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A Contemporary Look at the Precision of Modern Analytical Methods in Food Analysis and the Relevance of the Horwitz Equation. 现代食品分析方法的精确性和霍维茨方程的相关性。
Journal of AOAC International Pub Date : 2025-07-01 DOI: 10.1093/jaoacint/qsaf026
Stefan Ehling, Joseph J Thompson, Karen J Schimpf, Lawrence H Pacquette, Philip A Haselberger
{"title":"A Contemporary Look at the Precision of Modern Analytical Methods in Food Analysis and the Relevance of the Horwitz Equation.","authors":"Stefan Ehling, Joseph J Thompson, Karen J Schimpf, Lawrence H Pacquette, Philip A Haselberger","doi":"10.1093/jaoacint/qsaf026","DOIUrl":"10.1093/jaoacint/qsaf026","url":null,"abstract":"<p><strong>Background: </strong>The Horwitz equation models an empirically observed relationship between inter-laboratory relative standard deviation RSDR and analyte concentration expressed as a mass fraction. The Horwitz ratio (HorRat) is the ratio of observed RSDR to the corresponding calculated RSDR from the Horwitz equation. The empirical acceptable range is 0.5 to 2.0 for a successful multi-laboratory method validation trial.</p><p><strong>Objective: </strong>This work examines data from multi-laboratory trials on food analyses conducted between 2011 and 2017 for trends in analytical method precision and the applicability and relevance of the Horwitz model.</p><p><strong>Methods: </strong>Data on method precision from 20 multi-laboratory trials consisting of 961 data points were analyzed. The scope was limited to methods employing modern chromatographic and spectroscopic techniques and to well-defined small-molecule analytes and elements. Within-laboratory and inter-laboratory precision and their ratio, HorRat, goodness of fit to the Horwitz model, and variation of precision across the analytical range were examined.</p><p><strong>Results: </strong>The variance of inter-laboratory precision is largely (86%) independent of concentration and remains unexplained by the Horwitz equation. Only 52% of all data points fell within the Horwitz band (0.5-2.0), with 46% falling under 0.5, indicating substantially better inter-laboratory precision than predicted by the Horwitz equation at all concentration levels. Near-constant precision was confirmed across the analytical range of methods, even near the limit of quantitation.</p><p><strong>Conclusion: </strong>The analysis of the data in scope demonstrates that the analytical method precision routinely achievable with modern chromatographic and spectroscopic techniques, proper laboratory controls, and training is much better than that predicted by the Horwitz equation. HorRat has lost its relevance as a method performance criterion for judging the success of a multi-laboratory trial.</p><p><strong>Highlights: </strong>Recent data do not follow the Horwitz model. HorRat values <0.5 can be routinely achieved. Method precision is mostly independent of analyte concentration. Method-related factors have greater impact on precision.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"566-571"},"PeriodicalIF":0.0,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143665784","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}
引用次数: 0
Determination of Folic Acid in Various Dietary Supplement Dosage Forms by UPLC/PDA: Single-Laboratory Validation, First Action 2024.09. 不同膳食补充剂剂型中叶酸的UPLC/PDA测定:单实验室验证,第一行动2024.09。
Journal of AOAC International Pub Date : 2025-07-01 DOI: 10.1093/jaoacint/qsaf014
Lusi A, Mina Fakhary, Jennifer M Solano, Mohamed Koroma
{"title":"Determination of Folic Acid in Various Dietary Supplement Dosage Forms by UPLC/PDA: Single-Laboratory Validation, First Action 2024.09.","authors":"Lusi A, Mina Fakhary, Jennifer M Solano, Mohamed Koroma","doi":"10.1093/jaoacint/qsaf014","DOIUrl":"10.1093/jaoacint/qsaf014","url":null,"abstract":"<p><strong>Background: </strong>The AOAC Expert Review Panel (ERP) approved a method for the quantification of folic acid in various dietary supplement dosage forms containing tablets, 2-piece capsules, powder drinks, softgels, and gummies with First Action Official MethodSM status.</p><p><strong>Objective: </strong>The previously published method summarized a single-laboratory validation with parameters of linearity, LOD, LOQ, repeatability, recovery, specificity, and system suitability. Based on the request from the ERP, the recovery test for the gummies has been reperformed with a revised procedure.</p><p><strong>Methods: </strong>Determination of Folic Acid in Various Dietary Supplement Dosage Forms UPLC/PDA.</p><p><strong>Results: </strong>The recovery range of 94.6-106.5% was achieved by spiking 20, 50, and 80% in the gummy samples. Other adjustments or clarification of the method and minor typos were also addressed.</p><p><strong>Conclusion: </strong>After the revised method, report, and results were analyzed and discussed, the ERP adopted the method and provided recommendations for achieving Final Action status.</p><p><strong>Highlights: </strong>The revised method meets the requirements of Standard Method Performance Requirement (SMPR®) 2022.002.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"658-659"},"PeriodicalIF":0.0,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144210571","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}
引用次数: 0
Quality Evaluation of Gluten-Free Pasta Enhanced With Carboxymethyl Cellulose Gum: Rheological Properties, Characterization, Cooking Tests, and Sensory Analysis. 羧甲基纤维素胶增强无麸质面食的质量评价:流变特性、表征、烹饪试验和感官分析。
Journal of AOAC International Pub Date : 2025-07-01 DOI: 10.1093/jaoacint/qsaf042
Mahsa Mohseni, Peyman Mahasti Shotorbani, Afshin Akhondzadeh Basti, Yeganeh Azimi
{"title":"Quality Evaluation of Gluten-Free Pasta Enhanced With Carboxymethyl Cellulose Gum: Rheological Properties, Characterization, Cooking Tests, and Sensory Analysis.","authors":"Mahsa Mohseni, Peyman Mahasti Shotorbani, Afshin Akhondzadeh Basti, Yeganeh Azimi","doi":"10.1093/jaoacint/qsaf042","DOIUrl":"10.1093/jaoacint/qsaf042","url":null,"abstract":"<p><strong>Background: </strong>The increasing prevalence of gluten-related disorders, such as celiac disease, has raised the demand for gluten-free (GF) products, highlighting a significant economic and public health challenge.</p><p><strong>Objective: </strong>The purpose of this study is to create high-quality, nutritious GF pasta using rice flour, corn starch, pregelatinized starch, and carboxymethyl cellulose gum (CMC) as a substitute for semolina.</p><p><strong>Methods: </strong>To assess the impact of CMC on pasta dough quality, samples with 0.5, 1, and 1.5% CMC were prepared, along with a control (0% CMC) and a semolina sample. The resulting pasta was analyzed for chemical properties, cooking quality, texture, color, and sensory evaluation, comparing it to the control, a market GF pasta, and semolina pasta.</p><p><strong>Results: </strong>Rheological analysis showed that the storage modulus (G') was higher than the loss modulus (G'') in all formulations. Semolina pasta had a protein content of 13%, which was higher than that of the prepared GF pasta (4%) and market samples (8%). The addition of CMC reduced cooking loss from 11.07% (0% CMC) to 7.31% (1.5% CMC). Colorimetric assessments showed no significant differences among the GF samples. The sample with 1% CMC had the best texture and cooking quality.</p><p><strong>Conclusion: </strong>The addition of 1% CMC improves dough rheology, product quality, and consumer acceptance as an effective gluten substitute. This research highlights the potential of CMC gum to improve GF pasta quality, meeting consumer expectations for taste and texture while also inspiring innovations in various GF products across various food categories.</p><p><strong>Highlights: </strong>GF pasta was made using rice flour and corn starch. Adding 1% CMC improved the sensory evaluation, texture, and cooking quality of the GF pasta, with no significant effect on its color. In the frequency tests, G' was consistently greater than G'', indicating that the doughs were more elastic than viscous.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"539-548"},"PeriodicalIF":0.0,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144251604","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}
引用次数: 0
Unfolding the Nutraceutical Potentials of Dendrobium Nobile Lindl Orchid Flowers Based on Their Color Variation: A High-Resolution Mass Spectrometry-Based Untargeted Metabolomics Study. 基于颜色变化揭示石斛兰花的营养潜力:基于高分辨率质谱的非靶向代谢组学研究。
Journal of AOAC International Pub Date : 2025-07-01 DOI: 10.1093/jaoacint/qsaf025
Suman Natta, Nasiruddin Shaikh, Ekatpure Sachin, Amine Kassouf, Nishant Deshmukh, Sankar Prasad Das, Kaushik Banerjee
{"title":"Unfolding the Nutraceutical Potentials of Dendrobium Nobile Lindl Orchid Flowers Based on Their Color Variation: A High-Resolution Mass Spectrometry-Based Untargeted Metabolomics Study.","authors":"Suman Natta, Nasiruddin Shaikh, Ekatpure Sachin, Amine Kassouf, Nishant Deshmukh, Sankar Prasad Das, Kaushik Banerjee","doi":"10.1093/jaoacint/qsaf025","DOIUrl":"10.1093/jaoacint/qsaf025","url":null,"abstract":"<p><strong>Background: </strong>Dendrobium nobile is an edible orchid with diverse therapeutic properties. In northeastern Himalayan states of India, the extract of this flower is consumed by tribal populations for the treatment of diabetes, cancer, and cardiovascular diseases. However, the profile of biologically active compounds in the colored varieties of D. nobile orchid flowers cultivated in the northeastern Himalayan region is not well established, necessitating a thorough investigation.</p><p><strong>Objective: </strong>This study aims to establish and compare the metabolite profile of three types of D. nobile flowers (white, light pink, and dark pink) using liquid chromatography-high-resolution mass spectrometry (LC-HRMS).</p><p><strong>Methods: </strong>The homogenized and cryoground flower samples were extracted with aqueous methanol. After LC-MS data acquisition through full-scan (untargeted) and MS/MS (targeted) modes, data processing involved peak alignment, adduct identification, and integration. Results were compared by multivariate statistics using independent component analysis.</p><p><strong>Results: </strong>A total of 73 metabolites was identified, each with mass error of less than 5 ppm for both precursor and fragment ions. From anthocyanin classes, the chemometric analysis revealed 11 distinguishing biomarker metabolites, with variable influence on projection values above 1. Across the test accessions, three compounds, viz. cyanidin-3-diglucoside, delphinidin-3-sophoroside, and delphinidin-3-gentiobioside, revealed their discriminatory presence.</p><p><strong>Conclusions: </strong>The study identified the therapeutically important anthocyanins for metabolomic discrimination of three different D. nobile flower accessions. The study will be useful for authenticating D. nobile accessions, derived products, and selecting candidate traits for future breeding programs for varietal improvements.</p><p><strong>Highlights: </strong>This study identified and profiled the bioactive anthocyanin compounds in D. nobile orchid flowers grown in the northeastern Himalayan region of India, based on color variations using a non-target metabolomics approach.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"628-636"},"PeriodicalIF":0.0,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143665693","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}
引用次数: 0
Correction to: The Validation of the Wheat Gluten ELISA Kit. 更正:小麦面筋酶联免疫吸附测定试剂盒的验证。
Journal of AOAC International Pub Date : 2025-07-01 DOI: 10.1093/jaoacint/qsaf021
{"title":"Correction to: The Validation of the Wheat Gluten ELISA Kit.","authors":"","doi":"10.1093/jaoacint/qsaf021","DOIUrl":"10.1093/jaoacint/qsaf021","url":null,"abstract":"","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"660"},"PeriodicalIF":0.0,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143665785","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}
引用次数: 0
Full Validation of an HPLC-UV Analytical Method for Azithromycin Quantification Using Comparative Approaches: Total Error and ISO-GUM for Assessment of Uncertainty. 用比较方法对HPLC-UV阿奇霉素定量分析方法进行充分验证:总误差和ISO-GUM不确定度评估。
Journal of AOAC International Pub Date : 2025-07-01 DOI: 10.1093/jaoacint/qsaf044
Wafaa El-Ghaly, Asmae Elouari, Lamia Zaari Lambarki, Samir Ahid, Taha El Kamli, Adnane Benmoussa, Fadil Bakkali, Nour-Iddin Bamou, Taoufiq Saffaj, Fayssal Jhilal
{"title":"Full Validation of an HPLC-UV Analytical Method for Azithromycin Quantification Using Comparative Approaches: Total Error and ISO-GUM for Assessment of Uncertainty.","authors":"Wafaa El-Ghaly, Asmae Elouari, Lamia Zaari Lambarki, Samir Ahid, Taha El Kamli, Adnane Benmoussa, Fadil Bakkali, Nour-Iddin Bamou, Taoufiq Saffaj, Fayssal Jhilal","doi":"10.1093/jaoacint/qsaf044","DOIUrl":"10.1093/jaoacint/qsaf044","url":null,"abstract":"<p><strong>Background: </strong>Azithromycin is a complex molecule derived from erythromycin. The control of its dosage in conventional release tablets requires the analytical validation of its method to ensure accurate quantification and provide confidence in the reliability of the results for informed decision-making.</p><p><strong>Objective: </strong>This study aims to validate an innovative method for azithromycin quantification using the accuracy profile. Additionally, a comparison is made between the uncertainty measurements calculated from the validation data using two formulas proposed by Feinberg et al. and Saffaj and Ihssane and contrasted with the ISO GUM approach.</p><p><strong>Methods: </strong>A liquid chromatography system intended for azithromycin analysis equipped with a reversed-phase C18 stationary phase consisting of octadecyl silyl vinyl polymer in a UV detector operating at 210 nm at a temperature of 40°C in isocratic elution using a mobile phase of acetonitrile and dipotassium hydrogen phosphate buffer (6.7 g/L), in the fraction of (60:40, v/v) at pH = 8.</p><p><strong>Results: </strong>The various accuracy profiles are illustrated to ensure that a known quantity of anticipated findings acquired through the method stand inside the tolerance interval of 95% and remain within the previously set acceptance limits of ±5%. Measurement uncertainty provides comparable values using both formulas of the total error approach. However, it was observed that the ISO-GUM approach tends to overestimate the expanded uncertainty. Specifically, while the ISO-GUM approach provides a rigorous framework, the use of the validation data offers a more empirical uncertainty estimation.</p><p><strong>Conclusion: </strong>The approach based on the total error grants the ability to accurately close the routine uncertainty, emphasizing a complete validation.</p><p><strong>Highlights: </strong>The proposed method is robust for pharmaceutical application, demonstrating good accuracy, with 95% of tolerance and uncertainty limits falling within the predefined acceptance limits of ±5%.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"506-518"},"PeriodicalIF":0.0,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144059156","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}
引用次数: 0
Ochratoxin A in Human Milk From the MIREC Study. 母乳中的赭曲霉毒素A来自MIREC研究。
Journal of AOAC International Pub Date : 2025-07-01 DOI: 10.1093/jaoacint/qsaf051
Iulia Popa, The Minh Luong, Tye E Arbuckle, Jillian Ashley Martin, Terence Koerner, Jason Carere
{"title":"Ochratoxin A in Human Milk From the MIREC Study.","authors":"Iulia Popa, The Minh Luong, Tye E Arbuckle, Jillian Ashley Martin, Terence Koerner, Jason Carere","doi":"10.1093/jaoacint/qsaf051","DOIUrl":"10.1093/jaoacint/qsaf051","url":null,"abstract":"<p><strong>Background: </strong>Ochratoxin A (OTA) is a mycotoxin produced by multiple fungal species and is found in a variety of foods. Ingestion of OTA-contaminated foods by lactating mothers can lead to OTA exposure in infants.</p><p><strong>Methods: </strong>To help assess infants' exposure to OTA, milk samples from the Maternal-Infant Research on Environmental Chemicals (MIREC) Human Milk Study were analyzed. Human milk samples were collected (n = 494) and analyzed for OTA levels by HPLC.</p><p><strong>Results and discussion: </strong>The mean OTA concentration was 7.32 ± 9.25 ng/L, with 390 (79%) test samples testing positive for OTA and a range of 4.5-192 ng/L. Based on the food consumption questionnaires distributed among participants, higher OTA levels were observed with higher consumption of cottage cheese, hot cereal, and whole-grain bread and significant differences were found in OTA levels at different sites. The mean OTA level in the analyzed milk test samples was well below the amount found in infant formulas sold in Canada, which was determined by Health Canada to be safe.</p><p><strong>Conclusions: </strong>The concentrations of OTA found in human milk in this study are well below the amount deemed safe in infant formula by Health Canada and, therefore, unlikely to be of concern to infant health.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"652-657"},"PeriodicalIF":0.0,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144175586","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}
引用次数: 0
Method Development for Determining β-Nicotinamide Mononucleotide (NMN) in Cosmetics Using m-PFC-HPLC. m-PFC-HPLC法测定化妆品中β-烟酰胺单核苷酸(NMN)的方法建立。
Journal of AOAC International Pub Date : 2025-07-01 DOI: 10.1093/jaoacint/qsaf017
Tao Lan, Wenyu Zhang, Hongtao Chu, Zhenyu Yun, Bin Qu
{"title":"Method Development for Determining β-Nicotinamide Mononucleotide (NMN) in Cosmetics Using m-PFC-HPLC.","authors":"Tao Lan, Wenyu Zhang, Hongtao Chu, Zhenyu Yun, Bin Qu","doi":"10.1093/jaoacint/qsaf017","DOIUrl":"10.1093/jaoacint/qsaf017","url":null,"abstract":"<p><strong>Background: </strong>As a new cosmetic ingredient, NMN is widely used in cosmetics production, but due to the lack of a detection method, QC of related products cannot be achieved.</p><p><strong>Objective: </strong>This study will develop a detection method for NMN in three matrixes (facial mask essence, emulsion, and cream) for QC of related cosmetics.</p><p><strong>Methods: </strong>Given the high ester content in facial emulsions and creams, which can hinder the detection of trace substances, a novel multi-plug filtration clean-up (m-PFC) purification column packed with multi-walled carbon nanotubes (MWCNTs) was employed to purify these matrixes. An HPLC method for NMN in three matrixes (facial mask essence, emulsion, and cream) was established. Methodological verification was conducted.</p><p><strong>Results: </strong>Results demonstrated a good linear relationship within a range of 5.0-500 μg/mL, with an LOQ of 5.0 mg/kg. The RSD of the precision experiment was less than 3%, and the RSD for six repeated experiments ranged from 1.2 to 5.3%, indicating the method's stability, reliability, and good repeatability. Recovery rates in the three cosmetic matrixes were between 93.9 and 109.4%, with an RSD below 3.7%. This method was applied to detect NMN content in seven cosmetics purchased from an e-commerce platform; NMN was not detected in some products claiming to contain NMN.</p><p><strong>Conclusion: </strong>This method had the advantages of simple operation, high sensitivity, and good accuracy, and provides technical support for cosmetic regulation.</p><p><strong>Highlights: </strong>Through this study, we should raise awareness and supervision of NMN cosmetics by establishing relevant standards.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"489-496"},"PeriodicalIF":0.0,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143805210","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}
引用次数: 0
Comparison of Neutral Detergent Fiber Analysis Methods for Feed Ingredients, Diets, and Feces of Pigs. 猪饲料原料、日粮和粪便中性洗涤纤维分析方法的比较。
Journal of AOAC International Pub Date : 2025-07-01 DOI: 10.1093/jaoacint/qsaf030
Yoojin Koh, Jeonghyeon Son, Beob Gyun Kim
{"title":"Comparison of Neutral Detergent Fiber Analysis Methods for Feed Ingredients, Diets, and Feces of Pigs.","authors":"Yoojin Koh, Jeonghyeon Son, Beob Gyun Kim","doi":"10.1093/jaoacint/qsaf030","DOIUrl":"10.1093/jaoacint/qsaf030","url":null,"abstract":"<p><strong>Background: </strong>An accurate determination of fiber concentrations in feeds and feces is critical for the measurement of fiber digestibility in pigs. The method of AOAC INTERNATIONAL for determining amylase-treated neutral detergent fiber (aNDF; Method 2002.04) has been widely used for pig diets. To overcome the complexity of the AOAC procedure, the Ankom method is also available for determining aNDF. Although these two methods have been compared for ruminant diets and feces, a comparison of the methods for pig diets and feces has not been documented.</p><p><strong>Objective: </strong>The objective was to compare aNDF values determined by the AOAC (aNDFAOAC) and the Ankom methods (aNDFAnkom) of ingredients, diets, and feces for pigs.</p><p><strong>Methods: </strong>A total of 255 test samples, consisting of 26 feed ingredients, 39 diets, and 190 feces of pigs, were analyzed for aNDF. To compare the AOAC Method 2002.04 and Ankom methods for aNDF, regression analyses were performed with the aNDFAnkom minus the mean aNDFAnkom as an independent variable and the aNDFAOAC minus the aNDFAnkom as a dependent variable.</p><p><strong>Results: </strong>The aNDFAnkom were greater than the aNDFAOAC by 2.90% (standard error = 0.63; P < 0.001) on average for ingredients and by 2.56% (standard error = 0.34; P < 0.001) on average for diets. For feces, the aNDFAnkom were greater than the aNDFAOAC by 1.30% (standard error = 0.32; P < 0.001) on average. The differences between the aNDFAnkom and aNDFAOAC were not consistent across the data ranges represented by a linear bias (slope = -0.16; standard error = 0.04; P < 0.001) in feces.</p><p><strong>Conclusion: </strong>ANDF concentrations determined by the Ankom method were greater than from the AOAC method in pig feeds and feces.</p><p><strong>Highlights: </strong>Despite convenience, the Ankom method yields greater aNDF values compared with the AOAC method.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"648-651"},"PeriodicalIF":0.0,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143733666","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}
引用次数: 0
Improving Reproducibility of HPTLC Analysis for Cranberry Supplements through Digitization and Chemometric Preprocessing. 通过数字化和化学计量预处理提高蔓越莓补充剂HPTLC分析的重现性。
Journal of AOAC International Pub Date : 2025-06-30 DOI: 10.1093/jaoacint/qsaf063
Mengliang Zhang, Jianghao Sun, Elizabeth Corwin, James M Harnly
{"title":"Improving Reproducibility of HPTLC Analysis for Cranberry Supplements through Digitization and Chemometric Preprocessing.","authors":"Mengliang Zhang, Jianghao Sun, Elizabeth Corwin, James M Harnly","doi":"10.1093/jaoacint/qsaf063","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf063","url":null,"abstract":"<p><strong>Background: </strong>High-performance thin-layer chromatography (HPTLC) is widely used for the identification and quality assessment of botanical supplements. However, traditional interpretation methods are subjective, and variability between plates hinders reproducibility and inter-plate comparisons.</p><p><strong>Objective: </strong>This study aimed to enhance the reproducibility and analytical utility of HPTLC by digitizing chromatograms and applying chemometric preprocessing to cranberry dietary supplement analysis.</p><p><strong>Method: </strong>Cranberry supplements of diverse dosage forms were extracted and analyzed using a standardized HPTLC protocol. Plates were derivatized with natural products and anisaldehyde reagents and imaged under multiple lighting conditions. Digital chromatograms were processed using normalization and retention factor (RF) alignment. Chemometric methods, including principal component analysis (PCA) and analysis of variance principal component analysis (ANOVA-PCA), were applied to assess variability and improve classification.</p><p><strong>Results: </strong>The digitization and preprocessing workflow significantly reduced plate-related variability while enhancing classification accuracy. RF alignment lowered between plate variance from 23% to 11%, while increasing sample-type variance from 59% to 79%. Combining data from multiple derivatization and imaging conditions improved chemical fingerprinting and enabled tighter clustering in PCA models.</p><p><strong>Conclusions: </strong>The integration of digitized HPTLC data with chemometric preprocessing modernizes the analytical workflow, improves reproducibility, and enables more robust and interpretable botanical fingerprinting. This approach supports improved quality control of botanical products and aligns with emerging standards for data transparency and reusability.</p><p><strong>Highlights: </strong>Digitization and alignment reduce HPTLC variability and enhance reproducibility. Combined profiles from multiple derivatization conditions improve sample classification. Chemometric analysis enables better interpretation and data-driven quality control and assessment for botanicals.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-06-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144532015","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}
引用次数: 0
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