Journal of AOAC International最新文献

{"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":"Validation of Enzytec™ Liquid D-Lactic acid for Enzymatic Determination of D-Lactic acid in Selected Foods and Beverages: Official Method 2024.06 First Action.","authors":"Markus Lacorn, Thomas Hektor","doi":"10.1093/jaoacint/qsaf047","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf047","url":null,"abstract":"<p><strong>Background: </strong>D- and L-lactic acid are produced naturally by lactic acid bacteria and are found in fermented milk products, pickled vegetables, and cured meats. D-lactic acid is formed by some microorganisms only, e.g., Lactobacillus lactis, and Leuconostoc cremoris. D-Lactic acid is not formed or only in traces by \"higher organisms\", e.g., by animals. Therefore the presence of D-lactate may serve as an indicator for microbial contamination or spoilage, assuming that fermentation techniques have not been used.</p><p><strong>Objective: </strong>To validate the performance of the Enzytec™ Liquid D-Lactic acid for the determination of D-lactic acid in food and beverages such as milk and (fermented) milk products, fermented vegetable products, wines, beer, fruit and vegetable juices, egg and egg powder.</p><p><strong>Methods: </strong>The kit contains two ready-to-use components which makes handling easy and suitable for automation. D-lactic acids react in the presence of NAD and D-lactate dehydrogenase to pyruvate and NADH. The NADH formed is equivalent to the amount of D-lactic acid converted.</p><p><strong>Results: </strong>Ascorbic acid, 3-hydroxybutyric acid, and sulfite interfere at concentrations higher than 0.2, 0.2, and 0.05 g/L, respectively. Oxaloacetic acid, pyruvic acid and D-fructose do not interfere at or below concentrations of 0.2, 1, and 10 g/L, respectively. The calculated LOD when using a test volume of 100 µL is 5.4 mg/L and the LOQ is 15 mg/L. The practical upper measurement range is 600 mg/L. Relative intermediate precision was between 3.5 and 5.7% for pineapple juice, sauerkraut juice, wine and liquid egg. A reference material (wine) showed recoveries of 108%. For automation, three applications with different test volumes were validated. Linearity is given from 0.75 up to 3125 mg/L.</p><p><strong>Conclusions: </strong>The method is robust and accurate and was approved as AOAC Official Method of Analysis℠.</p><p><strong>Highlights: </strong>The ready-to-use components of the test kit have a shelf life of at least 24 months.</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":"144050628","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 Enzytec™ Liquid D-/L-Lactic Acid for Enzymatic Determination of D- and L-Lactic Acid in Selected Foods and Beverages: Official Method 2024.08 First Action.","authors":"Markus Lacorn, Thomas Hektor","doi":"10.1093/jaoacint/qsaf046","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf046","url":null,"abstract":"<p><strong>Background: </strong>Produced naturally by lactic acid bacteria, L-lactic acid is found in many fermented milk products such as yogurt, and also in pickled vegetables, cured meats and fish. It also serves as a quality parameter in wine, beer, whole egg, whole egg powder, and juices.</p><p><strong>Objective: </strong>To validate the performance of the Enzytec™ Liquid D-/L-Lactic acid for the determination of the sum of D- and L-lactic acid in food and beverages such as milk and (fermented) milk products, fermented vegetable products, wines, beer, fruit and vegetable juices, egg and egg powder.</p><p><strong>Methods: </strong>The kit contains two ready-to-use components which makes handling easy and suitable for automation. Both lactic acids react in the presence of NAD and D- or L-Lactate dehydrogenase to pyruvate and NADH. The NADH formed is equivalent to the amount of D-/L-lactic acid converted.</p><p><strong>Results: </strong>Ascorbic acid, 3-hydroxybutyric acid, and sulfite were found to have a low activity at concentrations higher than 0.5, 0.05, and 0.1 g/L, respectively. Oxaloacetic acid and D-fructose do not interfere at concentrations at or below 0.2 and 20 g/L, respectively. The calculated LOD when using a test solution volume of 100 µL is 3 mg/L and the LOQ is 10 mg/L. The practical upper measurement range is 600 mg/L. Relative intermediate precision was between 3.8 and 5.3% for pineapple juice, sauerkraut juice, wine and liquid egg. Cream cheese Certified Reference Materials showed a recovery between 98 and 103%. A reference wine was found with a recovery of 104%. For automation, three applications with different test solution volumes were validated. Linearity is given from 4 up to 3125 mg/L.</p><p><strong>Conclusions: </strong>The method is robust and accurate and was approved as AOAC Official Method of Analysis℠.</p><p><strong>Highlights: </strong>The ready-to-use components of the test kit have a shelf life of at least 24 months.</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":"144047399","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":"Evaluating the Lethal Dose (LD50) of Ivermectin for Common Carp: Insights from Oral Toxicity Study.","authors":"Haseena Shaik, Arun Sharma, Megha Kadam Badekar, Saurav Kumar, Arun Konduri, Manjunath Mathew, Chandru G, Ranjit Kumar Nadella, Rajisha Ravindran, Niladri Sekhar Chatterjee, Pani Prasad Kuricheti, Prasanna Kumar Patil","doi":"10.1093/jaoacint/qsaf048","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf048","url":null,"abstract":"<p><strong>Background: </strong>Ivermectin (IVM) is commonly used for the treatment of parasitic diseases in aquaculture and is administered either through oral or immersion methods, but it lacks regulatory approval.</p><p><strong>Objective: </strong>The aim of the present study was to determine the acute oral toxicity of Ivermectin by estimating the 96 h median lethal dose (LD50) using mortality as endpoint, for an economically important freshwater fish, Cyprinus carpio.</p><p><strong>Methods: </strong>Medicated feed was prepared by employing different doses of IVM top-dressed onto the commercial feed pellets. A single oral dose of IVM at different doses (mg/kg b.wt.) of 0 (control-T1), 1 (T2), 2.5 (T3), 5 (T4), 10 (T5), 12 (T6), 15 (T7), 18 (T8), 21 (T9), 25 (T10), and 50 (T11) was dissolved in Dimethyl sulfoxide (DMSO) and top-dressed using 0.5% W/V guar gum as a wet binder to the feed. The medicated feed was administered @ 3% b.wt. to all treatment groups and cumulative mortalities were recorded over a duration of 96 h.</p><p><strong>Results: </strong>The estimated LD50 of Ivermectin was found to be 8.91±3.46 mg/kg·b.wt. Furthermore, the treatment group (T2) was administered a single oral dose of 1 mg/kg b.wt., did not exhibit any noticeable behavioural changes compared to the control group. Similarly, LOAEL and NOEAL doses were found to be 2.5 mg/kg b.wt. and 1 mg/kg b.wt., respectively.</p><p><strong>Conclusion: </strong>This study provides valuable insights for further determining the safe dosage of IVM that can be used in aquaculture for the treatment of parasitic diseases.</p><p><strong>Highlight: </strong>The present study might be helpful for fixing the maximum residual limit (MRL) for IVM in the aquaculture sector and the data will be helpful for prescription of drug by regulatory authorities for treating parasitic diseases in fishes.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-04-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144047398","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}

{"title":"Characterization of Flavonoid Constituents in Four Yellow Camellia Leaves by UHPLC-MS/MS.","authors":"Shuyan Sun, Siyuan Ma, Liping Pang, Xiaofang Han, Tao Zhu, Wuzheng Li, Li Ge","doi":"10.1093/jaoacint/qsaf036","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf036","url":null,"abstract":"<p><strong>Background: </strong>Yellow camellias, recognized as health-promoting teas, are underexplored in terms of their flavonoid profiles. This study systematically investigates the flavonoid composition of four yellow camellia species: C. euphlebia, C. ptilosperma, C. nitidissima, and C. tunghinensis.</p><p><strong>Objective: </strong>The primary aim of this study was to systematically identify and quantify the flavonoid constituents in the leaves of four representative yellow camellia species (C. euphlebia, C. ptilosperma, C. nitidissima, and C. tunghinensis) using UHPLC-based mass spectrometry techniques.</p><p><strong>Methods: </strong>Flavonoid constituents were identified using UHPLC-Q-Exactive-MS. Quantitative analysis of 13 major flavonoids was conducted with a validated UHPLC-QqQ-MS/MS method.</p><p><strong>Results: </strong>A total of 189 flavonoid compounds were identified across all species. Quantitative analysis revealed significant interspecies variation in flavonoid content. C. nitidissima exhibited the highest flavonoid content (145.73 mg/g), followed by C. euphlebia (105.19 mg/g), C. ptilosperma (54.51 mg/g), and C. tunghinensis (51.68 mg/g).</p><p><strong>Conclusion: </strong>This study establishes comprehensive flavonoid profiles for four yellow camellia species, highlighting the species-specific differences in flavonoid levels and emphasizing their rich and diverse phytochemical compositions.</p><p><strong>Highlights: </strong>This study systematically investigates the flavonoid composition of four yellow camellia species: C. euphlebia, C. ptilosperma, C. nitidissima, and C. tunghinensis.</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":"144052480","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":"Effects of Different Cooking Methods on Cd Content and Health Risk Assessment of Cabbage Under Cd Stress.","authors":"Nannan Jing, Ke Liu, Li Long, Lili Zhang","doi":"10.1093/jaoacint/qsaf035","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf035","url":null,"abstract":"<p><strong>Background: </strong>Different cooking and processing methods to some extent influence the content of food elements. Karst plateau mountainous region has a significant geochemical high background of Cd.</p><p><strong>Objective: </strong>The study aims to explore the differences in health risks associated with different cooking methods for cabbage and provide a theoretical basis for safe production of cabbage in karst area and the reduction of consumption-related risks.</p><p><strong>Methods: </strong>Select three varieties of cabbage [Chi bai er hao (CB), Chun xin huo guo wang (CX), Qing cui chi bai cai (QC)] and use three different cooking methods to cook cabbage according to the cooking habits of local residents (raw, boiled, and fried) on the Cd content of cabbage were studied. The cabbages were grown in soil dosed with known amounts of Cd.</p><p><strong>Results: </strong>Cd content in cabbage significantly increased (P < 0.05) with the increase of exogenous Cd levels. The Cd content of cooked cabbage was significantly lower than that of raw cabbage (P < 0.05). The general rule was raw > stir-fried > boiled. The target hazard quotient (THQ) of cabbage consumption by local residents was found to be QC > CX > CB, and the THQ of different cooking methods was raw > stir-fried > boiled.</p><p><strong>Conclusion: </strong>Residents of the Karst region should choose vegetables that have Cd content below the limit standard and adopt reasonable cooking methods to reduce health risks. Compared to raw, the cooking method of boiling is the most effective, followed by stir-fried.</p><p><strong>Highlights: </strong>Commonly planted cabbage varieties in karst area; effects of different cooking methods on cadmium content in cabbage; health risk assessment of cabbage cooking methods on different consumer groups.</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":"144035602","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":"Evaluation of Modified QuEChERS Using Small-Scale SPE for the Analysis of Organophosphorus Pesticides in Spinach.","authors":"Takamitsu Otake, Kaori Machida, Keisuke Nakamura","doi":"10.1093/jaoacint/qsaf033","DOIUrl":"https://doi.org/10.1093/jaoacint/qsaf033","url":null,"abstract":"<p><strong>Background: </strong>The Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method has been widely applied to various compounds and matrices. However, the clean-up process of QuEChERS with dispersive solid-phase extraction (d-SPE) is considered to be not always sufficient. Therefore, a modified QuEChERS using small-scale SPE (abbreviated as \"modified QuEChERS\") for the clean-up process has seen an increasing number of users in Japan; it is therefore necessary to evaluate its performance.</p><p><strong>Objective: </strong>To evaluate the performance of modified QuEChERS for the analysis of nine organophosphorus pesticides (OPPs) in spinach, and to compare the various parameters among modified QuEChERS, QuEChERS, and the Japanese official multiresidue method (JOMM).</p><p><strong>Methods: </strong>The modified QuEChERS was evaluated by a recovery test using blank spinach samples and quantification using a pesticides-containing quality control spinach sample. A matrix effect was also evaluated for gas chromatography with mass spectrometry (GC/MS) with the stomach-shaped spiral large volume injection (LVI). Various parameters including accuracy, time, cost, and clean-up effect were compared among modified QuEChERS, QuEChERS, and JOMM.</p><p><strong>Results: </strong>The mean recoveries, the intra-day repeatability, and the inter-day reproducibility for modified QuEChERS were acceptable according to the validation guideline. The concentration of fenitrothion in the pesticides-containing quality control spinach sample obtained by modified QuEChERS was comparable that obtained by QuEChERS and JOMM. It was found that the clean-up of the blank spinach sample by modified QuEChERS using small-scale SPE can be more effective than that by QuEChERS using d-SPE. A matrix effect was newly evaluated in our analysis by GC/MS with the stomach-shaped spiral LVI.</p><p><strong>Conclusion: </strong>The modified QuEChERS is an accurate and simple method of analyzing OPPs in spinach.</p><p><strong>Highlight: </strong>The modified QuEChERS is not only accurate but also a fast, cost-effective, and environment-friendly method for analyzing OPPs in spinach.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-04-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144061120","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}