Journal of AOAC International最新文献

{"title":"Exploring the changes of volatile compounds in crude and processed turmeric using GC-MS based volatilomics.","authors":"Xiaoliu Hu, Zhaoxiang Zeng, Chao Su, Chengwu Song, Rongzeng Huang, Sen Li, Shan Cao, Shuna Jin","doi":"10.1093/jaoacint/qsaf055","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf055","url":null,"abstract":"<p><strong>Background: </strong>It is a common practice to process crude turmeric (CT) using different approaches, however, limited research is available on the comparison of volatile organic compounds (VOCs) before and after the processing.</p><p><strong>Objective: </strong>This study investigated the impact of five different processing methods on the VOCs of CT before and after processing.</p><p><strong>Method: </strong>The five types of processed turmeric included vinegar-treated turmeric (VT), mussel powder-treated turmeric (MT), water extract of rice-processed turmeric (RT), stir-fried turmeric (ST), and wine-processed turmeric (WT). The gas chromatography-mass spectrometry (GC-MS) technique was utilized to identify the volatile profiles. Volatilomics based on multivariate statistics was used to assess the key metabolic differences between five processed turmeric and CT within the VOCs.</p><p><strong>Results: </strong>A total of 79 VOCs were detected between processed turmeric and CT, with terpenoids accounting for most of them. In the ST and WT groups, compared to the CT group, the number of changes in VOCs was relatively small, whereas in the VT, RT, and MT groups, there were a greater number of changes, with most metabolites exhibiting a downward trend. Through the volatilomics analysis, 13 potential differential compounds were screened out, among which there were three common differential compounds.</p><p><strong>Conclusions: </strong>This study reveals the primary causes for the variations in VOCs in processed and CT, establishing the groundwork for evaluating the overall quality of processed turmeric and its use in therapeutic settings.</p><p><strong>Highlights: </strong>The study systematically compared the effects of five different turmeric processing methods on VOCs using GC-MS-based volatilomics, providing a data reference for research on the changes in its pharmacological activity.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-05-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144176355","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":"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":"https://doi.org/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 analysed. 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 analysed 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":""},"PeriodicalIF":0.0,"publicationDate":"2025-05-28","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}

{"title":"Polydopamine-Coated Magnetic Molecularly Imprinted Polymers as a Dispersive SPE Adsorbent for Selective Recognition and Enrichment of Basic Orange 2 in Food Matrices with High-Performance Liquid Chromatography Analysis.","authors":"Meihua Hu","doi":"10.1093/jaoacint/qsaf054","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf054","url":null,"abstract":"<p><strong>Background: </strong>Basic orange 2, as an industial dye, exhibits severe effects to human health and has been forbidden to use as food additives in many countries. The practical use of common pretreatment process for basic orange 2 in food might be limited owing to time consuming, high consumption of solvents and weak selectivity. Therefore, the aim of this study was to validate a pre-treatment technology for basic orange 2 based on simplicity, being rapid, good selectivity, high sensitivity and inexpensiveness to ensure the tongue safety for people.</p><p><strong>Objectives: </strong>To develop a strategy for the extraction and enrichment of basic orange 2 in food matrices by the specific magnetic molecularly imprinted polymers prior to the determination by HPLC.</p><p><strong>Methods: </strong>The polymers with basic orange 2 as the template were deposited on the surface of ferroferric oxide nanoparticles (Fe3O4@PDA MIPs) through the self-assembly of dopamine in the weak alkaline solution. The Fe3O4@PDA MIPs as a disperse SPE sorbent were used for extracting and detecting basic orange 2 using HPLC. Parameters influencing extracting efficiencies were optimized, including the mass of MIPs, pH value, time for ultrasonication, elution solvent and volume.</p><p><strong>Results: </strong>Under optimal experimental conditions, the detection linearity of basic orange 2 was in the range of 0.04-1.0 μg/mL with correlation coefficient of 0.9991 and the limit of detection (LOD) of 5.8 ng/mL. The recoveries from spiked samples were 73.3%-90% with RSD 3.1%-8.1% in food samples. Notably, the magnetic MIPs showed an excellent reusability during 3 times extraction procedures.</p><p><strong>Conclusion: </strong>The Fe3O4@PDA MIPs prepared have great potential for purification and enrichment of basic orange 2 prior to its determination by HPLC in dried beancurd stick, yellow fish, chili powder, drinks and wine.</p><p><strong>Highlights: </strong>The magnetic MIPs developed show good adsorption performance for basic orange 2 with a very low detection, and excellent reusability. The assay was applied to detect basic orange 2 in food samples successfully.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-05-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144145143","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":"Discrimination of Rhizoma Paridis and its Adulterants by FT-IR and HPLC Fingerprint Combined with Chemometrics.","authors":"Lei Cheng, Jingjing Dong, Jun Qian, Yinglin Liu, Qingshu Yang, Xi Liu, Baozhong Duan","doi":"10.1093/jaoacint/qsaf052","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf052","url":null,"abstract":"<p><strong>Background: </strong>Rhizoma Paridis (RP) is economically significant but identifies complex traditional medicine materials, which can be accidentally contaminated, deliberately substituted, or admixed with other species of similar morphological characteristics. This issue can affect quality and safety issues.</p><p><strong>Objective: </strong>In this study, the screening technique to detect adulteration in RP was developed using multiple fingerprints and chemometrics.</p><p><strong>Methods: </strong>Fourier transforms infrared (FT-IR) spectroscopy and high-performance liquid chromatography (HPLC) combined with chemometrics, including similarity analysis (SA), principal component analysis (PCA), orthogonal partial least squares discriminant analysis (OPLS-DA), and hierarchical clustering analysis (HCA), were applied for the identification of RP and its adulterants.</p><p><strong>Results: </strong>HPLC analysis was more sensitive than FT-IR for differentiating RP from its contaminants. Except for the slight overlapping between Paris polyphylla var. chinensis (Franch.) Hand.-Mazz. and Paris mairei H.Lév., the remaining species could be successfully differentiated by the chemometrics method.</p><p><strong>Conclusion: </strong>This study indicates that the fingerprint of FT-IR and HPLC combined with chemometrics may be a valuable tool for discriminating RP and its adulterants.</p><p><strong>Highlights: </strong>FT-IR and HPLC combined with chemometrics analysis were developed to discriminate between RP and adulterants. The chemometrics analysis using SA and OPLS-DA indicate significant differentiation in the chemical composition of these species. This research provides important chemotaxonomic references in species identification.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-05-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144113142","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Development of a LC-MS/MS Method for the Determination of Lauric Arginate Ethyl Ester (E243) in Food.","authors":"Yiu-Tung Wong, Ka-Lok Chan, Odi Hang-Wah Yiu, Chun-Ching Chen, Ting-Wai Leung, Kin-Wai Yeung","doi":"10.1093/jaoacint/qsaf053","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf053","url":null,"abstract":"<p><strong>Background: </strong>Lauric arginate ethyl ester (LAE) is a natural cationic surfactant exhibiting excellent antimicrobial activity and has been approved as safe additive in certain food according to the Codex Alimentarius Commission (CAC) General Standard for Food Additives (GSFA).</p><p><strong>Objective: </strong>This study aimed to develop an analytical method based on liquid chromatography tandem mass spectrometry (LC-MS/MS) for the analysis of LAE in food using isotope-labeled LAE as internal standard.</p><p><strong>Method: </strong>LAE in food was extracted by a mixture of acetonitrile (ACN)/Water (9:1) and analyzed by LC-MS/MS via internal standard calibration method using LAE-d23 hydrochloride as internal standard.</p><p><strong>Results: </strong>The limit of detection (LOD) values of LAE were 0.32 mg/kg in liquid samples and 1.0 mg/kg in solid samples. The limit of quantitation (LOQ) values were 4.4 mg/kg and 14 mg/kg in liquid and solid samples, respectively. Spike recoveries consistently fell within the range of 90% to 110% at three different fortification levels, accompanied by %RSD below 10% in each instance.</p><p><strong>Conclusions: </strong>An analytical method with LC-MS/MS detection for the analysis of LAE in various food matrices was successfully developed, validated and demonstrated to be fast, robust and reliable.</p><p><strong>Highlights: </strong>The developed analytical method with LC-MS/MS detection offered a fast and efficient way to analyse LAE in various food samples during a routine food surveillance programme.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-05-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144082955","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Simultaneous determination of five alkaloids in extracted and non-extracted poppy APIs by HPLC.","authors":"QiuPing Huang, Chao Li, Ruifeng Hao, Hua Tang, Qin Feng, Huiyue Cheng, Chen Zhu, Jianhua Wang","doi":"10.1093/jaoacint/qsaf049","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf049","url":null,"abstract":"<p><strong>Background: </strong>Poppy Active Pharmaceutical Ingredients (APIs) are mainly used in the production of antitussives, analgesics, and other preparations. The alkaloid components play a major role, but the use of some alkaloids can cause dependence and toxic side effects in patients.</p><p><strong>Objective: </strong>The main aim of this study was to develop an effective and simple high-performance liquid chromatography (HPLC) for the simultaneous determination of five alkaloids in three APIs.</p><p><strong>Method: </strong>Waters XBridge C18 column (4.6 mm × 150 mm, 3.5 μm) was used as the chromatographic column. Mobile phase A was composed of 5.5 mmol/L sodium heptane sulfonate solution-acetonitrile-methanol-phosphoric acid (83:7:10:0.22, v/v/v/v), and Mobile phase B was composed of 5.5 mmol/L sodium heptane sulfonate solution-acetonitrile-methanol-phosphoric acid (60:15:25:0.45, v/v/v/v). The flow rate was 1.2 mL/min; The detection wavelength was 230 nm; The column temperature was 40 °C.</p><p><strong>Results: </strong>The HPLC method was suitable for the simultaneous determination of the contents of five alkaloids in three APIs. The verification experiment showed that the linear relationship of the five alkaloids in their respective ranges was good (R2 ≥ 0.998); The average recoveries ranged from 87.62 to 103.18%; The RSDs of repeatabilities were 0.3∼2.7%.</p><p><strong>Conclusions: </strong>In this study, a new HPLC method was developed and successfully validated. Compared with the determination method of opium alkaloids specified in Pharmacopoeia, this HPLC method does not need a complex sample pretreatment process, improves detection efficiency, avoids the use of highly corrosive reagents, and reduces the experimental risk. It can simultaneously meet the determination of five alkaloids in three APIs.</p><p><strong>Highlights: </strong>This method can simultaneously quantify five alkaloids in three poppy APIs without a complex sample pretreatment process and the application of strong corrosive solvents. It is applied to these APIs for the first time, expanding the scope of alkaloid analysis and providing new data for comparative studies of different API sources.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144056052","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":"Chromatographic Detection and Determination of Cyproheptadine and Dexamethasone as Adulterants in Weight Gain Supplements.","authors":"Arwa Ilyas Ahmed, Hasan Saad Aldewachi, Mohammed Ibrahim Aladul","doi":"10.1093/jaoacint/qsaf050","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf050","url":null,"abstract":"<p><strong>Background: </strong>The increasing popularity of herbal medicines and dietary supplements has raised concern about potential adulteration with pharmaceutical drugs.</p><p><strong>Objective: </strong>To detect and determine cyproheptadine (CYP) and dexamethasone (DEX) as adulterants in weight gain herbal supplements found in the Iraqi market.</p><p><strong>Methods: </strong>Nine herbal supplements marketed as natural weight gainers were purchased from local pharmacies and were screened using high-performance liquid chromatography (HPLC) for qualitative and quantitative detection of CYP and DEX.</p><p><strong>Results: </strong>CYP was detected in seven of the nine products at levels of 2.65-8.6 mg per dosage unit. DEX was detected in all test solutions at levels of 6.2-18.75 mg per dosage unit.</p><p><strong>Conclusion: </strong>A large proportion of herbal weight gain supplements were found to contain undeclared pharmaceuticals with severe health implications. The findings call for the immediate institution of tighter regulatory control and regular quality control tests in the name of consumer safety.</p><p><strong>Highlights: </strong>Herbals and supplements for weight gain are increasingly popular but may be adulterated with pharmaceutical drugs which impose serious health risks for consumers. Urgent need for regulatory enforcement and routine quality checks are recommended.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-05-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144059130","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":"Optimizing Salmonella Detection in Beijing's Surface Water: Unveiling Rare Serotypes with a Modified Moore Swab (MMS) Method.","authors":"Xueshuo Wang, Yue Dou, Jingyun Li, Yao Bai, Shenghui Cui","doi":"10.1093/jaoacint/qsae089","DOIUrl":"10.1093/jaoacint/qsae089","url":null,"abstract":"<p><strong>Background: </strong>Salmonella, a notorious foodborne pathogen with a wide range of hosts, poses a significant public health concern globally. Contaminated surface water acts as a potential source of Salmonella transmission.</p><p><strong>Objective: </strong>To optimize a Salmonella detection method from large-volume water and analyze surface water samples in Beijing and characterize Salmonella isolates from these samples by whole genome sequencing.</p><p><strong>Methods: </strong>A microbial enrichment device based on the modified Moore swab (MMS) design was optimized and validated. Thirty-five water samples were collected and analyzed for Salmonella from 11 park lakes, two rivers, and two farms. Multiple characteristics of isolates were analyzed using antibiotic antimicrobial testing and whole genome sequencing.</p><p><strong>Results: </strong>The optimized MMS unit showed high efficiency (over 80% recovery) and a low detection limit (100 cells) for enriching and isolating Salmonella from large-volume water (10 L). Compared to the conventional method, the MMS device significantly improved Salmonella detection efficiency (62.86 versus 8.57%) in Beijing's surface water. Most of the Salmonella isolates from surface water belonged to rare serotypes from water wildlife susceptible to all the tested antimicrbials.</p><p><strong>Conclusion: </strong>The study demonstrates the optimized MMS's effectiveness for on-site enrichment of pathogens from large-volume water, validates the accuracy and sensitivity of a Salmonella detection method for surface water, and reveals previously unknown information about Salmonella contamination in Beijing's public water system.</p><p><strong>Highlights: </strong>Salmonella concentrations in water are typically very low: implementation of this method would successfully realize large-volume water sampling and on-site pathogen enrichment, and significantly improve Salmonella detection efficiency in surface water.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"429-434"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143451278","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":"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}