Journal of AOAC International最新文献

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Validation of an Automated Method for the Isolation and Purification of Fat-Soluble Vitamins and Cholesterol for Chromatographic Analysis. 用于色谱分析的脂溶性维生素和胆固醇的自动分离和纯化方法的验证。
Journal of AOAC International Pub Date : 2025-05-01 DOI: 10.1093/jaoacint/qsaf011
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}
引用次数: 0
Accurate Ripening Stage Classification of Pineapple Based on a Visible and Near-Infrared Hyperspectral Imaging System. 基于可见和近红外高光谱成像系统的菠萝成熟期精确分类。
Journal of AOAC International Pub Date : 2025-05-01 DOI: 10.1093/jaoacint/qsaf010
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}
引用次数: 0
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. 单稳定指示反相高效液相色谱(RP-HPLC)法测定两种牛用注射药品中依普诺菌素的建立与验证。
Journal of AOAC International Pub Date : 2025-05-01 DOI: 10.1093/jaoacint/qsaf006
Nayanthara U Dharmaratne, Abu M Rustum
{"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}
引用次数: 0
Validation of Enzytec™ Liquid Acetic Acid for Enzymatic Determination of Acetic Acid in Selected Foods and Beverages: Official Method 2024.01 First Action. 用于酶法检测某些食品和饮料中醋酸含量的 Enzytec™ 液体醋酸的验证:官方方法 2024.01 首次行动。
Journal of AOAC International Pub Date : 2025-05-01 DOI: 10.1093/jaoacint/qsaf015
Markus Lacorn, Thomas Hektor
{"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}
引用次数: 0
Quality Analysis of Peanut Oils and Peanut Diacylglycerol Edible Oils After Frying Using Raman Spectroscopy Combined with Oil Microscopy Method. 用拉曼光谱结合油显微技术分析花生油和花生二酰基甘油食用油油炸后的质量。
Journal of AOAC International Pub Date : 2025-05-01 DOI: 10.1093/jaoacint/qsaf002
Lingli Liu, Rui Liu, Zhenshi Chen, Yuanpeng Li, Mengjiao Xue, Meiyuan Chen, Wenchang Huang, Hanglin Lu, Jian Tang, Shan Tu, Jun Liu, Junhui Hu
{"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}
引用次数: 0
Comprehensive Screening of Per- and Polyfluoroalkyl Substances (PFAS) in Food Contact Materials: Utilizing Combustion Ion Chromatography for Total Organic Fluorine (TOF) Analysis. 食品接触材料中全氟和多氟烷基物质(PFAS)的综合筛选:利用燃烧离子色谱法进行总有机氟(TOF)分析。
Journal of AOAC International Pub Date : 2025-05-01 DOI: 10.1093/jaoacint/qsaf003
Jingli Hu, Richard E Cochran, Cynthia M Grim, Neil G Rumachik
{"title":"Comprehensive Screening of Per- and Polyfluoroalkyl Substances (PFAS) in Food Contact Materials: Utilizing Combustion Ion Chromatography for Total Organic Fluorine (TOF) Analysis.","authors":"Jingli Hu, Richard E Cochran, Cynthia M Grim, Neil G Rumachik","doi":"10.1093/jaoacint/qsaf003","DOIUrl":"10.1093/jaoacint/qsaf003","url":null,"abstract":"<p><strong>Background: </strong>Per- and polyfluoroalkyl substances (PFAS) comprise thousands of fluorinated chemicals. They are of growing concern because many PFAS compounds are persistent and toxic. Food contact materials (FCMs) containing PFAS pose multiple exposure pathways to humans, prompting 12 states to enact laws banning FCMs with PFAS levels exceeding 100 ppm total organic fluorine (TOF).</p><p><strong>Objective: </strong>While LC-MS is often used to measure targeted PFAS compounds, much of the total PFAS content in the sample may be missed. To understand organic fluorine content in samples more comprehensively, we developed a method using combustion ion chromatography (CIC) to measure TOF and extractable organic fluorine (EOF) in FCMs.</p><p><strong>Methods: </strong>This technology utilizes combustion under an oxygen and argon atmosphere. All gaseous, acidic combustion products are collected in water, with ions separated on an ion-exchange column and detected by conductivity. Total fluorine (TF) was measured by combusting 10-50 mg FCM. Total inorganic fluorine (TIF) was measured by extracting cryo-ground FCM with water followed by direct injection to the ion chromatography (IC) system. TOF was then calculated by subtracting TIF from TF. EOF was determined by CIC after extracting analytes from the ground FCM using methanol-acetonitrile (80 + 20, by volume).</p><p><strong>Results: </strong>The method detection limit (MDL) for TOF is 0.51 ppm, exceeding the sensitivity requirements of current state regulations. A comparison of EOF to TOF revealed that EOF constitutes less than 15% of the TOF in the FCM samples.</p><p><strong>Conclusion: </strong>TOF is a critical metric for assessing PFAS contamination in FCMs, as targeted LC-MS approaches may miss much of the PFAS in the samples.</p><p><strong>Highlights: </strong>We developed a sensitive and automated method to determine TOF and EOF in FCMs. The method can be used to screen for PFAS in FCMs, ensuring compliance with current regulations on PFAS contamination.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"367-379"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143018225","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
Development of Reference Material for White Granulated Sugar. 白砂糖标准物质的研制。
Journal of AOAC International Pub Date : 2025-05-01 DOI: 10.1093/jaoacint/qsae101
Guihua Wang, Jiawei Li, Ailing Xiao, Jianjin Chen, Qiuting Ping, Juan Yu, Yufeng Gao, Qiaoyun Cheng
{"title":"Development of Reference Material for White Granulated Sugar.","authors":"Guihua Wang, Jiawei Li, Ailing Xiao, Jianjin Chen, Qiuting Ping, Juan Yu, Yufeng Gao, Qiaoyun Cheng","doi":"10.1093/jaoacint/qsae101","DOIUrl":"10.1093/jaoacint/qsae101","url":null,"abstract":"<p><strong>Background: </strong>White granulated sugar, a significant commodity in bulk trade and a widely used raw material, plays a crucial role in the food, energy, and medicine industries. A certified reference material (CRM) for white granulated sugar provides a valuable tool for monitoring and maintaining the safety and quality of white granulated sugar and other related products. The colorimetric value, conductivity ash, sucrose content, and reducing sugar content serve as essential factors that determine the quality of white granulated sugar.</p><p><strong>Objective: </strong>A CRM for grade one white granulated sugar was developed. A comprehensive study was carried out to assess its homogeneity and stability, and then the designated property values were determined.</p><p><strong>Methods: </strong>Collaborative certification across 11 laboratories was applied to validate its property values and evaluate corresponding uncertainties.</p><p><strong>Results: </strong>The designated property values and expanded uncertainties (k = 2) were determined to be 75.6 ± 2.8 IU, 0.0100 ± 0.0004 g/100g, 99.71 ± 0.08 g/100g, and 0.0226 ± 0.0024 g/100g for colorimetric value, conductivity ash, sucrose content, and reducing sugar content, respectively.</p><p><strong>Conclusion: </strong>The reference material (RM) was sufficiently homogeneous between and within bottles and remained stable for up to 20 months.</p><p><strong>Highlights: </strong>The developed CRM of sugar could be an effective support for method validation, capability validation, QC, and metrological traceability in the sugar and food industries.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"472-478"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142808887","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
Co-Estimating Estradiol Valerate and Medroxyprogesterone Acetate in a Combined Hormonal Product: A Novel Short Runtime UPLC Method. 联合激素产品中戊酸雌二醇和醋酸甲孕酮的联合测定:一种新的短时间UPLC方法。
Journal of AOAC International Pub Date : 2025-05-01 DOI: 10.1093/jaoacint/qsaf016
Erdal Dinç, Adem Mert
{"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":"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 QC and accurate analysis of hormones in tablets used for hormone replacement therapy (HRT).</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 HRT tablets.</p><p><strong>Methods: </strong>Chromatographic separation of EV and MPG was achieved using an ACQUITY UPLC BEH C18 (1.7 μm, 2.1 × 100 mm) column and a mixture containing water-acetonitrile-methanol-0.10 M phosphate buffer pH 2.14 (6:44:42:8, v/v). 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 time 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>Conclusion: </strong>This validated UPLC method is a cost-effective and efficient tool for routine quality control of EV and MPG in HRT tablets, ensuring reliable pharmaceutical analysis.</p><p><strong>Highlights: </strong>This study introduces the first ultra-performance liquid chromatography with photodiode array detection (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":"313-319"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","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}
引用次数: 0
Chemical Fingerprints Combined with Chemometric Analysis to Evaluate and Distinguish Between Plantago Asiatica L. and Plantago Depressa Willd. 化学指纹图谱结合化学计量学分析评价和区分车前草和大车前草。
Journal of AOAC International Pub Date : 2025-05-01 DOI: 10.1093/jaoacint/qsaf023
Guoqiang Liu, Zicheng Ma, Jinli Wen, Xiaoran Zhao, Yanru Deng, Lili Sun, Xiaoliang Ren
{"title":"Chemical Fingerprints Combined with Chemometric Analysis to Evaluate and Distinguish Between Plantago Asiatica L. and Plantago Depressa Willd.","authors":"Guoqiang Liu, Zicheng Ma, Jinli Wen, Xiaoran Zhao, Yanru Deng, Lili Sun, Xiaoliang Ren","doi":"10.1093/jaoacint/qsaf023","DOIUrl":"10.1093/jaoacint/qsaf023","url":null,"abstract":"<p><strong>Background: </strong>Plantago, also known as plantain, has been used as a traditional herb in Asia for centuries to treat urinary tract inflammation and kidney disease. Recently, there has been increasing interest in its potential applications in the food industry. In China, there are two common species, namely Plantago asiatica L. (PAL) and P. depressa Willd. (PDW), which are not distinguished in folk and clinical practices, leading to safety and efficacy risks in plantago applications.</p><p><strong>Objectives: </strong>The objective of this study is to establish a reliable method for differentiating and evaluating the quality of PAL and PDW by integrating fingerprint analysis with multivariate chemometrics.</p><p><strong>Methods: </strong>HPLC was used to collect characteristic chemical information from the whole plant in 13 PAL and 18 PDW samples, establishing fingerprints for the different species. Multiple chemometric methods, including hierarchical cluster analysis (HCA), principal component analysis (PCA), and partial least-squares discriminant analysis (PLS-DA), were employed to analyze the chemical differences between the two species and to identify chemical markers. Finally, the differences in the content of the three chemical markers in the two plantago samples were determined and analyzed.</p><p><strong>Results: </strong>The analysis revealed a distinct classification of PAL and PDW into two groups. Significant differences were observed in the content of key components such as plantamajoside, acteoside, and isoacteoside between the two species.</p><p><strong>Conclusion: </strong>This study provides a reliable scientific basis for the rational application and quality evaluation of plantago. The findings contribute to ensuring the safe and effective use of plantago in various applications.</p><p><strong>Highlights: </strong>HPLC fingerprinting combined with chemometrics identified three key markers distinguishing PAL and PDW, supporting quality control and medicinal development.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"479-487"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143712290","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
FTIR Spectroscopic Analysis of Plant Proteins and Correlation with Functional Properties. 植物蛋白的FTIR光谱分析及其与功能特性的相关性
Journal of AOAC International Pub Date : 2025-05-01 DOI: 10.1093/jaoacint/qsaf005
Janvi D Patel, Zili Gao, Lili He
{"title":"FTIR Spectroscopic Analysis of Plant Proteins and Correlation with Functional Properties.","authors":"Janvi D Patel, Zili Gao, Lili He","doi":"10.1093/jaoacint/qsaf005","DOIUrl":"10.1093/jaoacint/qsaf005","url":null,"abstract":"<p><strong>Background: </strong>The development of plant-based products faces challenges like raw material standardization and time-consuming functionality measurements. FTIR spectroscopy provides a quick, non-destructive way to analyze protein molecular characteristics.</p><p><strong>Objective: </strong>This study explored the classification capability of FTIR in analyzing five plant protein isolates-soy, mung bean, pea, fava bean, and lentil-and assessed its predictive ability for functional property measurement such as water absorption capacity (WAC), oil absorption capacity (OAC), solubility (SOL), foaming, and emulsification.</p><p><strong>Methods: </strong>Functional properties were calculated using traditional methods of measurements. Principal component analysis (PCA) and partial least-squares (PLS) regression analysis were used to study FTIR spectra and their correlation with functional properties.</p><p><strong>Results: </strong>PCA revealed distinct clusters for each protein source based on their FTIR spectra, indicating molecular differences. WAC and OAC prediction models showed strong correlations, with prediction correlation coefficients (Rp) of more than 0.99 and cross-validation correlation coefficients (Rcv) ranging from 0.85 to 0.92. Models for SOL and emulsifying activity index (EAI) display promising potential. Moreover, WAC and OAC predictions exhibited robust results with protein blends of various ratios. The expanded WAC model predicted with an Rp of 0.99 and an Rcv of 0.95, while the expanded OAC model had an Rp of 0.99 and an Rcv of 0.84.</p><p><strong>Conclusion: </strong>The results underscore FTIR has the potential to identify plant proteins, aiding in raw material verification and QC as well as being an alternative to analyzing functional properties of plant proteins.</p><p><strong>Highlights: </strong>This study demonstrates the potential of FTIR spectroscopy as a rapid, non-destructive tool for plant protein characterization and functional property prediction. FTIR successfully distinguished five plant protein isolates-soy, mung bean, pea, fava bean, and lentil-through PCA-based spectral clustering. Strong predictive models for water and oil absorption capacities (WAC and OAC) were developed, with prediction correlation coefficients (Rp) values exceeding 0.99 and cross-validation correlation coefficients (Rcv) ranging from 0.84 to 0.95. Functional property predictions for solubility (SOL) and emulsifying activity index (EAI) showed promising potential. These findings highlight FTIR's capability for protein classification, raw material verification, and rapid functional property assessment in quality control applications.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"348-356"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143191557","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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