Journal of AOAC International最新文献

{"title":"Development and Validation of a Capillary Zone Electrophoresis Method for the Determination of Lacosamide in Pharmaceutical Dosage Forms Using Box-Behnken Experimental Design.","authors":"Kadri Güleç, Dilek Ak","doi":"10.1093/jaoacint/qsag074","DOIUrl":"https://doi.org/10.1093/jaoacint/qsag074","url":null,"abstract":"<p><strong>Background: </strong>Lacosamide (LAC) is a third-generation antiseizure medication requiring reliable analytical methods for pharmaceutical quality control. No capillary electrophoresis (CE) method has been reported for its determination in dosage forms, and existing HPLC methods often involve high solvent consumption and limited sensitivity.</p><p><strong>Objective: </strong>To develop and validate a stability-indicating capillary zone electrophoresis method with diode array detection (CZE-DAD) for LAC determination in Lamide® tablets, optimized using a Box-Behnken design (BBD).</p><p><strong>Methods: </strong>Separation was performed by using a bare fused-silica capillary (40 cm effective length, 75 µm i.d.) with 5.7 mM sodium acetate buffer (pH 4.0) at ∼23 kV and peaks were detected at 210 nm. Metoprolol succinate served as the internal standard. ICH Q2(R1) guideline is followed for validation. Stability was assessed under five ICH stress conditions, and in vitro dissolution was profiled in gastric (0.1 N HCl, pH 1.2) and intestinal (PBS, pH 6.8) media.</p><p><strong>Results: </strong>The method demonstrated excellent linearity (r² = 0.9992) over 1.25 × 10⁻⁶ to 7.99 × 10⁻⁵ M, with LOD/LOQ of 0.034/0.102 µg/mL. Precision (%RSD) was <2.0%, and accuracy ranged from 99.61 to 101.81%. Mean LAC content in tablets was 98.21 ± 1.13% of the labelled amount. Forced degradation studies confirmed the stability-indicating capability of the method. In gastric medium, ≥95% release was achieved by 60-120 min; in intestinal medium, ≥95% was attained between 1 and 2 h.</p><p><strong>Conclusions: </strong>The first CZE-DAD method for determination of LAC in pharmaceutical tablets was successfully validated. It offers 2.5-3.5-fold superior sensitivity and higher separation efficiency (N > 12,000) compared to reported HPLC methods. Minimal solvent consumption aligns with green analytical chemistry principles, making this method well-suited for routine quality control.</p><p><strong>Highlights: </strong>First CE method reported for the determination of LAC in dosage forms; BBD-optimized with metoprolol succinate as internal standard; superior LOD (0.034 µg/mL); stability-indicating under five ICH stress conditions; biorelevant dissolution profiling.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148681436","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 Sustainable RP-HPLC Method for Tofacitinib Quantification in MCM-41 and MCM-48 Silica Nanoparticles and its In-vitro Application.","authors":"Vidhi S Pandya, Nidhi R Trivedi, Manish N Nandpal, Meghana N Patel, Bhupendra G Prajapati, Amit A Patel, Samir G Patel, Ravish J Patel","doi":"10.1093/jaoacint/qsag073","DOIUrl":"https://doi.org/10.1093/jaoacint/qsag073","url":null,"abstract":"<p><strong>Background: </strong>Tofacitinib is a Janus kinase inhibitor approved by the FDA, for the treatment of autoimmune disorders.</p><p><strong>Objective: </strong>The research aimed to develop, validate, and apply a simple, rugged, and environmentally sustainable RP-HPLC method for the quantitative estimation of Tofacitinib in in-house developed Mesoporous Silica Nanoparticles (MCM-41 and MCM-48), intended for formulation-related analytical applications, while systematically evaluating environmental and analytical sustainability.</p><p><strong>Method: </strong>The chromatographic separation was achieved on Inertsil® C18 column using an isocratic mobile Phase of Milli-Q water and Acetonitrile (65:35, v/v) at a Flow rate of 1.0 mL/min, with PDA detection at 287 nm and a total run time of 15 min. The validated approach was applied to formulation based analytical studies. Environmental and analytical sustainability was evaluated using the AGREE and the RGB-12 whiteness model.</p><p><strong>Results: </strong>The method exhibited excellent specificity without interference from formulation excipients and showed Linearity over 1-24 µg/mL (r² = 0.9987). High accuracy (98-102%), precision 0.06-1.31% RSD), and sensitivity (LOD - 0.28 µg/mL and LOQ - 0.848 µg/mL) in compliance with ICH guidelines, enabled reliable estimation of Tofacitinib. The method demonstrated good ruggedness (0.012-1.33% RSD), indicating reliability under small deliberate changes. High AGREE and RGB-12 whiteness (0.79 and 87.0) values confirmed the enhanced sustainability and practical feasibility.</p><p><strong>Conclusion: </strong>The developed RP-HPLC method integrates reliable analytical performance with green and white chemistry principles, rendering it suitable for routine quality control and formulation-oriented research involving mesoporous silica based drug delivery systems.</p><p><strong>Highlights: </strong>A novel sustainable RP-HPLC method was developed and validated for the analysis of TFC-loaded MCM-41 and MCM-48 MSNs. The method demonstrated excellent performance in accordance with ICH Q2 (R2) guidelines. It was successfully applied for drug content determination and in vitro diffusion studies. Sustainability assessment using AGREE and RGB-12 models confirmed favourable greenness and whiteness, with reduced analysis time and resource consumption compared to reported methods.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148681478","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":"Enzymatic Determination of L-Malic Acid in Selected Foods and Beverages: AOAC Official Method 2025.03 First Action.","authors":"Markus Lacorn, Thomas Hektor","doi":"10.1093/jaoacint/qsag069","DOIUrl":"https://doi.org/10.1093/jaoacint/qsag069","url":null,"abstract":"<p><strong>Background: </strong>L-malic acid is one of the most important acids present in fruits. Its determination is important in the manufacture of beer, fruit and vegetable products. In the wine industry, its level is monitored during malolactic fermentation. It is also added to a variety of products as food preservative and flavor enhancer.</p><p><strong>Objective: </strong>To validate the performance of the Enzytec™ Liquid L-Malic acid test kit for the determination of L-Malic Acid in foods and beverages such as fruit juice (concentrates and products), vegetable juice, wine, beer, sauces, and carbonated soft drinks.</p><p><strong>Methods: </strong>The kit contains two ready-to-use components only which makes handling easy and suitable for automation. L-malic acid is oxidized to oxaloacetate by L-malate dehydrogenase and NAD+. The NADH produced is equivalent to the amount of L-malate converted and is measured at 340 nm.</p><p><strong>Results: </strong>The Limit of Detection (LOD) was determined to be 8 mg/L for 100 µL test volume and the measurement range is 15 to 500 mg/L. Trueness was checked by analyzing a reference wine sample resulting in a recovery between 96 and 99%. Recovery was checked by spiking and resulted in mean values from 97 to 105% for red wine, beer, soft drink, carrot juice, apple juice, acerola juice concentrate, BBQ sauce, and quince jelly. Relative intermediate precision is between 1.5 and 3.6% for carrot juice, BBQ sauce, NIST SRM 3282, and a reference wine. D-tartaric acid and meso-tartaric acid interfere and cause a creep during the reaction. Sulfite interferes at concentrations higher than 0.025 g/L but can be masked by glyoxal. For automation, three applications with different test volumes were validated. Linearity is given from 3.5 to 2500 mg/L.</p><p><strong>Conclusions: </strong>The method was approved as AOAC Official Method of Analysis℠.</p><p><strong>Highlights: </strong>Real time and in-use stability are at least 24 months.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-07-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148611372","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":"Portable Near Infrared Spectroscopy Study for Turmeric Adulteration Detection.","authors":"Jiaxing Zeng, Zhengtao Wu, Erhao Zhang, Zhendong Liu, Tangwei Zhang, Liang Li","doi":"10.1093/jaoacint/qsag068","DOIUrl":"https://doi.org/10.1093/jaoacint/qsag068","url":null,"abstract":"<p><strong>Background: </strong>Turmeric powder is commonly adulterated with low-cost plant-based materials for economic gain; however, rapid on-site detection methods remain limited.</p><p><strong>Objective: </strong>This study is based on the development of a rapid, non-destructive method that uses portable near infrared spectroscopy, chemometrics, and deep learning, enabling the detection of corn flour adulteration in turmeric powder.</p><p><strong>Methods: </strong>A total of 330 adulterated samples (0-50% corn flour) were prepared, and corresponding NIR spectra were collected across the range of 900-1700 nm. A systematic comparison was carried out using eight pre-processing methods, three feature selection strategies (PCA, CARS, UVE), and multiple modeling algorithms. A dual-attention CNN-LSTM multi-task network was developed to simultaneously perform adulteration classification and content regression.</p><p><strong>Results: </strong>The optimization of the PLS model was performed through second derivative (D2) pre-processing and UVE feature selection (78.5% compression). The CNN-LSTM dual-attention model achieved a classification accuracy of 98.9% and a remarkable regression performance (R2 = 0.9927, RMSE = 1.3825, and RPD = 11.64), significantly outperforming traditional PLS models. Weight visualization revealed that the learned attention maps corresponded closely to the characteristic spectral features associated with the curcumin attenuation and starch enhancement.</p><p><strong>Conclusions: </strong>The integration of portable NIR spectroscopy with a multi-task deep learning model offers a robust, efficient, and accurate strategy for on-site rapid screening of turmeric adulteration under controlled experimental conditions.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-07-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148611357","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 novel Loop-mediated Isothermal Amplification Method for Screening Detection of Genetically Modified Cotton.","authors":"Mika Matsumoto, Mari Onishi, Yasutaka Minegishi, Reona Takabatake","doi":"10.1093/jaoacint/qsag066","DOIUrl":"https://doi.org/10.1093/jaoacint/qsag066","url":null,"abstract":"<p><strong>Background: </strong>Limited domestic cotton production in Japan has led to large amounts of cottonseed being imported for food and feed. Consequently, genetically modified (GM) cotton seeds have been introduced into the country, and a qualitative method is required for the detection of unauthorized GM cotton.</p><p><strong>Objective: </strong>The aim of this study is to develop a testing method that is simpler, more rapid, and more cost-effective than conventional polymerase chain reaction (PCR) technique.</p><p><strong>Methods: </strong>A novel method was developed for the screening detection of unauthorized GM cotton seeds using loop-mediated isothermal amplification (LAMP) to target the 35S promoter of the cauliflower mosaic virus (P35S), neomycin phosphotransferase Ⅱ (NPTII), and the endogenous cotton gene stearoyl acyl carrier protein desaturase (sad1).</p><p><strong>Results: </strong>The method limit of detection (LOD) was determined to be ≤ 0.1%, which is equivalent to the corresponding LOD achieved using the conventional PCR method. A simpler detection method based on single-stranded tag hybridization on a chromatography-printed-array strip system (denoted DNA chromatography) was also developed. This method allowed visual detection of the amplification of multiple DNA samples at the LOD level.</p><p><strong>Conclusions: </strong>Compared with the conventional PCR approach, the developed detection method is cost-effective, rapid, and simple.</p><p><strong>Highlights: </strong>The developed method facilitates the analysis of GM crops and will be expected to help prevent the unintended spread of GM crops into the environment.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-07-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148474984","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":"QuEChERS - UHPLC-ToF-MS Method for Regulated and Emerging Mycotoxins Including Ergot Alkaloids in Rice.","authors":"Ana R S Mateus, Filipa Carreiró, Sílvia C Barros, Carla Brites, Angelina Pena, Ana Sanches-Silva","doi":"10.1093/jaoacint/qsag063","DOIUrl":"https://doi.org/10.1093/jaoacint/qsag063","url":null,"abstract":"<p><strong>Background: </strong>Rice is susceptible to contamination by mycotoxins and ergot alkaloids, posing significant risks to food safety. Despite growing evidence of their co-occurrence, few methods allow simultaneous determination of regulated, emerging, and ergot alkaloids in rice.</p><p><strong>Objective: </strong>A screening method based on QuEChERS method coupled with UHPLC-ToF-MS was develop and validated for the simultaneous determination of 11 mycotoxins and 12 ergot alkaloids in rice.</p><p><strong>Methods: </strong>Chromatographic parameters, including column selection, gradient program, flow rate, and injection volume, were optimized to ensure adequate separation and sensitivity. Two extraction approaches, solid-liquid extraction (SLE) and QuEChERS, were systematically compared, and key parameters such as extraction solvent, extraction time, and salt composition were optimized to maximize recoveries across chemically diverse analytes. The validated method was applied to 41 commercially available rice samples from the Portuguese market.</p><p><strong>Results: </strong>The validated method showed recoveries between 71-119%, repeatability (RSDr ≤ 20%), inter-day precision (RSDR ≤ 25%), and limits of quantification compliant with EU performance criteria. Aflatoxin G2 and sterigmatocystin were the most frequently detected mycotoxins, with three samples exceeding the legal limit for total aflatoxins (4 µg/kg). Mycophenolic acid was also detected in two samples.</p><p><strong>Conclusion: </strong>The developed method demonstrated adequate sensitivity, selectivity, and precision for multi-mycotoxin surveillance, highlighting the relevance of monitoring emerging mycotoxins in rice.</p><p><strong>Highlights: </strong>QuEChERS combined with UHPLC-ToF-MS enables simultaneous screening of 23 analytes, including ergot alkaloids, regulated myxotoxins and emerging mycotoxins. The method was validated according to Regulation (EU) 2023/2782. Aflatoxin G2 and sterigmatocystin were detected in Portuguese market rice. Mycophenolic acid was detected as an emerging contaminant.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-07-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148474944","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 Novel Near-Infrared Fluorescent Probe for Quantifying Cysteine in Fruit and Vegetable Samples.","authors":"Jin Zhang, Yuyu Xu, Huang Xin, Hui Luo, Xiang Jiang","doi":"10.1093/jaoacint/qsag064","DOIUrl":"https://doi.org/10.1093/jaoacint/qsag064","url":null,"abstract":"<p><strong>Background: </strong>Cysteine (Cys) is an essential amino acid for the human body. It naturally exists in various foods and serves as a crucial additive in the food industry, so accurate quantification of Cys is vital for food. Several probes for detecting Cys have been developed. However, the majority of fluorescent probes exhibit limitations in food applications.</p><p><strong>Objective: </strong>This study aimed to develop a dual-channel near-infrared fluorescent probe (NC-NIR) for selective and sensitive quantification of Cys in various food samples.</p><p><strong>Methods: </strong>The detection performance of the NC-NIR probe was systematically evaluated, including its dual-channel response spectra, reaction mechanism, limit of detection (LOD), selectivity, response time, and feasibility for analyzing actual samples.</p><p><strong>Results: </strong>The probe (NC-NIR) exhibits high selectivity and low LOD = 34 nM) for the detection of Cys. The NC-NIR probe exhibits dual-channel fluorescence response toward Cys, exhibiting emission wavelengths at 550 nm and 825 nm. Furthermore, NC-NIR exhibits near-infrared characteristics that can overcome background fluorescence in food, and has been successful in detecting Cys content in apples, jujubes, broccoli, pears, onions, and milk slices.</p><p><strong>Conclusions: </strong>This dual‑channel NIR probe offers a promising near-infrared strategy for in-situ quantification of Cys in food samples.</p><p><strong>Highlights: </strong>A dual-channel, low background, high selectivity and low LOD probe for the detection of Cys in food samples.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148427742","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 the Multiplex PCR Assays for Detection of Salmonella spp. and Cronobacter sakazakii on Stainless Steel and Sealed Concrete Surfaces Compared with FDA-BAM Reference Methods.","authors":"Elba V Arias-Rios, Jinge Huang, James Jiang, Shawn Owens, Khristian Saclayan, Caleb Johnson, Fereidoun Forghani, Mansour Samadpour","doi":"10.1093/jaoacint/qsag062","DOIUrl":"https://doi.org/10.1093/jaoacint/qsag062","url":null,"abstract":"<p><strong>Background: </strong>Rapid laboratory detection methods need to be tested against reference methods to confirm their efficiency and suitability.</p><p><strong>Objective: </strong>In an unpaired study, the IEH Salmonella-Cronobacter spp. and Cronobacter sakazakii-Salmonella Multiplex PCR Assays' performance was compared with the FDA-BAM reference methods Chapter 5 for Salmonella and Chapter 29 for Cronobacter sakazakii detection on stainless-steel (SS) and sealed concrete (SC) surfaces.</p><p><strong>Methods: </strong>Seeking a shorter enrichment time for the candidate method, the Salmonella-Cronobacter broth enrichments for 18, 20, 22, and 24 h at 35 °C were analyzed with the IEH Multiplex PCR Assays. Two pathogen cocktails were prepared: one including S. Typhimurium ATCC 19585, S. Senftenberg 775W, and S. Enteritidis PT30, and a second one including C. sakazakii MEI 27583, C. sakazakii ATCC 29544, and C. sakazakii ATCC 29004. The Salmonella and C. sakazakii cocktails were independently inoculated onto separate SS and SC following the AOAC guidelines. Additionally, a competing microorganism was added at a concentration 10-100-times higher than that of the pathogens.</p><p><strong>Results: </strong>The candidate method yielded zero false negatives and zero false positives, with 100% sensitivity and 100% specificity for both SS and SC surfaces, regardless of the inoculation level (high, low, and uninoculated) and the enrichment time (i.e. 18, 20, 22, and 24 h for Salmonella, and 20, 22, and 24 h for C. sakazakii). The candidate method successfully detected both target microorganisms on both surface types with a minimum enrichment of 20 h. Statistical analysis using the probability of detection (POD) confirmed the equivalency between the candidate method and the reference methods at either inoculation level or enrichment time (P > 0.05).</p><p><strong>Conclusion: </strong>The IEH Salmonella-Cronobacter spp. and Cronobacter sakazakii-Salmonella Multiplex PCR Assays demonstrated performance comparable to the FDA-BAM reference methods for the detection of Salmonella and C. sakazakii on SS and SC, with a significantly shorter turnaround time.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148427738","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":"Study on the Impurity Profile and Its Correlation With the Production Process in the Estazolam API and Tablets.","authors":"Zhenjing Hu, Dandan Shen, Qun Wu, Ji Nie, Yuanqing Liu, Wenxing Mao, Lixin Hou, Jianhua Wang","doi":"10.1093/jaoacint/qsaf041","DOIUrl":"10.1093/jaoacint/qsaf041","url":null,"abstract":"<p><strong>Background: </strong>Estazolam is a benzodiazepine drug widely used in clinical practice. Currently, estazolam tablets on the Chinese market are generic drugs. To meet the requirements of national standards and uniformity, the impurity analysis methods were developed for active pharmaceutical ingredient (API) and tablets of estazolam.</p><p><strong>Objective: </strong>A high-performance liquid chromatography with ultraviolet detection (HPLC-UV) method was developed to achieve enhanced sensitivity and resolution for the quantitative analysis of related substances. This method was applied to determine impurity levels in generic estazolam tablets from 12 Chinese manufacturers and APIs from 4 manufacturers. The liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was used to determine the impurity profiles. The impurity content and impurity profiles were used as evaluation indicators to trace the correlation between the differences in impurity profiles and the production process.</p><p><strong>Methods: </strong>The content of both eight known and unknown impurities was quantitatively determined by the HPLC-UV method. A principal component external standard method with correction factor was used for calculation, and detailed methodological validation was performed according to ICH guidelines. The structures of impurities in Chinese marketed products and the innovator drugs were qualitatively identified by the LC-MS/MS method, and differences in impurity profiles were compared.</p><p><strong>Results: </strong>This study identified two USP-listed process impurities, two unknown process impurities, and one non-pharmacopeial degradation product. The unknown impurities were successfully separated and preliminarily characterized.</p><p><strong>Conclusions: </strong>Three API process impurities were key contributors to preparation impurity profile variations. Impurity levels showed close correlation with API synthesis routes and purification processes. A novel degradation product emerged during formulation, generated under light/heat stress, but minimally impacted tablet impurity variations.</p><p><strong>Highlights: </strong>The optimized HPLC method demonstrated enhanced sensitivity and separation efficiency. API manufacturers should prioritize purification process optimization for impurities exceeding 0.1% thresholds to ensure drug safety.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"468-478"},"PeriodicalIF":1.7,"publicationDate":"2026-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144035740","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":"The Prediction of Quality Markers of Notopterygium incisum Based on Mass Transfer Law and Network Pharmacology.","authors":"Meiju Guo, Shuo Li, Jiaxuan Luo, Wenxuan Bao, Qian Li","doi":"10.1093/jaoacint/qsag011","DOIUrl":"10.1093/jaoacint/qsag011","url":null,"abstract":"<p><strong>Background: </strong>To address medication safety concerns from depleted Notopterygium incisum Ting ex H. T. Chang (NI) resources and inconsistent quality, this study employed the quality markers (Q-Marker) concept of traditional Chinese medicine to screen potential Q-Markers via multistep compositional transfer analysis and network pharmacology.</p><p><strong>Objective: </strong>This study aimed to screen the Q-Markers of NI for treating cardiovascular diseases.</p><p><strong>Methods: </strong>An approach integrating mass transfer analysis, network pharmacology, and HPLC fingerprinting was employed. First, HPLC fingerprints of 13 batches of NI were established. A representative batch was selected to prepare fresh medicinal materials, processed decoction pieces, and standard decoctions. Additionally, blood-absorbed components were collected, and fingerprints for all sample types were established. The transfer rates of seven index components (chlorogenic acid, nodakenin, ferulic acid, psoralen, bergapten, phenethyl ferulate, and isoimperatorin) were determined via similarity evaluation and least-squares discriminant analysis. Network pharmacology and molecular docking were further used to analyze the associations between NI's bioactive components and therapeutic targets for cardiovascular diseases.</p><p><strong>Results: </strong>This study employed an integrated approach of HPLC fingerprinting, mass transfer analysis, network pharmacology, and molecular docking. After establishing HPLC fingerprints for 13 NI batches, a representative batch was processed from fresh herbs, decoction pieces, standard decoctions, and blood-absorbed components for analysis, after which a determination was made for the transfer rates of seven index components and their associations with cardiovascular disease targets.</p><p><strong>Conclusion: </strong>Chlorogenic acid, nodakenin, ferulic acid, phenethyl ferulate, and isoimperatorin are potential Q-Markers of NI for the treatment of cardiovascular diseases.</p><p><strong>Highlights: </strong>In this study, mass transfer analysis, network pharmacology, and HPLC fingerprinting were integrated, combined with orthogonal partial least-squares discriminant analysis (OPLS-DA) and molecular docking. Potential Q-Markers of NI for the treatment of cardiovascular diseases were identified.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"607-618"},"PeriodicalIF":1.7,"publicationDate":"2026-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146151544","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}