Journal of AOAC International最新文献

{"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}

{"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}

{"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}

{"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}

{"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}

{"title":"Rapid Screening of Multiple Pesticide Residues in Lycii Fructus and Raw Juice Samples Using an Automated Sample Cleanup Platform Combined with GC-Q-TOF/MS.","authors":"Ting Chen, Renyuan Zhu, Wen Zhang, Yanli Xu, Xingzhi Wang","doi":"10.1093/jaoacint/qsaf008","DOIUrl":"10.1093/jaoacint/qsaf008","url":null,"abstract":"<p><strong>Background: </strong>Lycii Fructus and its raw juice are widely consumed but may be contaminated with pesticide residues, posing health risks. Traditional methods for pesticide residue detection are often labor-intensive and time-consuming.</p><p><strong>Objective: </strong>This study aims to develop a rapid, automated method for screening pesticide residues in Lycii Fructus and its raw juice using a combination of micro solid-phase extraction (μ-SPE) and gas chromatography-quadrupole-time-of-flight mass spectrometry (GC-Q-TOF/MS).</p><p><strong>Methods: </strong>An automated sample cleanup platform (PAL-RTC, Precision Automated Liquid Handler-Robotic Tool Change) was integrated with μ-SPE technology for sample preparation. Matrix-matched external standards were used for quantification, and method validation was conducted to compare μ-SPE with dispersive solid-phase extraction (d-SPE). Performance parameters including linearity, LOQ, recovery rates, and RSDs were evaluated.</p><p><strong>Results: </strong>In total, 84.5% of the pesticides showed strong linearity (R2 > 0.99) over the concentration range 2-1000 μg/L. The LOQ for 91.4% of pesticides was below 20 μg/kg, with recovery rates between 70 and 120% and RSD ≤20%. Screening detection limits (SDLs) were between 1 and 20 μg/kg, with 96.8% of pesticides having an SDL below 5 μg/kg. The μ-SPE method demonstrated superior reproducibility at the low spiking level (10 μg/kg), detecting 415 pesticides, compared to 369 for d-SPE. Analysis of 100 Lycii Fructus and 50 raw juice samples revealed the presence of 24 pesticides, including 3 restricted types.</p><p><strong>Conclusions: </strong>The μ-SPE method, integrated with PAL-RTC and GC-Q-TOF/MS, offers a more efficient and accurate approach for detecting pesticide residues in Lycii Fructus and its raw juice compared to traditional methods, reducing labor and improving reproducibility.</p><p><strong>Highlights: </strong>Compared to the d-SPE method, the μ-SPE method integrated with PAL-RTC demonstrated better reproducibility and stability at low spiking levels, significantly enhancing the efficiency of sample cleanup.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"357-366"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143442806","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 Optimization of Extraction Methodologies for the Determination of Antibiotics in Honey by UHPLC-ToF-MS.","authors":"Helena Rodrigues, Marta Leite, Beatriz Oliveira, Andreia Freitas","doi":"10.1093/jaoacint/qsaf043","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf043","url":null,"abstract":"<p><strong>Background: </strong>The administration of antibiotics to food-producing animals, including bees, is a common practice employed to prevent or treat bacterial diseases. Such practices may result in the presence of veterinary residues in honey, potentially compromising the safety and health of consumers. In the European Union, maximum residue limits (MRLs) have not been established for pharmacological substances in honey. In this context, the development of accurate and robust analytical methodologies is of paramount importance for the appropriate risk assessment.</p><p><strong>Objective: </strong>This study aimed to develop and optimize a multi-class method for the determination of veterinary drug residues from seven classes (β-lactams, lincosamides, macrolides, quinolones, sulfonamides, tetracyclines and diaminopyrimidines) using ultra-high performance liquid chromatography coupled to time-of-flight mass spectrometry (UHPLC-ToF-MS).</p><p><strong>Methods: </strong>A preliminary assessment was conducted to evaluate the feasibility of solid-liquid extraction, given the complex matrix of compounds present in honey, by analysing different solvent solutions in acetonitrile, methanol, water, and/or McIlvaine buffer. The subsequent phase of the study involved the optimisation of a purification/clean-up method. This was achieved by comparing the efficacy of several solid-phase extraction (SPE) and QuEChERS protocols.</p><p><strong>Results: </strong>The results indicated that the most efficacious extraction were acetonitrile-based solutions, specifically acetic acid 1% and formic acid 0.1% in ACN-H2O (80:20, v/v). Finally, the method with the most optimal analytical performance in terms of recovery and matrix effect entailed an initial extraction step with formic acid 0.1% in ACN-H2O (80:20, v/v), followed by a modified QuEChERS protocol.</p><p><strong>Conclusion: </strong>Acidified organic solvents in combination with QuEChERS method revealed to be the most effective for the determination of antibiotics in honey, ensuring optimum extraction with minimum matrix interference.</p><p><strong>Highlights: </strong>The developed analytical protocol with further detection by high resolution mass spectrometry will be important to assess health risks and to add value to the consumption of honey and honey-based products.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-04-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144059092","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":"https://doi.org/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 8 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":""},"PeriodicalIF":0.0,"publicationDate":"2025-04-21","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":"A New UHPLC-UV-MS Method for Detection and Identification of Bioactive Compounds.","authors":"Adam T Zarth, Ana M Magallanes López","doi":"10.1093/jaoacint/qsaf039","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf039","url":null,"abstract":"<p><strong>Background: </strong>The development of analytical methods in food science has grown parallel with consumers' concern about food composition. There is desire to better understand the phytochemicals present in foods and feeds. Comprehensive screening of nutrients and bioactive compounds can be challenging due to the vast differences in molecular properties of the compounds.</p><p><strong>Objective: </strong>To develop a sensitive liquid chromatography-mass spectrometry (LC-MS) analytical method to detect, identify, and quantify hundreds of compounds from a broad range of molecular categories in a single method, from hydrophilic (e.g., organic acids) to hydrophobic (e.g., sterols) nutrients.</p><p><strong>Method: </strong>The chromatographic separation was tailored for a balanced detection of hydrophilic and hydrophobic compounds, with attention towards the separation of isomeric polyphenols. The chromatographic separation was performed in 45 min on a C18-PFP stationary phase, which provided enhanced resolution of isomers. The method employs two columns in series to improve the resolution, which requires ultra-high-pressure instrumentation (1,000 bar). The addition of an in-line ultraviolet (UV) diode-array detector allowed for spectral profile confirmation of the identities of many targeted and unknown compounds.</p><p><strong>Results: </strong>The developed method was applied in this work to measure different types of bioactives recognized to have health benefits: flavonoids, phenolic acids, vitamins, tocochromanols, phytosterols, sugars, organic acids, lipids, amines, nucleic acids, and many other small molecules. Four chocolate products were analyzed as a demonstration of the range of the method.</p><p><strong>Conclusions: </strong>This method has enabled discoveries of new commercial value in the food processing industry by capturing information on a wider range of analytes than previous individual methods, and this data can be leveraged to promote the health and well-being of consumers.</p><p><strong>Highlights: </strong>This new LC-UV-MS methodology provides a more comprehensive analysis of a broad range of molecularly diverse bioactive constituents in raw materials and finished products in the food and feed industry.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-04-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144032709","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":"Liquid- and Gas Chromatography with Tandem Mass Spectrometric Technique to Optimize and Validate the Analysis of Pesticides in Honey: a Large Scope, Multi-Class, Multi-Residue Method.","authors":"Partha P Choudhury, Sachin C Ekatpure, Abhishek Mandal, Veena Rao Udupi, Kusuma D Krishnamurthy, Nethravati Bheemiah, Seema Shenvi, Kaushik Banerjee","doi":"10.1093/jaoacint/qsaf040","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf040","url":null,"abstract":"<p><strong>Background: </strong>Honey is a nutrient-rich food item with a complex matrix due to its diverse nutritional components. This complexity poses challenges in the analysis of pesticide residues, affecting accuracy and precision of results. A comprehensive and reliable method is required for the detection and quantification of these contaminants.</p><p><strong>Objective: </strong>To develop and validate a method for simultaneous analysis of pesticide residues in various honey types using liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS).</p><p><strong>Methods: </strong>Honey samples (5 g) were extracted using acetonitrile (10 mL) and water (10 mL) for LC-MS/MS analysis, while ethyl acetate (10 mL) was used for GC-MS/MS analysis. The extract was cleaned using primary secondary amine (PSA) before pesticide residue quantification by LC-MS/MS and GC-MS/MS. The method performance was evaluated based on recoveries (70-120%) and repeatability (RSD <20%) at a limit of quantification of 0.01 mg/kg, in accordance with SANTE/11312/2021 guidelines.</p><p><strong>Results: </strong>The developed method demonstrated compliance with regulatory requirements, ensuring reliable determination of pesticide residues in honey samples. A study on matrix variability from 14 different honey samples revealed that each honey type exhibited a unique matrix effect for the targeted pesticides. To minimize this effect, the use of honey type-specific matrix-matched standards is recommended.</p><p><strong>Conclusion: </strong>The study successfully developed a simple, robust, and high-throughput analytical method for the quantitative determination of pesticide residues in honey. Given its high selectivity, sensitivity, and rugged performance, the method can be implemented in regulatory testing for the analysis of targeted compounds across a wide range of honey matrices.</p><p><strong>Highlights: </strong>A method for pesticide residue analysis in honey was developed using LC-MS/MS and GC-MS/MS. The method showed acceptable recoveries (within 70-120%) and repeatability (RSD <20%) at an LOQ of 0.01 mg/kg. Each honey type exhibited a unique matrix effect, emphasizing the need for matrix-matched standards for residue quantifications. The method demonstrated high throughput, selectivity, and sensitivity, making it suitable for regulatory testing.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-04-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144055855","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}