Linlin Wu, Meixu Chen, Xinyi Huo, Qilin Xu, Xianggang Yin, Xiao Han Zhao, Yifeng Zhou, Jun Huang
{"title":"基于设计质量原则开发和验证测定菊花中黄曲霉毒素的 DLLME-HPLC-FLD 方法","authors":"Linlin Wu, Meixu Chen, Xinyi Huo, Qilin Xu, Xianggang Yin, Xiao Han Zhao, Yifeng Zhou, Jun Huang","doi":"10.1002/pca.3445","DOIUrl":null,"url":null,"abstract":"IntroductionAflatoxins, potent carcinogens produced by Aspergillus species, present significant health risks and commonly contaminate herbal products such as <jats:styled-content style=\"fixed-case\"><jats:italic>Chrysanthemum morifolium</jats:italic></jats:styled-content>. Detecting these toxins in <jats:styled-content style=\"fixed-case\"><jats:italic>C. morifolium</jats:italic></jats:styled-content> proves challenging due to the complex nature of the herbal matrix and the fluctuating levels of toxins found in different samples.ObjectivesThis study aimed to develop and optimize a novel method for the detection of aflatoxins in <jats:styled-content style=\"fixed-case\"><jats:italic>C. morifolium</jats:italic></jats:styled-content> using dispersive liquid–liquid microextraction combined with high‐performance liquid chromatography‐fluorescence detection based on quality by design principles.MethodologyThe method involved determining critical method attributes and parameters through the Plackett–Burman design, followed by optimization using the Box–Behnken design. Monte Carlo simulation was employed to establish a design space, which was experimentally verified. Method validation was performed to confirm accuracy, precision, and stability.ResultsThe developed method exhibited excellent linearity (<jats:italic>R</jats:italic><jats:sup>2</jats:sup> > 0.9991) for aflatoxins B<jats:sub>1</jats:sub>, B<jats:sub>2</jats:sub>, G<jats:sub>1</jats:sub>, and G<jats:sub>2</jats:sub> across a range of concentrations, with recovery rates between 85.52% and 102.01%. The validated method effectively quantified aflatoxins in <jats:styled-content style=\"fixed-case\"><jats:italic>C. morifolium</jats:italic></jats:styled-content> under different storage conditions, highlighting the impact of temperature and storage time on aflatoxin production.ConclusionThis study successfully established a reliable and effective method for the detection of aflatoxins in <jats:styled-content style=\"fixed-case\"><jats:italic>C. morifolium</jats:italic></jats:styled-content>, highlighting the importance of strict storage conditions to reduce aflatoxin contamination. Using a quality by design framework, the method demonstrated robustness and high analytical performance, making it suitable for routine quality control of herbal products.","PeriodicalId":20095,"journal":{"name":"Phytochemical Analysis","volume":"113 1","pages":""},"PeriodicalIF":3.0000,"publicationDate":"2024-09-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Development and validation of a DLLME‐HPLC‐FLD method for determination of aflatoxins in Chrysanthemum morifolium based on quality by design principles\",\"authors\":\"Linlin Wu, Meixu Chen, Xinyi Huo, Qilin Xu, Xianggang Yin, Xiao Han Zhao, Yifeng Zhou, Jun Huang\",\"doi\":\"10.1002/pca.3445\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"IntroductionAflatoxins, potent carcinogens produced by Aspergillus species, present significant health risks and commonly contaminate herbal products such as <jats:styled-content style=\\\"fixed-case\\\"><jats:italic>Chrysanthemum morifolium</jats:italic></jats:styled-content>. Detecting these toxins in <jats:styled-content style=\\\"fixed-case\\\"><jats:italic>C. morifolium</jats:italic></jats:styled-content> proves challenging due to the complex nature of the herbal matrix and the fluctuating levels of toxins found in different samples.ObjectivesThis study aimed to develop and optimize a novel method for the detection of aflatoxins in <jats:styled-content style=\\\"fixed-case\\\"><jats:italic>C. morifolium</jats:italic></jats:styled-content> using dispersive liquid–liquid microextraction combined with high‐performance liquid chromatography‐fluorescence detection based on quality by design principles.MethodologyThe method involved determining critical method attributes and parameters through the Plackett–Burman design, followed by optimization using the Box–Behnken design. Monte Carlo simulation was employed to establish a design space, which was experimentally verified. Method validation was performed to confirm accuracy, precision, and stability.ResultsThe developed method exhibited excellent linearity (<jats:italic>R</jats:italic><jats:sup>2</jats:sup> > 0.9991) for aflatoxins B<jats:sub>1</jats:sub>, B<jats:sub>2</jats:sub>, G<jats:sub>1</jats:sub>, and G<jats:sub>2</jats:sub> across a range of concentrations, with recovery rates between 85.52% and 102.01%. The validated method effectively quantified aflatoxins in <jats:styled-content style=\\\"fixed-case\\\"><jats:italic>C. morifolium</jats:italic></jats:styled-content> under different storage conditions, highlighting the impact of temperature and storage time on aflatoxin production.ConclusionThis study successfully established a reliable and effective method for the detection of aflatoxins in <jats:styled-content style=\\\"fixed-case\\\"><jats:italic>C. morifolium</jats:italic></jats:styled-content>, highlighting the importance of strict storage conditions to reduce aflatoxin contamination. Using a quality by design framework, the method demonstrated robustness and high analytical performance, making it suitable for routine quality control of herbal products.\",\"PeriodicalId\":20095,\"journal\":{\"name\":\"Phytochemical Analysis\",\"volume\":\"113 1\",\"pages\":\"\"},\"PeriodicalIF\":3.0000,\"publicationDate\":\"2024-09-12\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Phytochemical Analysis\",\"FirstCategoryId\":\"99\",\"ListUrlMain\":\"https://doi.org/10.1002/pca.3445\",\"RegionNum\":3,\"RegionCategory\":\"生物学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q2\",\"JCRName\":\"BIOCHEMICAL RESEARCH METHODS\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Phytochemical Analysis","FirstCategoryId":"99","ListUrlMain":"https://doi.org/10.1002/pca.3445","RegionNum":3,"RegionCategory":"生物学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"BIOCHEMICAL RESEARCH METHODS","Score":null,"Total":0}
Development and validation of a DLLME‐HPLC‐FLD method for determination of aflatoxins in Chrysanthemum morifolium based on quality by design principles
IntroductionAflatoxins, potent carcinogens produced by Aspergillus species, present significant health risks and commonly contaminate herbal products such as Chrysanthemum morifolium. Detecting these toxins in C. morifolium proves challenging due to the complex nature of the herbal matrix and the fluctuating levels of toxins found in different samples.ObjectivesThis study aimed to develop and optimize a novel method for the detection of aflatoxins in C. morifolium using dispersive liquid–liquid microextraction combined with high‐performance liquid chromatography‐fluorescence detection based on quality by design principles.MethodologyThe method involved determining critical method attributes and parameters through the Plackett–Burman design, followed by optimization using the Box–Behnken design. Monte Carlo simulation was employed to establish a design space, which was experimentally verified. Method validation was performed to confirm accuracy, precision, and stability.ResultsThe developed method exhibited excellent linearity (R2 > 0.9991) for aflatoxins B1, B2, G1, and G2 across a range of concentrations, with recovery rates between 85.52% and 102.01%. The validated method effectively quantified aflatoxins in C. morifolium under different storage conditions, highlighting the impact of temperature and storage time on aflatoxin production.ConclusionThis study successfully established a reliable and effective method for the detection of aflatoxins in C. morifolium, highlighting the importance of strict storage conditions to reduce aflatoxin contamination. Using a quality by design framework, the method demonstrated robustness and high analytical performance, making it suitable for routine quality control of herbal products.
期刊介绍:
Phytochemical Analysis is devoted to the publication of original articles concerning the development, improvement, validation and/or extension of application of analytical methodology in the plant sciences. The spectrum of coverage is broad, encompassing methods and techniques relevant to the detection (including bio-screening), extraction, separation, purification, identification and quantification of compounds in plant biochemistry, plant cellular and molecular biology, plant biotechnology, the food sciences, agriculture and horticulture. The Journal publishes papers describing significant novelty in the analysis of whole plants (including algae), plant cells, tissues and organs, plant-derived extracts and plant products (including those which have been partially or completely refined for use in the food, agrochemical, pharmaceutical and related industries). All forms of physical, chemical, biochemical, spectroscopic, radiometric, electrometric, chromatographic, metabolomic and chemometric investigations of plant products (monomeric species as well as polymeric molecules such as nucleic acids, proteins, lipids and carbohydrates) are included within the remit of the Journal. Papers dealing with novel methods relating to areas such as data handling/ data mining in plant sciences will also be welcomed.