Wafaa El-Ghaly, Lamia Zaari Lambarki, Taha El Kamli, Adnane Benmoussa, Fadil Bakkali, Nour-Iddin Bamou, Taoufiq Saffaj, Fayssal Jhilal
{"title":"A Comparative Analysis of Analytical Validation Approaches for Quality Assurance: Exploring Holistic Strategies in the Validation of Quantitative Methods-A Case Study of Hesperidin.","authors":"Wafaa El-Ghaly, Lamia Zaari Lambarki, Taha El Kamli, Adnane Benmoussa, Fadil Bakkali, Nour-Iddin Bamou, Taoufiq Saffaj, Fayssal Jhilal","doi":"10.1093/jaoacint/qsaf004","DOIUrl":"10.1093/jaoacint/qsaf004","url":null,"abstract":"<p><strong>Background: </strong>Analytical validation is a sequence of operations aiming to evaluate the accuracy, reliability, and cost of analytical results for making informed decisions in method selection and meeting the requirements of regulatory institutions.</p><p><strong>Objective: </strong>This study aims to perform an analytical validation by comparing three different approaches: the accuracy profile, the uncertainty profile, and the conventional validation to assess the capability of each method in confirming the robustness of the results.</p><p><strong>Methods: </strong>The accuracy profile offers a comprehensive assessment of analytical performance and integrates systematic and random errors to determine if future results will satisfy the predefined acceptance limits. Meanwhile, the uncertainty profile, which is complementary and innovative, allows uncertainty estimation from validation data. These approaches were developed after conventional validation that relies on statistical methodologies based on separate evaluations of method criteria to provide a comparative framework for evaluating new methods.</p><p><strong>Results: </strong>This comparison will give recommendations for best practices related to analytical validation. The uncertainty profile is a graphical decision-making tool for determining full validation by integrating analytical validation and the estimation of measurement uncertainty, evaluating two statistical methods: β-expectation tolerance intervals and β-content, γ-confidence tolerance intervals, using a formula introduced by Saffaj and Ihssane, predicting that 95% of future results will fall within the acceptance limits of ±5%, revealing that the tolerance intervals for β-expectation are smaller than β-content, γ-confidence.</p><p><strong>Conclusion: </strong>The total error approaches offer robust recommendations for optimal methods for routine application.</p><p><strong>Highlights: </strong>This study highlights the critical need for appropriate analytical validation and the challenges arising from the absence of clear guidelines for that purpose. Different approaches emphasize the significant impact of the choice of an adequate method, which remains pivotal for providing accurate results in real-world scenarios. Concrete examples and simulations illustrate the viewpoints associated with different approaches to making decisions.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"435-448"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143071302","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 and Characterization of Acidic Degradation Products of Moxidectin Drug Substance Including Degradation Pathways Using LC, HRMS, and NMR.","authors":"Tyler C Huang, Ayesha Nisathar, Frank Rinaldi","doi":"10.1093/jaoacint/qsae096","DOIUrl":"10.1093/jaoacint/qsae096","url":null,"abstract":"<p><strong>Background: </strong>Moxidectin is an active pharmaceutical ingredient (API) extensively used in various drug products within the pharmaceutical and animal health sectors. Despite its widespread use, the analytical methods prescribed by the United States Pharmacopeia (USP) and European Pharmacopoeia (EP, Ph. Eur.) exhibit significant limitations. These methods fail to adequately separate key impurities of (23Z)-moxidectin (EP impurity L) and 3,4-epoxy-moxidectin, potentially affecting the quality control, purity assessment, and safety of moxidectin-containing products.</p><p><strong>Objective: </strong>The objective was to develop and validate an alternative, improved stability-indicating high-performance liquid chromatography (HPLC) method for the identification, assay, and quantification of related substances in the moxidectin drug substance, along with the analysis of its degradation pathways.</p><p><strong>Methods: </strong>High-resolution mass spectrometry (HRMS) and nuclear magnetic resonance (NMR) were employed to comprehensively examine moxidectin and its two degradation products under specified acidic conditions. The degradation products were isolated and identified using a range of analytical techniques, including HRMS, NMR, and other relevant methods.</p><p><strong>Results: </strong>The epoxy derivative of moxidectin (relative retention time [RRT] = 1.2) was not identified under the studied acidic degradation conditions. HRMS data indicated that the degradant at RRT = 1.2 is an isomer of moxidectin, as it exhibited an identical molecular ion. Detailed NMR studies on moxidectin and its impurity at RRT-1.2 revealed differences in carbon and proton chemical shifts at positions C-22 and C-24, strongly supporting the identification of the structure as an oxime geometric isomer of moxidectin, i.e. (23Z)-moxidectin.</p><p><strong>Conclusions: </strong>The findings revealed specific degradation products formed under acidic conditions, offering valuable insights into the chemical transformations of moxidectin. This information is crucial for assessing the drug's stability profile and ensuring the quality and safety of moxidectin-containing products.</p><p><strong>Highlights: </strong>The HPLC method developed in this study significantly improves on existing USP/EP methods with regard to a separation of key impurities of (23Z)-moxidectin and 3,4-epoxy-moxidectin, offering robust performance for routine analysis of bulk moxidectin API batches and stability samples in quality control (QC) laboratories.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"320-336"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142824979","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":"Retraction of: Differentiation Between Humic and Non-Humic Substances Using Alkaline Extraction and Ultraviolet Spectroscopy.","authors":"","doi":"10.1093/jaoacint/qsae102","DOIUrl":"10.1093/jaoacint/qsae102","url":null,"abstract":"","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"488"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12048169/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143018609","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":"The Effects of Compound Starter Culture, Sugar, and Soy Milk on the Quality and Probiotic Activity of Milk-Soy Mixed Yogurt.","authors":"Wenxie Jiang, Sungjun Han, Lu Wang, Xinxin Li","doi":"10.1093/jaoacint/qsaf001","DOIUrl":"10.1093/jaoacint/qsaf001","url":null,"abstract":"<p><strong>Background: </strong>Yogurt has emerged as an essential nutritional food in contemporary diets, and the development of new multi-component yogurt formulations has become a focal point of current research.</p><p><strong>Objective: </strong>In this study, the effects of fermentation compounds and the addition of sugar and soy milk on the quality and probiotic activity of milk-soy mixed yogurt were studied to determine the optimal formation of mixed yogurt.</p><p><strong>Methods: </strong>The various fermentation compounds (YO-MIX 883, Lactobacillus casei complex starter cultures, and L. paracasei compound starter cultures), different concentrations of milk-soy additions (0, 25, 50, 75, and 100%) and sugar (2, 4, 6, and 8%) were tested within each experimental group, and the pH, appropriate acidity, and total viable bacterial count of the fermented milk-soy mixed yogurt were determined throughout the fermentation and refrigeration processes.</p><p><strong>Results: </strong>The obtained results showed that the L. paracasei complex was particularly effective for the fermentation of soy milk. The mixed yogurt formulation, comprising 50% soy milk and 4∼6% sucrose, exhibited enhanced acidity, superior sensory evaluation scores, and overall improved product quality. It was observed that during refrigeration an increase in the milk content of yogurt corresponded to a more pronounced post-acidification effect. The optimal formulation for the milk-soy mixed yogurt identified in this research consisted of 0.3% L. paracasei compound fermenter, 6% sucrose, and 40% soy milk. Under these optimal conditions, the mixed yogurt achieved an acidity level of 76°T, a sensory score of 92 points, and a survival index of 1.25. Additionally, the yogurt exhibited a distinctive soybean aroma in its aftertaste, contributing to its overall quality. Furthermore, the probiotic survival index of the mixed yogurt containing 40% soy milk, following simulated gastrointestinal fluid digestion, was recorded at 0.767, indicating that the probiotic activity in this yogurt was significantly higher than that of other yogurts.</p><p><strong>Conclusion: </strong>The obtained results provide a theoretical foundation for the future industrial production of milk-soy mixed yogurt products.</p><p><strong>Highlights: </strong>The mixed yogurt formulation, comprising 50% soy milk and 4∼6% sucrose, exhibited overall improved product quality. L. paracasei complex was more suitable for the fermentation of soy milk. Sucrose was more suitable for the fermentation of mixed yogurt. The more milk was added, the stronger the post-acidification effect of yogurt during refrigeration. The milk-soy mixed yogurt with high probiotic activity following artificial simulation of gastrointestinal fluid digestion had the potential for industrial production.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"380-394"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142934319","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}
Eni Themeli, Tam Mai, Fereidoun Forghani, Mansour Samadpour
{"title":"Performance Validation of the IEH Laboratories Multiplex PCR Listeria Detection System for Environmental Samples in Comparison to Health Canada Reference Method (MFHPB-30) for Listeria Detection.","authors":"Eni Themeli, Tam Mai, Fereidoun Forghani, Mansour Samadpour","doi":"10.1093/jaoacint/qsaf013","DOIUrl":"10.1093/jaoacint/qsaf013","url":null,"abstract":"<p><strong>Background: </strong>Laboratory detection methods are commonly tested against gold standards and corresponding reference methods to confirm their suitability and efficiency.</p><p><strong>Objective: </strong>The IEH Listeria Test System (multiplex PCR) was tested against Health Canada's reference method (MFHPB-30) for the simultaneous detection of Listeria spp. and Listeria monocytogenes on three different surfaces: plastic (PL), sealed concrete (SC), and stainless steel (SS).</p><p><strong>Methods: </strong>The R2 medium was used for pre-enrichment of the samples at 35°C for 24 h, followed by the IEH Listeria multiplex PCR. Each individual surface coupon (PL, SC, and SS) was inoculated with either Listeria innocua, L. monocytogenes, or L. welshimeri along with two non-target microorganisms of concern and subjected to candidate (IEH Listeria multiplex PCR) and reference method (MFHPB-30) testing in an unpaired manner, including culture confirmation for the IEH method.</p><p><strong>Results: </strong>The candidate method demonstrated 0% false negative, 0% false positive, 100% sensitivity, and 100% specificity after only 24 h enrichment followed by multiplex PCR.</p><p><strong>Conclusions: </strong>Evaluating the differences between the candidate and reference method detection probabilities across all three surface types revealed that the candidate method was equivalent to MFHPB-30, while requiring significantly less time for detection.</p><p><strong>Highlights: </strong>IEH Listeria system performed equivalently to the reference method, without being affected by the surface type and while decreasing the detection time to a total of less than 28 hours.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"422-428"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143470435","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}
Marleen van Aardt, Andrew R Komarek, Michael Roche, Elise Ivarsen
{"title":"Validation of an Automated Method for the Isolation and Purification of Fat-Soluble Vitamins and Cholesterol for Chromatographic Analysis.","authors":"Marleen van Aardt, Andrew R Komarek, Michael Roche, Elise Ivarsen","doi":"10.1093/jaoacint/qsaf011","DOIUrl":"10.1093/jaoacint/qsaf011","url":null,"abstract":"<p><strong>Background: </strong>The isolation and purification of vitamins A, E, D, and cholesterol from food and feed test materials, for quantitation, is currently a time-consuming and labor-intensive process. It includes separate steps for saponification, extraction, purification, and solvent evaporation. A new instrument (FLEX) was developed that improves and automates all steps involved, and which uses solid-phase extraction (SPE). This study validates the FLEX automated method.</p><p><strong>Objectives: </strong>The objective of this study was to validate the automated method by recovery of standards, analysis of reference materials, comparison against proficiency test materials, and comparison against manual reference methods.</p><p><strong>Methods: </strong>The FLEX instrument automatically adds reagents, mixes, and heats to saponify test materials, filters the digestate, extracts with SPE, and evaporates solvent.</p><p><strong>Results: </strong>The accuracy of the automated FLEX instrument method was confirmed by the agreement with National Institute of Standards and Technology (NIST) reference materials for retinol, α-tocopherol, cholecalciferol, ergocalciferol, and cholesterol. Accuracy was also compared against manual reference methods on 11 different food types that ranged from 4-100% fat, 0-75% protein, and 0-85% carbohydrate. The automated and manual methods were highly correlated with no bias or distortion over the range of test materials. Precision was similar to the manual methods for retinol recovery but improved for α-tocopherol and cholecalciferol analysis. The accuracy of the automated method also was confirmed for feed analysis. Eleven different animal feeds were analyzed in the FLEX instrument and results were highly correlated with Association of American Feed Control Officials proficiency test results.</p><p><strong>Conclusion: </strong>The automated method accurately and efficiently performed the multiple analytical steps necessary for the isolation and purification of the analytes in preparation for chromatographic analysis.</p><p><strong>Highlights: </strong>The automated method was compared against industry standard methods and yielded equivalent results and improved precision. SPE technology was optimized to efficiently elute non-polar analytes, while retaining protein and other medium-polar analytes.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"412-421"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12048171/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143442891","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}
Hongjuan Chang, Qinghua Meng, Zhefeng Wu, Liu Tang, Zouquan Qiu, Chunyu Ni, Jiahui Chu, Juncheng Fang, Yuqing Huang, Yu Li
{"title":"Accurate Ripening Stage Classification of Pineapple Based on a Visible and Near-Infrared Hyperspectral Imaging System.","authors":"Hongjuan Chang, Qinghua Meng, Zhefeng Wu, Liu Tang, Zouquan Qiu, Chunyu Ni, Jiahui Chu, Juncheng Fang, Yuqing Huang, Yu Li","doi":"10.1093/jaoacint/qsaf010","DOIUrl":"10.1093/jaoacint/qsaf010","url":null,"abstract":"<p><strong>Background: </strong>Pineapples are a popular tropical fruit with economic value, and determining the optimum ripeness of pineapples to assess their quality is crucial for harvesting, marketing, production, and processing.</p><p><strong>Objective: </strong>In this study, spectral information and soluble solid content (SSC) of pineapple ripening stages (unripe, ripe, and overripe) were analyzed by 400-1000 nm hyperspectral imaging (HSI) in order to determine the best classification model of pineapple ripening.</p><p><strong>Methods: </strong>Four different preprocessing methods, i.e., standard normal variate (SNV), multiplicative scatter correction (MSC), normalization, and Savitzky-Golay (SG) smoothing, in combination with successive projection algorithms (SPA), and bootstrapping soft shrinkage (BOSS) for feature wavelength extraction, were used to compare the full wavelength and the two types of feature extraction support vector machine (SVM), extreme learning machine (ELM), K-nearest neighbors (KNN), and random forest (RF), four supervised machine learning classifiers for maturity classification.</p><p><strong>Results: </strong>For pineapple ripeness classification, SNV preprocessing RF showed the best results with 94.44% accuracy at both full wavelength and 28 wavelengths selected in SPA. A total of 33 wavelengths selected from BOSS achieved a test accuracy of 97.22% by RF.</p><p><strong>Conclusion: </strong>These results demonstrate the potential of near-infrared hyperspectral imaging (NIR-HSI) as a non-destructive, fast, and correct tool for pineapple ripeness identification. The method can be applied to classify and grade marketed pineapple fruits to address pineapple quality issues related to uneven ripeness.</p><p><strong>Highlights: </strong>The visible and near-infrared hyperspectral imaging (VIS-NIR-HSI) system combining machine learning and wavelength selection successfully classified pineapple ripening stages, an approach that could improve the ability to classify pineapples at the ripening stage in large packaging companies. In addition, finding key wavelengths or features that can be classified corresponding to pineapple ripening stages has the advantage of developing a low-cost, fast, and effective multispectral imaging system compared to the NIR-HSI system.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"293-303"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143451226","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 and Validation of a Single Stability-Indicating Reversed-Phase High-Performance Liquid Chromatography (RP-HPLC) Method for Identification and Assay of Eprinomectin in Two Different Commercial Injectable Drug Products for Cattle.","authors":"Nayanthara U Dharmaratne, Abu M Rustum","doi":"10.1093/jaoacint/qsaf006","DOIUrl":"10.1093/jaoacint/qsaf006","url":null,"abstract":"<p><strong>Background: </strong>Eprinomectin (EPRN) is a semi-synthetic macrocyclic lactone exhibiting antiparasitic activity and is widely used as an active pharmaceutical ingredient (API) in veterinary drug products.</p><p><strong>Objective: </strong>This study aimed to develop a single stability-indicating reversed-phase (RP)-HPLC method to identify and assay EPRN in two different injectable drug products for cattle.</p><p><strong>Methods: </strong>The RP-HPLC method is carried out on a Halo-C18 column (100 mm × 4.6 mm id, 2.7 µm particle size) maintained at 55°C. The analytes are separated by a gradient elution at a flow rate of 0.8 mL/min and detected at a wavelength of 245 nm. The mobile phase-A (MPA) of the method is 0.1% (v/v) aqueous perchloric acid, and mobile phase-B (MPB) is ethanol (EtOH). The Ascentis Express C18 column (100 mm × 4.6 mm id, 2.7 µm particle size) was identified and validated as an equivalent column for the prescribed method.</p><p><strong>Results: </strong>The RP-HPLC method described in this article can adequately separate all major related substances of EPRN in the two drug products from EPRN B1a and EPRN B1b within 20 min.</p><p><strong>Conclusion: </strong>The developed RP-HPLC method for the identification and assay of EPRN was successfully validated in accordance with the guidelines outlined in the International Conference on Harmonization (ICH) Q2(R2), and demonstrated to be robust, linear, accurate, precise, specific, and stability-indicating.</p><p><strong>Highlights: </strong>The new RP-HPLC method exhibits a higher level of selectivity but is yet rapid and simple, making it suitable for routine and non-routine analysis in research and QC laboratories.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"304-312"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143476964","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 Enzytec™ Liquid Acetic Acid for Enzymatic Determination of Acetic Acid in Selected Foods and Beverages: Official Method 2024.01 First Action.","authors":"Markus Lacorn, Thomas Hektor","doi":"10.1093/jaoacint/qsaf015","DOIUrl":"10.1093/jaoacint/qsaf015","url":null,"abstract":"<p><strong>Background: </strong>In the food industry, acetic acid is used as a food additive acidity regulator (code E260), in the form of vinegar as a condiment and in the pickling of vegetables and other foods. For wine and juices there are threshold values for acetic acid. Enzytec™ Liquid Acetic acid is an enzymatic test kit based on acetate kinase activity for the determination of acetic acid.</p><p><strong>Objective: </strong>The aim of this study was to validate the Enzytec method in a single laboratory for determination of acetic acid in wines, juices, kombucha, beer, sausage meat, sauces/remoulades, and culture media for microbiology.</p><p><strong>Methods: </strong>The method was evaluated for selectivity, ruggedness, stability, LOD, LOQ, linearity, dilutability, and method performance in wine, juices, beer, kombucha, sauces, culture media, and sausage meat.</p><p><strong>Results: </strong>The test is specific to acetic acid and shows no relevant interferences. The calculated LOD for a test volume of 100 µL is 2.2 mg/L and the LOQ is 3.8 mg/L. The practical upper measurement range is 1300 mg/L for a test volume of 100 µL. Spiking of wine, juice, kombucha, beer, sauces, sausages, and culture media for microbiology resulted in recoveries between 88 and 103%. Intermediate precision was between 1.8 and 3.8%. For automation, two applications with different test volumes and different measurement ranges were validated. Linearity was demonstrated from 8 mg/L up to 6.2 g/L (depending on the test volume).</p><p><strong>Conclusion: </strong>The method is robust and accurate for manual and automated applications. The method was accepted as a First Action Official MethodSM.</p><p><strong>Highlights: </strong>The ready-to-use components of the test kit have a shelf life of 25 months.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"395-411"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12048170/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143560483","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":"Quality Analysis of Peanut Oils and Peanut Diacylglycerol Edible Oils After Frying Using Raman Spectroscopy Combined with Oil Microscopy Method.","authors":"Lingli Liu, Rui Liu, Zhenshi Chen, Yuanpeng Li, Mengjiao Xue, Meiyuan Chen, Wenchang Huang, Hanglin Lu, Jian Tang, Shan Tu, Jun Liu, Junhui Hu","doi":"10.1093/jaoacint/qsaf002","DOIUrl":"10.1093/jaoacint/qsaf002","url":null,"abstract":"<p><strong>Background: </strong>The thermal stability and quality of fats change during oil-frying, directly impacting food safety and nutritional value; however, traditional analysis methods are time-consuming and complex.</p><p><strong>Objective: </strong>This study aimed to develop a rapid monitoring protocol using a portable Raman spectrometer for peanut oils and peanut diacylglycerol (DAG) edible oils after frying zero to five times at 150°C.</p><p><strong>Methods: </strong>Raman spectral data and the acid and peroxide values were determined for 48 oil test samples. Raman spectral data were analyzed using the characteristic band intensity ratio method and oil microscopy method.</p><p><strong>Results: </strong>The peroxide values of peanut oil correlated with I729/I1076, I1076/I1300, and I1268/I1655 (I: Raman spectral intensity; subscript: wave number corresponding to Raman shift), whereas the acid and peroxide values of peanut DAG edible oil correlated with I863/I1655, I1076/I1300, and I1268/I1655. Oil microscopy method analysis revealed that the fried peanut DAG oil had higher trans-fatty acid and acid values (AV) and lower unsaturated fatty AVs than regular peanut oil. Furthermore, oil microscopy method revealed changes in the functional groups of the oils and fats, further elucidating the quality changes that occur in oils and fats after frying.</p><p><strong>Conclusion: </strong>Raman spectroscopy combined with oil microscopy method can be used to rapidly monitor the quality of frying oil after frying.</p><p><strong>Highlights: </strong>Peanut DAG oil is more oxidatively stable after frying than peanut oil; a characteristic band intensity ratio method can be used to classify frying oils; the peroxide value of peanut oil is related to I729/I1076, I1076/I1300, and I1268/I1655; the acid and peroxide values of peanut DAG edible oil are related to I863/I1655, I1076/I1300, and I1268/I1655; oil microscopy method revealed oil functional group changes and could improve frying quality analysis.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"337-347"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143784665","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}