Journal of AOAC International最新文献

{"title":"Validation of the Level 2 Modification for the Neogen® Molecular Detection Assay 2-Salmonella Enteritidis/Salmonella Typhimurium Method for Detection of the Monophasic Variant Salmonella enterica  1,4,[5],12:-:1,2. AOAC Performance Tested MethodSM 122302.","authors":"Quynh-Nhi Le, Vanessa Tsuhako, Mark Mozola","doi":"10.1093/jaoacint/qsae088","DOIUrl":"10.1093/jaoacint/qsae088","url":null,"abstract":"<p><strong>Background: </strong>The Neogen® Molecular Detection Assay 2-Salmonella Enteritidis/Salmonella Typhimurium (MDA2-SE/ST) method, Performance Tested MethodSM (PTM) 122302, is a nucleic acid amplification test for specific detection of Salmonella enterica ser. Enteritidis (SE) and Salmonella enterica ser. Typhimurium (ST), including the ST monophasic variant Salmonella enterica  1,4,[5],12: i:-, in select poultry samples. Results for SE and ST are generated separately.</p><p><strong>Objective: </strong>The objective of the study was to validate the MDA2-SE/ST method for detection of an additional monophasic variant of ST, S. enterica  1,4,[5],12:-:1,2.</p><p><strong>Methods: </strong>A single strain of S. enterica  1,4,[5],12:-:1,2 was tested as part of a seven-strain inclusivity/exclusivity test panel. Strains were tested after growth in two enrichment media used in the method, buffered peptone water (BPW) and buffered peptone water, ISO formulation (BPW-ISO), and at two incubation temperatures, 35 ± 2°C and 41.5 ± 1°C.</p><p><strong>Results: </strong>S. enterica  1,4,[5],12:-:1,2 produced positive results in the ST assay and negative results in the SE assay in both enrichment media and at both incubation temperatures. Results for the other six test strains were as expected under all conditions.</p><p><strong>Conclusions: </strong>The MDA2-SE/ST method can detect the monophasic variant S. enterica  1,4,[5],12:-:1,2 as well as S. enterica ser. Typhimurium and the monophasic variant S. enterica  1,4,[5],12: i:-. The MDA2-SE/ST method maintains inclusiveness for S. enterica ser. Typhimurium despite flagellar antigen variation.</p><p><strong>Highlights: </strong>The data were reviewed by the AOAC PTM Program and approval was granted for modification of the MDA2-SE/ST method, PTM 122302.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"263-268"},"PeriodicalIF":0.0,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142635058","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":"Development of a Modified QuEChERS Extraction for the Detection of Rosemary Extracts (E392) Expressed as Sum of Carnosol and Carnosic Acid in Food by LC-MS/MS.","authors":"Yiu-Tung Wong, Tak-Shing Leung, Wai-Hong Fung","doi":"10.1093/jaoacint/qsae099","DOIUrl":"10.1093/jaoacint/qsae099","url":null,"abstract":"<p><strong>Background: </strong>Rosemary extracts are derived from the leaves of Rosmarinus officinalis and commonly employed as a natural food preservative. They serve as natural antioxidants in food, preventing spoilage and extending shelf life.</p><p><strong>Objective: </strong>This study aimed to develop a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction with liquid chromatography tandem mass spectrometry (LC-MS/MS) for the analysis of rosemary extracts in food as the sum of its markers carnosol and carnosic acid.</p><p><strong>Method: </strong>Carnosol and carnosic acid in food were extracted by a modified QuEChERS extraction after the addition of analyte protectants during extraction and analyzed by LC-MS/MS via an internal standard calibration method. 2,2'-isopropylidienediphenol and podocarpic acid were used as internal standards for carnosol and carnosic acid, respectively.</p><p><strong>Results: </strong>The limit of detection (LOD) of carnosol and carnosic acid were all less than 1 mg/kg, while their corresponding values of limit of quantitation (LOQ) ranged from 1.44 to 3.12 mg/kg in various matrixes. Spike recoveries at three fortification levels (10, 50, and 300 mg/kg) were all within 90-110% with RSD less than 10% in all cases.</p><p><strong>Conclusions: </strong>A modified QuEChERS extraction with LC-MS/MS detection for the analysis of rosemary extracts in food was successfully developed, validated, and demonstrated to be fast, robust, and reliable.</p><p><strong>Highlights: </strong>The developed modified QuEChERS extraction with LC-MS/MS detection offered a fast and efficient way to analyze rosemary extracts in various foods during a routine food surveillance program.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"199-206"},"PeriodicalIF":0.0,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142831518","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 Neogen® Molecular Detection Assay 2-Salmonella Enteritidis/Salmonella Typhimurium Method for Specific Detection of Salmonella enterica Ser. Enteritidis and Salmonella enterica Ser. Typhimurium in Chicken Carcass Rinse and Raw Ground Chicken: AOAC Performance Tested MethodSM 122302.","authors":"Quynh-Nhi Le, Toni Bartling, Mark Mozola, Cynthia Zook, Christina Barnes, Brooke Roman, Preetha Biswas, Susan Noe, Robert Donofrio","doi":"10.1093/jaoacint/qsae086","DOIUrl":"10.1093/jaoacint/qsae086","url":null,"abstract":"<p><strong>Background: </strong>The Neogen® Molecular Detection Assay 2-Salmonella Enteritidis/Salmonella Typhimurium (MDA2-SE/ST) method is a rapid, nucleic acid amplification-based test for specific detection of Salmonella enterica ser. Enteritidis (SE) and Salmonella enterica ser. Typhimurium (ST), including the ST monophasic variant Salmonella enterica  1,4, [5], 12: i:-, in select poultry samples. Results for SE and ST are generated separately.</p><p><strong>Objective: </strong>The objective of the study was to validate the MDA2-SE/ST method for detection of SE and ST in chicken carcass rinse and raw ground chicken (325 g) for Performance Tested MethodsSM (PTM) certification.</p><p><strong>Methods: </strong>The study consisted of inclusivity/exclusivity testing and independent laboratory testing of chicken carcass rinse and raw ground chicken using inoculated matrixes. Data were analyzed using a paired probability of detection model to determine if differences in the number of positive results obtained with the MDA2-SE/ST and reference methods were significant.</p><p><strong>Results: </strong>In inclusivity testing, all 50 SE strains produced positive results in the SE assay and negative results in the ST assay. All 53 ST strains (including the monophasic variant) produced positive results in the ST assay and negative results in the SE assay. All 35 exclusivity strains produced negative results in both assays. The exclusivity panel included multiple non-SE group D1  Salmonella serovars, multiple non-ST group B serovars, Salmonella spp. from other somatic groups, and other Enterobacteriaceae. In matrix testing, results for the MDA2-SE/ST and reference methods were in complete agreement for both matrixes.</p><p><strong>Conclusions: </strong>Results of the validation study showed that the MDA2-SE/ST method is an accurate, specific method for detection of SE and ST in select poultry matrixes.</p><p><strong>Highlights: </strong>The data were reviewed by the AOAC PTM Program, and approval was granted for certification of the Molecular Detection Assay 2-Salmonella Enteritidis/Salmonella Typhimurium method as PTM 122302.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"253-262"},"PeriodicalIF":0.0,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142635059","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":"https://doi.org/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 LC high resolution MS (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 ten-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 clean-up. Residues from imported laboratory samples were also detected and identified using this method.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-03-01","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":"Quantitation of Usnic Acid from Three Usnea Species, Its Commercial Formulations Using High-Performance Thin-Layer Chromatography-Mass Spectrometry (HPTLC-MS) and Their Metabolite Profiling Using UPLC-QTof-MSE.","authors":"Kiran Kumar Tatapudi, Siva Bandi, Ramulu Kotta, Vinayaka Kanivebagilu Shankaranarayana, Vaikundamoorthy Ramalingam, Katragadda Suresh Babu","doi":"10.1093/jaoacint/qsae074","DOIUrl":"10.1093/jaoacint/qsae074","url":null,"abstract":"<p><strong>Background: </strong>The genus Usnea (Parmeliaceae; lichenized Ascomycetes) is pale grayish-green fruticose lichens, which grow as leafless mini-shrubs and comprise about 360 species. Most of the Usnea species are edible and are utilized in preparation of traditional foods as well as in medicines to combat a wide range of ailments.</p><p><strong>Objective: </strong>This study aimed to quantify usnic acid (UA) in three Usnea spp. (Usnea ghattensis [UG], Usnea orientalis [UO], and Usnea undulata [UU]) using HPTLC-MS. Additionally, chemical profiling of acetone extracts using UPLC-QTof-MSE resulted in the identification of 16 compounds based on their MS/MS fragmentation patterns.</p><p><strong>Methods: </strong>Hyphenated techniques, HPTLC-MS, and UPLC-QTof-MSE have been proposed to quantify UA and analyze metabolites in crude extracts qualitatively. This method allowed tentative characterization of metabolites from Usnea spp.</p><p><strong>Results: </strong>The quantification study showed excellent linearity for UA at 0.25-1 µg/band with a correlation coefficient r2 > 0.99, and the LOD and LOQ were found to be 51.7 and 156.6 ng/band, respectively. Furthermore, UPLC-QTof-MSE analysis of crude extracts led to identification of lichen secondary metabolites through their exact molecular masses and MS/MS fragmentation studies.</p><p><strong>Conclusion: </strong>The present study summarizes an HPTLC method for quantification of UA in three different Usnea spp. Additionally, two herbal formulations containing Usnea spp. as an ingredient, the developed method was validated as per the ICH guidelines and further UPLC-QTof-MSE analysis facilitated tentative characterization of 16 different secondary metabolites based on their MS/MS fragmentation patterns.</p><p><strong>Highlights: </strong>A rapid HPTLC method for quantification of UA in three different Usnea spp., along with two herbal formulations, and metabolite profiling using UPLC-QTof-MSE.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"180-188"},"PeriodicalIF":0.0,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142368043","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":"Level 2 Modification (Matrix Extension) Study of the Neogen® Molecular Detection Assay 2-Salmonella Enteritidis/Salmonella Typhimurium Method: Detection of Salmonella enterica Ser. Enteritidis and Salmonella enterica Ser. Typhimurium in Cooked Breaded Chicken and Raw Ground Chicken (25 g). AOAC Performance Tested MethodSM 122302.","authors":"Quynh-Nhi Le, Mark Mozola, Erin Crowley, Andrew Deterding, Brooke Roman","doi":"10.1093/jaoacint/qsae087","DOIUrl":"10.1093/jaoacint/qsae087","url":null,"abstract":"<p><strong>Background: </strong>The Neogen® Molecular Detection Assay 2-Salmonella Enteritidis/Salmonella Typhimurium (MDA2-SE/ST) method is a nucleic acid amplification test for specific detection of Salmonella enterica ser. Enteritidis (SE) and Salmonella enterica ser. Typhimurium (ST), including the ST monophasic variant Salmonella enterica  1,4, [5], 12: i:-, in select poultry samples. Results for SE and ST are generated separately. The method was previously validated for testing of chicken carcass rinse and raw ground chicken (325 g).</p><p><strong>Objective: </strong>The objective of the study was to validate the MDA2-SE/ST method for detection of SE and ST in cooked breaded chicken and raw ground chicken (25 g) as a Level 2 modification for Performance Tested MethodSM certification.</p><p><strong>Methods: </strong>Inclusivity/exclusivity testing and independent laboratory testing of cooked breaded chicken and raw ground chicken (25 g) were conducted.</p><p><strong>Results: </strong>In inclusivity testing with buffered peptone water (BPW-ISO) broth at 41.5°C, all 50 SE strains produced positive results in the SE assay and negative results in the ST assay. All 53 ST strains (including the monophasic variant) produced positive results in the ST assay and negative results in the SE assay. All 35 exclusivity strains produced negative results in both assays. The exclusivity panel included multiple non-SE group D1  Salmonella serovars, multiple non-ST group B serovars, Salmonella spp. from other somatic groups, and other Enterobacteriaceae. In matrix testing, there were no significant differences in the number of positive results obtained with the MDA2-SE/ST and reference methods by probability of detection analysis at the 95% confidence level.</p><p><strong>Conclusion: </strong>Results of the matrix extension study showed that the MDA2-SE/ST method is an accurate method for detection of SE and ST in cooked breaded chicken and raw ground chicken (25 g).</p><p><strong>Highlights: </strong>Validation of the MDA2-SE/ST method for two additional matrixes provides users with additional capability for specific detection of SE and ST in poultry products.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"269-278"},"PeriodicalIF":0.0,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142607773","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 of Anticholinesterase Active Compounds from the Ethylacetate Fraction of Hydroalcoholic Extract of Itrifal Sana Using TLC-bioautography-MS and Its Validation Using an In Silico Molecular Approach.","authors":"Monalisha Samal, Aslam Siddiqui, Mohammad Irfan Dar, Varsha Srivastava, Muzayyana Khan, Rabea Parveen, Shahid Hussain Ansari, Sayeed Ahmad","doi":"10.1093/jaoacint/qsae095","DOIUrl":"10.1093/jaoacint/qsae095","url":null,"abstract":"<p><strong>Background: </strong>Traditional formulations are used extensively throughout the world due to their holistic approach to health and wellness with the fewest possible adverse effects. Itrifal Sana is a traditional Unani polyherbal formulation: a unique combination that makes it synergistically potent, capable of providing dual benefits for health and well-being. Even though the formulation is frequently utilized, there is no scientific evidence to support its therapeutic efficiency.</p><p><strong>Objective: </strong>The present study was designed to detect and identify bioactives, responsible for acetylcholinesterase inhibitory activity, by TLC-bioautography-MS and its validation using an in silico molecular approach.</p><p><strong>Methods: </strong>Authentication of the formulation was performed using macroscopy and powder microscopy. Quality control was performed using ultra-performance liquid chromatography-mass spectrometry (UPLC-MS) fingerprint analysis. TLC-bioautography-MS was performed to detect the bioactives responsible for acetylcholinesterase inhibitory activity and the findings were validated using an in silico approach.</p><p><strong>Results: </strong>The TLC-bioautography-MS revealed the presence of rosmarinic acid, kaempferol, and apigenin as potential bioactive anticholinesterase metabolites. UPLC-MS analysis demonstrated the separation of 48 phytocompounds in the most active fraction of the formulation. In silico analysis of identified metabolites showed acetylcholinesterase inhibitory activity in ten identified metabolites, and, moreover, rosmarinic acid and lobeline showed the highest potential activity.</p><p><strong>Conclusion: </strong>Our findings indicate that Itrifal Sana, which was investigated for the first time, has enormous potential for managing alzheimer's disease (AD) caused by acetylcholinesterase enzyme inhibition. The findings were derived through a successful TLC-bioautography-MS and in silico approach; however, further research on the full efficacy using in vitro cell line studies, in vivo studies, pharmacokinetics studies, and toxicity studies is still needed.</p><p><strong>Highlights: </strong>TLC-bioautography-MS and an in silico molecular approach offer much more effective, accurate, and reliable results than conventional methods in the identification and validation of bioactive components from Itrifal Sana, a polyherbal formulation that helps to advance the development of natural product-based therapeutics for cholinesterase dysfunctional diseases.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"189-198"},"PeriodicalIF":0.0,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142824980","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":"Specific Determination of (-)- and (+)-Gossypol in Vegetable Oil by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry with Chiral Pre-Column Derivatization.","authors":"Mimi Guo, Yameng Wang, Yalin Xue, Zhangqun Duan, Qiaoying Chang","doi":"10.1093/jaoacint/qsae076","DOIUrl":"10.1093/jaoacint/qsae076","url":null,"abstract":"<p><strong>Background: </strong>As the unique ingredient of cottonseed oil, gossypol is toxic and there are differences between the enantiomers. Although the determination of (-)- and (+)-gossypol in cotton plants or cottonseed has been performed, the detection of the gossypol enantiomers in vegetable oil has rarely been reported.</p><p><strong>Objective: </strong>To develop a specific inspection method for (-)- and (+)-gossypol in vegetable oil by ultra-performance liquid chromatography (UPLC)-tandem mass spectrometry with chiral pre-column derivatization.</p><p><strong>Methods: </strong>(-)- and (+)-Gossypol were separated on an ACQUITY C18 reverse-phase column (100 mm × 2.1 mm, 1.7 μm) maintained at 40°C on an UPLC system with gradient elution. The mobile phases were composed of methanol (solvent A) and water containing 0.1% formic acid (solvent B). Analytes were detected using an electrospray ionization (ESI) source in positive mode. The contents of (-)- and (+)-gossypol standard derivatives were quantified by multiple reaction monitoring (MRM) with the transitions of m/z 633/483 for quantitative ion pairs and m/z 633/558 for qualitative ion pairs.</p><p><strong>Results: </strong>The results indicated that the quantitative analysis could be accomplished within 12.5 min and the LODs of (-)- and (+)-gossypol were 25.55 and 14.67 μg/kg, respectively. When this method was applied to olive oil spiked with gossypol standards, good recoveries [95.37-105.84% for (-)-gossypol and 98.96-105.14% for (+)-gossypol] and RSDs [3.41-6.02% for (-)-gossypol and 4.50-6.94% for (+)-gossypol)] were achieved.</p><p><strong>Conclusion: </strong>The present study confirms the feasibility of determining gossypol enantiomers and achieves trace determination of (-)- and (+)-gossypol in vegetable oil. These results make this method more suitable for the qualitative identification of whether the vegetable oil has been mixed with cottonseed oil.</p><p><strong>Highlights: </strong>The trace determination of (-)- and (+)-gossypol in vegetable oils has been achieved. This method provides technical support for further identification of whether commercially available vegetable oil has been mixed with cottonseed oil.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"144-150"},"PeriodicalIF":0.0,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142484151","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 11+Myco MS-PREP® Method for Determination of Aflatoxins, Fumonisins, Deoxynivalenol, Ochratoxin A, Zearalenone, HT-2, and T-2 Toxins in Cereals, Baby Food, Spices, and Animal Feed by Immunoaffinity Column with LC-MS/MS: AOAC Performance Tested MethodSM 112401.","authors":"Dave Leeman, Andrew B Allan, Helen Cameron, Carol Donelly, Adam Tramaseur, Joanna Stratton, Susan J MacDonald","doi":"10.1093/jaoacint/qsae097","DOIUrl":"10.1093/jaoacint/qsae097","url":null,"abstract":"<p><strong>Background: </strong>The 11+Myco MS-PREP® immunoaffinity column (IAC) contains a gel suspension of monoclonal antibodies specific to the toxins of interest. Following sample extraction, the IAC is used for cleanup and concentration of mycotoxins prior to analysis by LC with tandem mass spectrometry (LC-MS/MS).</p><p><strong>Objective: </strong>This study evaluated the IAC with LC-MS/MS method for Performance Tested MethodSM certification for simultaneous determination and confirmation of aflatoxins (AF) B1, B2, G1, G2, and M1; deoxynivalenol (DON), fumonisins B1, B2, and B3; ochratoxin A (OTA); T-2; HT-2; and zearalenone (ZON) from corn, wheat, cereal-based baby food (with and without dairy ingredients), paprika, chili powder, and animal feed.</p><p><strong>Methods: </strong>A single extraction method using acetonitrile-water (1 + 1, by volume) was used for all matrixes. The method developer validated all matrixes and an independent laboratory verified method performance on corn and animal feed. Data were analyzed for recovery, repeatability precision, LOD, LOQ, confirmation of identity, and method selectivity.</p><p><strong>Results: </strong>Recovery (72-138%) and repeatability (0.46-24%), with the exception of sporadic data points, were within acceptance criteria. LOQ was estimated as AFB1 0.018-0.32 μg/kg, AFB2 0.037-0.28 μg/kg, AFG1 0.019-0.14 μg/kg, AFG2 0.036-0.28 μg/kg, DON 4.0-75 μg/kg, fumonisin B1 4.9-37 μg/kg, fumonisin B2 4.0-32 μg/kg, fumonisin B3 2.0-16 μg/kg, OTA 0.15-4.4 μg/kg, T-2 0.5-7.5 μg/kg, HT-2 0.70-7.5 μg/kg, and ZON 1.3-7.2 μg/kg, depending on matrix. Method performance was verified with reference and QC materials. Selectivity and confirmation of identity were also demonstrated.</p><p><strong>Conclusion: </strong>The 11+Myco MS-PREP IAC with LC-MS/MS method demonstrated acceptable performance for simultaneous determination of 12 mycotoxins in seven matrixes.</p><p><strong>Highlight: </strong>The data were reviewed by the AOAC Performance Tested MethodsSM Program and approval was granted for certification of the 11+Myco MS-PREP Method as PTM 112401.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"207-252"},"PeriodicalIF":0.0,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11879221/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142815336","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":"Co-Estimating Estradiol Valerate and Medroxyprogesterone Acetate in a Combined Hormonal Product: A Novel Short Runtime UPLC Method.","authors":"Erdal Dinç, Adem Mert","doi":"10.1093/jaoacint/qsaf016","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf016","url":null,"abstract":"<p><strong>Background: </strong>Hormones regulate growth, development, and reproductive functions. While deficiencies can lead to various health problems, excessive intake may cause metabolic disorders and side effects. Therefore, there is a need to develop new, reliable, and economical methods for quality control and accurate analysis of hormones in tablets used for hormone replacement therapy.</p><p><strong>Objective: </strong>To develop a novel, reliable, and cost-effective, ultra-performance liquid chromatography (UPLC) method for accurately quantifying estradiol valerate (EV) and medroxyprogesterone acetate (MPG) in hormone replacement therapy tablets.</p><p><strong>Method: </strong>Chromatographic separation of EV and MPG was achieved using an ACQUITY UPLC BEH C18 (1.7 μm, 2.1 mm × 100 mm) column and a mixture containing water (6%), acetonitrile (44%), methanol (42%), and 0.10 M phosphate buffer (8%, pH = 2.14). Chromatographic detection was accomplished at 280.0 nm for EV and 240.0 nm for MPG, with a flow rate of 0.34 mL/min at a column temperature of 40 °C. The method's validity was assessed using individual and spiked sample analyses.</p><p><strong>Results: </strong>The validated UPLC method offered an alternative procedure to quantify EV and MPG in commercial hormone tablets. This method demonstrated highly accurate, and precise analytic results with a short retention and low cost. The measured concentrations of EV and MPG in the tablet samples were found within the expected ranges, confirming the method's suitability for reliable hormone quantification in commercial tablets.</p><p><strong>Highlights: </strong>This study introduces the first UPLC-PDA method for analyzing EV and MPG in a commercial hormone formulation. The method showed excellent assay results in the analysis of real samples.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143560476","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}