance liquid chromatography-high-resolution mass spectrometry (UHPLC-HRMS) method for the simultaneous determination of MEIs in tea. The validated method was employed to determine the contents of MEIs across various tea types and to explore their potential sources.</p><p><strong>Methods: </strong>Sample pretreatment was performed using a modified QuEChERS approach with isotope dilution. Chromatographic separation was achieved on a HILIC column using a gradient elution program with mobile phases consisting of 5 mmol/L ammonium acetate containing 0.1% formic acid in water and acetonitrile. Detection was carried out using Q-TOF with SWATH for MS/MS quantification.</p><p><strong>Results: </strong>The method exhibited excellent linearity (r > 0.999) within the concentration range of 2-50 µg/L. The limits of detection (LODs) ranged from 0.0024 to 0.0045 mg/kg. The recovery ranged from 82 to 100.2%, with RSDs between 1.1 and 4.6%. Statistical analysis indicated that heavily fermented and roasted teas exhibited significantly higher MEI levels than lightly processed teas did (p < 0.001). Laboratory simulations experiments showed that MEI formation increased substantially at the baking temperature of 150°C.</p><p><strong>Conclusions: </strong>The developed UHPLC-HRMS method is accurate and precise and is suitable for the simultaneous quantification of three MEIs in tea. These results suggest that the MEI content in tea is associated with degree of fermentation and roasting, likely originating from Maillard reaction-derived byproducts.</p><p><strong>Highlights: </strong>The proposed HRMS method mitigated the limitations commonly associated with conventional LC-MS approaches, Furthermore, the validated method was successfully employed to quantify MEI contents in tea subjected to various fermentation and roasting processes, thereby contributing to a better understanding of MEI's potential formation pathways.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"387-394"},"PeriodicalIF":1.7,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145679845","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":"Research on the Preparation and Application of Lyoprotectants for Hanseniaspora uvarum BF-345 Derived from Indigenous Grape Juice.","authors":"Qiao Song, Jiawei Yang, Tao Peng, Hongmei Tong, Xiaolun Zhou, Jing Wang","doi":"10.1093/jaoacint/qsaf110","DOIUrl":"10.1093/jaoacint/qsaf110","url":null,"abstract":"<p><strong>Background: </strong>The extensive use of imported commercial Saccharomyces cerevisiae active dry powder preparations has led to a serious homogenization of wine products in China.</p><p><strong>Objective: </strong>In recent years, there has been growing interest in developing and applying indigenous non-Saccharomyces yeasts to enhance the diversity and distinctive character of wines.</p><p><strong>Methods: </strong>In this study, a promising indigenous strain, Hanseniaspora uvarum BF-345, previously isolated from local grape juice, was investigated due to its desirable fermentation properties, robust stress tolerance, and high β-glucosidase activity. Response surface methodology (RSM) was employed to optimize the composition of a cryoprotectant formulation for the vacuum freeze-drying of BF-345.</p><p><strong>Results: </strong>The optimal protectant formulation was determined as follows: 5.63% skim milk powder, 12.89% maltitol, and 7.02% sucrose. Under these conditions, the viability of the freeze-dried cells reached 85.2%, representing a 27.3% increase compared to the pre-optimized formulation.</p><p><strong>Conclusion: </strong>The prepared active dry yeast complied with the Chinese national standard GB/T 20886.2-2021 and maintained a viability above 70% after 6 months of sealed storage at 4°C.</p><p><strong>Highlights: </strong>In micro-vinification trials with cabernet sauvignon, the fermentation system inoculated with the freeze-dried powder exhibited higher yeast cell counts and more favorable fermentation kinetics than that inoculated with a liquid seed culture.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"425-435"},"PeriodicalIF":1.7,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145812510","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":"Correction to: Determination of Subsidiary Colors in D&C Red No. 36 (Pigment Red 4) by HPLC and UHPLC.","authors":"","doi":"10.1093/jaoacint/qsag013","DOIUrl":"10.1093/jaoacint/qsag013","url":null,"abstract":"","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"437"},"PeriodicalIF":1.7,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146215173","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":"High-Throughput Quantification of Pesticide Residues in Complex Matrix (Chili Powder) Using Liquid Chromatography Tandem Mass Spectrometry: Inter- and Intra-Day Validation.","authors":"Raviraj Chandrakant Shinde, Macky Suraliwala, Dharmendra Kumar, Sagar Atugade, Pandit Shiragave","doi":"10.1093/jaoacint/qsaf079","DOIUrl":"10.1093/jaoacint/qsaf079","url":null,"abstract":"<p><strong>Background: </strong>Chili powder is a widely consumed spice; however, during cultivation chili crops are often subjected to pesticide treatments to control pests and diseases. Thus, monitoring pesticide residues in such matrixes is crucial for food safety and to comply with national as well as international regulations for export/import purposes. However, accurate analysis of pesticide residue in chili powder is challenging due to its complex nature.</p><p><strong>Objective: </strong>To develop and validate a high-throughput LC-MS/MS method for the quantification of multiclass pesticide residues in a complex chili powder matrix.</p><p><strong>Methods: </strong>The acetonitrile-based extraction method was optimized for chili powder samples. The targeted analytes were separated using reverse-phase liquid chromatography and detected using tandem mass spectrometry. Validation was conducted following SANTE guidelines to comply with regulatory requirements.</p><p><strong>Results: </strong>The method with an optimized sample preparation workflow demonstrated a lower matrix effect of <35% for the target pesticides. The LOQ was determined to be 0.005 mg/kg for 135 analytes, with recovery ranging from 70 to 110%, and intra-day and inter-day precision (RSD) were below 15%. Analysis of market/incurred samples and measurement uncertainty further provided more confidence in the method performance.</p><p><strong>Conclusions: </strong>The developed LC-MS/MS method provides a robust, sensitive, and high-throughput approach for the quantification of pesticide residues in complex chili powder. Its intra- and inter-day validation confirms suitability for routine analysis in food safety laboratories.</p><p><strong>Highlights: </strong>A high-throughput LC-MS/MS method is developed for pesticide analysis in complex chili powder. The method was validated according to SANTE 11312/2021-v2 with excellent precision and accuracy. Suitable for routine food safety monitoring of a wide range of pesticide residues in a testing laboratory.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"353-359"},"PeriodicalIF":1.7,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144984023","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":"Pesticide and Veterinary Drug Residues in Food.","authors":"Jon W Wong, Eric Verdon","doi":"10.1093/jaoacint/qsag021","DOIUrl":"10.1093/jaoacint/qsag021","url":null,"abstract":"","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"279-280"},"PeriodicalIF":1.7,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147597259","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":"Investigation of Nanoflow Liquid Chromatography High-Resolution MS (nanoLC-HRMS) for the Analysis of Veterinary Drug Residues in Fish and Shrimp.","authors":"Sherri B Turnipseed, Christine R Casey, Jessica P Rafson","doi":"10.1093/jaoacint/qsaf018","DOIUrl":"10.1093/jaoacint/qsaf018","url":null,"abstract":"<p><strong>Background: </strong>A wide-scope screening method for veterinary drugs and other contaminants in aquaculture products using liquid chromatography (LC) high-resolution mass spectrometry (HRMS) was developed previously. Using nanoflow LC could significantly increase the sensitivity of this method.</p><p><strong>Objective: </strong>The objective of this study was to evaluate the potential advantages of nanoLC-HRMS as a screening method for veterinary drug residues in seafood.</p><p><strong>Method: </strong>Preliminary nanoLC-HRMS investigations included comparison of nanospray source options and evaluation of nanoLC columns, mobile phases, and gradient programs. The optimized method was tested using tissue fortified with a mixture of veterinary drugs and pesticides.</p><p><strong>Results: </strong>Using nanoLC columns with integrated emitters provided stable electrospray ionization resulting in chromatographic peaks with reproducible retention times and peak areas; diagnostic MS2 product ions were also detected. Coupling nanoLC to HRMS increased the area counts for many target analytes by 2-3 orders of magnitude. Less concentrated extracts could be analyzed with simplified preparation and minimal ion suppression. Replicate extractions of fortified fish generally gave relative standard deviations under 20%. Most analytes could be identified at concentrations 10-fold less than the target testing levels with detection limits in final extracts corresponding to 0.01-0.02 picograms injected on-column. Acceptable linearity was observed using solvent, matrix-matched, and matrix-extracted standard curves. Disadvantages of nanoLC-HRMS included the inability to detect some classes of compounds, i.e., dyes and avermectins, and longer wait times between chromatographic analyses.</p><p><strong>Conclusions: </strong>Significant increases in sensitivity were observed with nanoLC-HRMS. Analytical results from fortified fish and shrimp showed the method to be suitable for qualitative screening, analyte identification, and quantification with minimal matrix effects.</p><p><strong>Highlights: </strong>A wide variety of veterinary drugs and pesticides could be reproducibly detected and identified in fortified fish and shrimp using nanoLC-HRMS with minimal cleanup. Residues from imported laboratory samples were also detected and identified using this method.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"294-303"},"PeriodicalIF":1.7,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143560477","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":"Correction to: Development of Psilocybe Mushroom Species Reference Material-Cultivation Parameters and Chemical Profiles.","authors":"","doi":"10.1093/jaoacint/qsaf104","DOIUrl":"10.1093/jaoacint/qsaf104","url":null,"abstract":"","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"436"},"PeriodicalIF":1.7,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13148766/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145807246","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":"Development of 1H qNMR Analytical Procedure for Purity Determination of Imazosulfuron and 1,4-BTMSB-d4 for ISO 17034 Accreditation.","authors":"Toru Miura, Yang Liu, Anton Bzhelyansky, Takashi Ohtsuki, Hiroshi Matsufuji","doi":"10.1093/jaoacint/qsaf099","DOIUrl":"10.1093/jaoacint/qsaf099","url":null,"abstract":"<p><strong>Background: </strong>Quantitative NMR spectroscopy (qNMR) can be used to determine chemical purity. This applies to the resonating nuclei of all the present chemical species, enabling quantitation of the analyte against chemically nonidentical calibrator molecules.</p><p><strong>Objective: </strong>Validation approaches for determining chemical purity with qNMR are being endorsed by major pharmacopoeias and other standard-setting bodies. In this study, we investigated the purity determination, uncertainty evaluation, and method validation of imazosulfuron using qNMR to gain ISO 17034 accreditation.</p><p><strong>Methods: </strong>We ensured the NIST traceability of imazosulfuron by calibrating 1,4-BTMSB-d4 (determining its purity and uncertainty) using NIST PS 1 and then calibrating imazosulfuron using the calibrated 1,4-BTMSB-d4. Purity and uncertainty determinations were performed using qNMR, as per the proposed revisions to the USP General Chapters <761> and <1761>. Method development and validation were performed as described in these chapters using the principles of Analytical Quality by Design (AQbD).</p><p><strong>Results: </strong>First, we defined a target measurement uncertainty of ±2.0% (k = 2) as the Analytical Target Profile (ATP). Next, we established robust operating parameters for qNMR and determined the purity and uncertainty of 1,4-BTMSB-d4. Subsequently, we determined the purity and uncertainty of imazosulfuron using the calibrated 1,4-BTMSB-d4 to verify that the qNMR method produced reportable values that met the ATP criteria.</p><p><strong>Conclusions: </strong>The purity and uncertainty of imazosulfuron were 98.2% ± 1.2% (k = 2), meeting the ATP criteria. We then moved on to the next stage to monitor and ensure that the qNMR method remains properly controlled and to satisfy the ATP criteria during routine use. Based on the above, we established a validation scheme that meets the requirements of ISO 17034 by leveraging AQbD considerations.</p><p><strong>Highlights: </strong>The AQbD principles shift the focus of method validation toward procedure design and development, resulting in more rational design, efficient development, and validation.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"406-414"},"PeriodicalIF":1.7,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145357340","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}