Michael W DeGregorio, Chiao-Jung Kao, Gregory T Wurz
{"title":"Complexity of Translating Analytics to Recent Cannabis Use and Impairment.","authors":"Michael W DeGregorio, Chiao-Jung Kao, Gregory T Wurz","doi":"10.1093/jaoacint/qsae015","DOIUrl":"10.1093/jaoacint/qsae015","url":null,"abstract":"<p><p>While current analytical methodologies can readily identify cannabis use, definitively establishing recent use within the impairment window has proven to be far more complex, requiring a new approach. Recent studies have shown no direct relationship between impairment and Δ9-tetra-hydrocannabinol (Δ9-THC) concentrations in blood or saliva, making legal \"per se\" Δ9-THC limits scientifically unjustified. Current methods that focus on Δ9-THC and/or metabolite concentrations in blood, saliva, urine, or exhaled breath can lead to false-positive results for recent use due to the persistence of Δ9-THC well outside of the typical 3-4 h window of potential impairment following cannabis inhalation. There is also the issue of impairment due to other intoxicating substances-just because a subject exhibits signs of impairment and cannabis use is detected does not rule out the involvement of other drugs. Compounding the matter is the increasing popularity of hemp-derived cannabidiol (CBD) products following passage of the 2018 Farm Bill, which legalized industrial hemp in the United States. Many of these products contain varying levels of Δ9-THC, which can lead to false-positive tests for cannabis use. Furthermore, hemp-derived CBD is used to synthesize Δ8-THC, which possesses psychoactive properties similar to Δ9-THC and is surrounded by legal controversy. For accuracy, analytical methods must be able to distinguish the various THC isomers, which have identical masses and exhibit immunological cross-reactivity. A new testing approach has been developed based on exhaled breath and blood sampling that incorporates kinetic changes and the presence of key cannabinoids to detect recent cannabis use within the impairment window without the false-positive results seen with other methods. The complexity of determining recent cannabis use that may lead to impairment demands such a comprehensive method so that irresponsible users can be accurately detected without falsely accusing responsible users who may unjustly suffer harsh, life-changing consequences.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"493-505"},"PeriodicalIF":0.0,"publicationDate":"2024-05-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139975146","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}
Alaa Reda, Hanaa Saleh, Eman A Bahgat, Michael Gamal Fawzy
{"title":"Different Eco-Friendly Spectrophotometric Approaches Including Direct and Manipulations of Zero and Ratio Spectra for Simultaneous Determination of Novel Nasal Spray Combination Used in Seasonal Allergic Rhinitis.","authors":"Alaa Reda, Hanaa Saleh, Eman A Bahgat, Michael Gamal Fawzy","doi":"10.1093/jaoacint/qsae016","DOIUrl":"10.1093/jaoacint/qsae016","url":null,"abstract":"<p><strong>Background: </strong>The presentation of rhinitis has drawn increasing attention in recent years due to the possibility of overlap or confusion between allergic rhinitis symptoms and those of COVID-19. Azelastine hydrochloride (AZH) and mometasone furoate (MOF) are two of the most efficient combinations for enhancing the symptoms of seasonal allergic rhinitis.</p><p><strong>Objective: </strong>This work concerns applying and validating different accurate and simple spectrophotometric approaches for simultaneous quantification of the binary mixture of AZH and MOF in raw material, laboratory-prepared mixtures, and pharmaceutical preparation. Moreover, assessment of the environmental impact of the applied approaches on the environment was also a key goal of this study.</p><p><strong>Methods: </strong>AZH was determined using the direct spectrophotometric (D0) method, while four reliable spectrophotometric approaches namely, induced dual wavelength (IDW), ratio subtraction (RS), ratio difference (RD), and ratio derivative (1DD) were used for MOF determination.</p><p><strong>Results: </strong>The methods were validated in line with the International Conference of Harmonization standards. In the AZH range of (5-56 µg/mL) and MOF range of (2-20 µg/mL), the linearity of the proposed approaches was investigated with high accuracy findings. There were no significant differences between the obtained results and those of the reported method when compared statistically. Furthermore, the applied spectrophotometric methods were deemed to be eco-friendly according to Green Analytical Procedure Index (GAPI) and Analytical Greenness Calculator (AGREE) assessment metrics.</p><p><strong>Conclusions: </strong>The applied spectrophotometric methods are simpler, more eco-friendly, and take a shorter time to precisely estimate many measurements compared to the only reported chromatographic analysis.</p><p><strong>Highlights: </strong>Neither publications of novel spectrophotometric methods nor reported green ones have been available for simultaneous determination of the binary mixture of AZH and MOF, so this work has a great significance and novelty in the area of pharmaceutical analysis.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"512-518"},"PeriodicalIF":0.0,"publicationDate":"2024-05-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139975147","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":"Eco-Friendly Simultaneous Estimation of Ponceau 4R and Carmoisine Employing an Analytical Quality by Design-Aided RP-HPLC Method in Commercial Food Samples Utilizing a Green Ultrasound-Assisted Extraction Technique.","authors":"Atyurmila Chakraborty, Kavitha Jayaseelan","doi":"10.1093/jaoacint/qsae020","DOIUrl":"10.1093/jaoacint/qsae020","url":null,"abstract":"<p><strong>Background: </strong>Ponceau 4R (E124) and carmoisine (CMS; E122) are frequently utilized azo synthetic dyes in the food industry owing to their aesthetically pleasing coloration and broad consumer acceptability. It is imperative to prioritize environmentally favorable technologies for quantifying these dyes, as excessive consumption of these poses significant health risks.</p><p><strong>Objective: </strong>The primary objective of this research was to establish a reversed-phase (RP)-HPLC method that could simultaneously detect Ponceau 4R and CMS, implementing green analytical chemistry (GAC) and analytical quality by design (AQbD), using an ultrasound-assisted extraction (UAE) technique in commercial food samples.</p><p><strong>Methods: </strong>An Agilent Eclipse Plus column (C18, 250 × 4.6 mm id, 5 µm) was utilized for effective separation with a mobile phase of ethanol-acetate buffer pH 5 (60:40, v/v), flow rate of 1 mL/min, and detection wavelength of 515 nm. Critical variables selected for method optimization were ethanol percentage and flow rate, determined using central composite design (CCD). In order to adhere to the 12 principles of green chemistry, hazardous solvents were substituted with ethanol, which is distinguished by its ease of use, effectiveness, and ecological sustainability. The greenness assessment was conducted utilizing the green analytical procedure index (GAPI), analytical eco-scale (AES), and analytical greenness metrics (AGREE).</p><p><strong>Results: </strong>The respective retention times for Ponceau 4R and CMS were 2.276 and 3.450 min. The recovery rate of Ponceau 4R and CMS fluctuated between 70% and 102% and 80% and 102%, respectively, across various marketed food samples. The procedure passed validation in accordance with the International Conference on Harmonization Q14 guidelines.</p><p><strong>Conclusion: </strong>The devised method demonstrates that the validation parameters like linearity, precision, sensitivity, and reproducibility are within the specified limits of ICH guidelines. The greenness assesment tools GAPI, AES, and AGREE produced the most favorable results.</p><p><strong>Highlights: </strong>In future, environmentally sustainable, solvent-based, robust AQbD methodologies for assessing varieties of food colorants may be adopted and improved commercially.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"430-442"},"PeriodicalIF":0.0,"publicationDate":"2024-05-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140066315","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 Mass Spectrometry-Based Method for Quantification of Total Cashew Protein in Roasting Oil.","authors":"Shimin Chen, Melanie L Downs","doi":"10.1093/jaoacint/qsae019","DOIUrl":"10.1093/jaoacint/qsae019","url":null,"abstract":"<p><strong>Background: </strong>Food allergen cross-contact during food preparation and production is one of the causes of unintentional allergen presence in packaged foods. However, little is known about allergen cross-contact in shared frying or roasting oil, which prevents the establishment of effective allergen controls and may put allergic individuals at risk. To better understand the quantity of allergen transferred to frying oil and subsequent products, an analytical method is needed for quantifying protein in oil that has been exposed to frying/roasting conditions.</p><p><strong>Objective: </strong>The goal of this study was to develop a parallel reaction monitoring LC-MS/MS method to quantify the amount of cashew protein in shared roasting oil.</p><p><strong>Methods: </strong>The sample preparation method was evaluated to improve protein extractability and peptide performance. Four quantitative peptides representing cashew 2S and 11S proteins were selected as targets based on their sensitivity, heat stability, and specificity. A calibration strategy was developed to quantify the amount of total cashew protein in oil. Method performance was evaluated using a heated cashew-in-oil model system.</p><p><strong>Results: </strong>The method showed high recovery in oil samples spiked with 100 or 10 parts per million (ppm) total cashew protein heated at 138 or 166°C for 2-30 min. Samples (100 ppm total cashew protein) heated for 30 min had more than 90% recovery when treated at 138°C and more than 50% when heated at 166°C.</p><p><strong>Conclusion: </strong>The method is fit-for-purpose for the analysis of cashew allergen cross-contact in oil.</p><p><strong>Highlights: </strong>A novel MS-based method was developed that can accurately quantify the amount of cashew protein present in heated oil.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"443-452"},"PeriodicalIF":0.0,"publicationDate":"2024-05-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140013848","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":"AMR Threat Perception Assessment of Heterotrophic Bacteria From Shrimp Aquaculture Through Epidemiological Cut off Values.","authors":"Ranjit Kumar Nadella, Satyen Kumar Panda, Anuj Kumar, Devananda Uchoi, Pankaj Kishore, Madhusudana Rao Badireddy, Pani Prasad Kuricheti, Ram Prakash Raman, Mukteswar Prasad Mothadaka","doi":"10.1093/jaoacint/qsae011","DOIUrl":"10.1093/jaoacint/qsae011","url":null,"abstract":"<p><strong>Background: </strong>Emergence and dissemination of antibiotic resistance is one of the major risks associated with the rampant usage of antibiotics in food-producing animals including aquaculture.</p><p><strong>Objective: </strong>To determine Epidemiological Cut-OFF (ECOFF) values of heterotrophic bacterial populations from shrimp culture environments against five different antibiotics.</p><p><strong>Methods: </strong>In this present study, bacterial samples were isolated from Penaeus vannamei culture environment in different locations of Andhra Pradesh, which is the aquaculture hub of India. The bacterial isolates were assessed for antibiotic resistance towards five antibiotics belonging to different classes (oxytetracycline, chloramphenicol, erythromycin, ciprofloxacin, and co-trimoxazole) by the disc diffusion method. Determination of Epidemiological Cut-OFF (ECOFF) values and analysis by employing normalized resistance interpretation (NRI) was carried out.</p><p><strong>Results: </strong>The most dominant bacterial populations from shrimp culture were Vibrio spp. (pathogenic bacteria) followed by Bacillus spp. (probiotic bacteria). The bacterial isolates showed highest resistance towards oxytetracycline (overall 23.38%) and in location L6 (59.4%) followed by co-trimoxazole (31.1%). ECOFF values calculated by employing NRI showed that the disc diffusion data were distributed in a normalized manner. The maximum ECOFF value was obtained for ciprofloxacin (23.32 mm), while the minimum value was observed for oxytetracycline (9.05 mm). The antibiotic resistant phenotypes showed that the majority of the heterotrophic bacterial isolates (>60%) belonged to the non-wild type phenotype and primarily towards oxytetracycline (90%).</p><p><strong>Conclusion: </strong>The presence of non-wild antibiotic-resistant phenotypes of heterotrophic bacterial populations (which include not only pathogenic bacteria but also probiotic bacteria) indicates that shrimp culture ponds may be a reservoir for drug-resistant bacteria and there is a greater risk associated with transmission of resistant genes across bacterial flora.</p><p><strong>Highlights: </strong>NRI analysis of antibiotic disc diffusion data of heterotrophic bacterial populations in shrimp aquaculture environments revealed that majority of them belonged to non-wild type (90%) paticularly to oxytetracycline in comparison to other studied antibiotics (chloramphenicol, erythromycin, ciprofloxacin and co-trimoxazole).</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"479-486"},"PeriodicalIF":0.0,"publicationDate":"2024-05-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139747920","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}
Jonatas Lobato Duarte, Leonardo Delello Di Filippo, Alberto Gomes Tavares, Marlus Chorilli
{"title":"Analytical Method for Quantifying Monoterpenoids (p-Cymene and Myrcene) in Nanoemulsions Using High-Performance Liquid Chromatography.","authors":"Jonatas Lobato Duarte, Leonardo Delello Di Filippo, Alberto Gomes Tavares, Marlus Chorilli","doi":"10.1093/jaoacint/qsae012","DOIUrl":"10.1093/jaoacint/qsae012","url":null,"abstract":"<p><strong>Background: </strong>Myrcene and cymene, aromatic monoterpenes found in plants and essential oils, possess distinctive aromatic qualities. However, their volatility and limited solubility pose challenges in precise handling and formulation. Meanwhile, nanoemulsions emerge as promising drug delivery systems, improving the bioavailability and stability of these active ingredients.</p><p><strong>Objective: </strong>This article aimed to develop an HPLC method for the quantification of two monoterpenoids, p-cymene and myrcene, in nanoemulsions.</p><p><strong>Method: </strong>The method used a Phenomenex® Synergi™ Fusion-RP column (150 mm × 4.6 mm id, 4 μm particle size) on an HPLC system with isocratic elution. The mobile phase was composed of acetonitrile and water (60:40, v/v) and was validated in terms of specificity, linearity, accuracy, precision, robustness, and selectivity.</p><p><strong>Results: </strong>The method provided accurate and precise results with a correlation coefficient of 0.999 and RSD values of less than 2%. The method can be used for quality control of nanoemulsions containing these monoterpenoids and as a reference for future studies on their efficacy and stability.</p><p><strong>Conclusions: </strong>The study demonstrates the feasibility of using HPLC for the quantification of monoterpenoids in nanoemulsions and its potential as a quality control tool for nanoemulsion-based drug delivery systems.</p><p><strong>Highlights: </strong>The method's accuracy, precision, and reliability, as evidenced by high correlation coefficients and low RSD values, underscore its suitability for ensuring the consistent formulation of these monoterpenoid-containing nanoemulsions, while also serving as a reference point for future research endeavors in this field.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"506-511"},"PeriodicalIF":0.0,"publicationDate":"2024-05-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139944813","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":"Variation in Botanical Reference Materials: Similarity of Actaea Racemosa Analyzed by Flow Injection Mass Spectrometry.","authors":"James Harnly, Roy Upton","doi":"10.1093/jaoacint/qsad137","DOIUrl":"10.1093/jaoacint/qsad137","url":null,"abstract":"<p><strong>Background: </strong>Botanical reference materials (BRMs) generally account for the species, cultivar, and year and location of harvest that result in variability in the chemical composition that may lead to statistically significant differences using chemometric methods.</p><p><strong>Objective: </strong>To compare the chemical composition of five species of Actaea root BRMs, four herbal sources of A. racemosa root BRMs, and A. racemosa BRMS, and commercial roots and supplements using chemometric methods and selected pre-processing approaches.</p><p><strong>Method: </strong>Samples were analyzed by flow injection mass spectrometry (FIMS), principal component analysis (PCA), and factorial multivariate analysis of variance (mANOVA).</p><p><strong>Results: </strong>Statistically significant (P = 0.05) compositional differences were found between three genera (Actaea, Panax, and Ginkgo), five species of Actaea (A. racemosa, A. cimicifuga, A. dahurica, A. pachypoda, and A. rubra) root BRMs, four herbal sources of A. racemosa root BRMs, and A. racemosa BRMS and commercial roots and supplements. The variability of 6% of the BRM variables was found to be quantitatively conserved and reduced the compositional differences between the four sources of root BRMs. Compositional overlap of A. racemosa and other Actaea BRMs was influenced by variation in technical repeats, pre-processing methods, selection of variables, and selection of confidence limits. Sensitivity ranged from 94 to 97% and specificity ranged from 21 to 89% for the pre-processing protocols tested.</p><p><strong>Conclusions: </strong>Environmental, genetic, and chemometric factors can influence discrimination between species and authentic botanical reference materials.</p><p><strong>Highlights: </strong>Frequency distribution plots derived from soft independent modeling of class analogy provide excellent means for understanding the impact of experimental factors.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"332-344"},"PeriodicalIF":0.0,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10907137/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139033116","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}
Elisabeth Halbmayr-Jech, Roman Kittl, Patrick Weinmann, Christopher Schulz, Anna Kowalik, Matthias König, Jasmin Korp, Christoph Sygmund, Sharon L Brunelle
{"title":"Determination of Lactose in Lactose-Free and Low-Lactose Milk, Milk Products, and Products Containing Dairy Ingredients by the LactoSens®R Amperometry Method: Final Action 2020.01.","authors":"Elisabeth Halbmayr-Jech, Roman Kittl, Patrick Weinmann, Christopher Schulz, Anna Kowalik, Matthias König, Jasmin Korp, Christoph Sygmund, Sharon L Brunelle","doi":"10.1093/jaoacint/qsad120","DOIUrl":"10.1093/jaoacint/qsad120","url":null,"abstract":"<p><strong>Background: </strong>The LactoSens®R method was previously shown to have acceptable accuracy and repeatability precision as required by AOAC Standard Method Performance Requirements (SMPR®) 2018.009 for determination of lactose in low-lactose or lactose-free milk, milk products, and products containing dairy ingredients and was awarded Official Method of AnalysisSM (OMA) First Action status in 2020.</p><p><strong>Objective: </strong>The method was subjected to a multilaboratory validation (MLV) study to evaluate the reproducibility precision of the method.</p><p><strong>Methods: </strong>Fourteen validation materials were provided to 15 laboratories in seven countries as blind duplicates. The materials ranged from 0 to 173 mg/100 g lactose. Each laboratory analyzed the blind duplicates according to OMA 2020.01. The data were analyzed for repeatability and reproducibility precision.</p><p><strong>Results: </strong>RSDr values varied from 2.81 to 8.76%, and RSDR values varied from 4.25 to 12.5%. When sorted by category and concentration range, these results met the repeatability and reproducibility criteria required by SMPR 2018.009.</p><p><strong>Conclusions: </strong>The data generated in the MLV support the adoption of OMA 2020.01 as Final Action status.</p><p><strong>Highlights: </strong>The LactoSensR method, as described by OMA 2020.01, provides an accurate and precise determination of lactose in a variety of low-lactose and lactose-free milk, milk products, and products containing dairy ingredients in minutes.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"254-259"},"PeriodicalIF":0.0,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41160416","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":"Simultaneous Determination of Amphenicols in Animal-Derived Foods by Solvent and Solid Phase Extraction With Ultrahigh-Performance Liquid Chromatography Tandem Mass Spectrometry.","authors":"Feng Liu, Yaya Yan, Yi Yao, Yingxu Qin, Fei Xu","doi":"10.1093/jaoacint/qsad127","DOIUrl":"10.1093/jaoacint/qsad127","url":null,"abstract":"<p><strong>Background: </strong>The consumption of foods containing amphenicols, a type of antibiotic, is a major concern for human health. A stable and accurate detection method can provide technical support for food-safety monitoring.</p><p><strong>Objective: </strong>An effective and efficient method was established for determining amphenicols in animal-derived foods through the simultaneous use of solid-phase extraction (SPE) cleanup and ultrahigh-performance liquid chromatography/mass spectrometry (UPLC-MS/MS).</p><p><strong>Method: </strong>Samples were extracted using 1.0% ammoniated ethyl acetate solution, degreased with n-hexane, and then concentrated and cleaned using a C18 SPE column. Next, gradient elution was performed using methanol and 0.05% aqueous ammonia as the mobile phase, followed by separation using a C18 column. The target compound was detected using electrospray ionization, both in positive and negative modes, through multiple reaction monitoring, and quantified using an internal-standard method.</p><p><strong>Results: </strong>The content of chloramphenicol (CAP), florfenicol (FF), and florfenicol amine (FFA) (content range: 0.2-8.0 µg/kg) as well as that of thiamphenicol (TAP; content range: 1.0-40.0 µg/kg) show a good linear relationship, with a correlation coefficient of r > 0.999. Furthermore, recoveries of 86.7-111.9% and relative standard deviations of <9.0% were achieved. The limits of detection and quantification are obtained as 0.03-0.33 and 0.1-1.0 μg/kg, respectively.</p><p><strong>Conclusions: </strong>The proposed method has excellent stability and accuracy, and can be successfully used for the qualitative and quantitative determination of amphenicols, i.e., CAP, TAP, FF, and FFA residues in 210 animal-derived food samples, of which FF and FFA were detected in four samples.</p><p><strong>Highlights: </strong>A stable and accurate method was successfully established for the simultaneous determination of CAP, TAP, FF, and FFA in animal-derived foods using UPLC-MS/MS. Effective sample pretreatment was established, lipids were removed using n-hexane, concentration and cleanup were achieved with the C18 SPE column, and matrix effects were effectively reduced, thus improving the method's accuracy and stability. The method was validated for eight common animal-source foods, including beef, lamb, pork, chicken, egg, milk, fish, and honey. This method has good applicability for CAP, TAP, FF, and FFA in animal-derived foods.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"267-276"},"PeriodicalIF":0.0,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138471397","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":"Sugar Profile Method by High-Performance Anion-Exchange Chromatography with Pulsed Amperometric Detection in Food, Dietary Supplements, Pet Food, and Animal Feeds: Interlaboratory Validation Study, Final Action 2018.16.","authors":"Andrew J Ruosch, David J Ellingson","doi":"10.1093/jaoacint/qsad138","DOIUrl":"10.1093/jaoacint/qsad138","url":null,"abstract":"<p><strong>Background: </strong>A method for sugar profile analysis granted First Action 2018.16 was subjected to a multi-laboratory study.</p><p><strong>Objective: </strong>Perform a multi-laboratory study with this method to determine the performance parameters of repeatability and reproducibility against the AOAC Standard Method Performance Requirements (AOAC SMPR 2018.001) for Final Action status.</p><p><strong>Methods: </strong>Eleven laboratories from three different countries participated in the study. Each laboratory was provided practice materials for successful method setup. Each laboratory then proceeded with analysis of blind duplicates of 10 different products covering the scope of the method. Results were reported to the study directors with any modifications and assessed following the procedures of Appendix D of the AOAC Official Methods of AnalysisSM (guidelines for collaborative study procedures).</p><p><strong>Results: </strong>The majority of results from the study met the SMPR requirements. The data is presented along with any outlying observations or modifications. The method was proven to be flexible across different instrumentation and laboratories, and the method was updated to provide further system suitability and guidelines to maintain the performance of the method across the large scope of matrixes.</p><p><strong>Conclusion: </strong>The results from the collaborative study supported the method for Final Action status. The Expert Review Panel reviewed and voted to move the method forward to Final Action and was followed by review from the Official Methods Board and granted approval.</p><p><strong>Highlights: </strong>The method was granted Final Action Official Methods status.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"303-319"},"PeriodicalIF":0.0,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139033115","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}