{"title":"QuEChERS萃取- uplc -MS/MS同时测定海带和紫菜中氯霉素类药物含量的方法建立及验证","authors":"Kaili Gao , Kunming Zheng , Juan Yuan , Qian Huang , Ruiqi Liu , Jiamin Tian , Xiaoping Wu , Xingang Meng","doi":"10.1016/j.jchromb.2025.124632","DOIUrl":null,"url":null,"abstract":"<div><div>The analysis of the content of chloramphenicol (CAPs) in Laminaria japonica and <em>Porphyra yezoensis</em> samples is crucial for quality control of seaweed products. In this study, the analytical method using QuEChERS combined with Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry (UPLC-MS/MS) was established to separate and detect residues of chloramphenicol, thiamphenicol, and florfenicol in Laminaria japonica and <em>Porphyra yezoensis</em>. The extraction solvent used was acetonitrile, and a 1:1 mixture of graphitized carbon black (GCB) and C18 was employed as the purifying agent. Electrospray ionization (ESI) in negative ion mode with multiple reaction monitoring (MRM) was employed, coupled with the isotope internal standard quantification method. The results demonstrated good linearity within a range of 0.0005–0.050 μg/mL for chloramphenicol, thiamphenicol, and florfenicol with correlation coefficient (r) of 0.999. The method detection limit was 0.4 μg/kg, while the quantitation limit was 1.0 μg/kg. Furthermore, during validation experiments where concentrations ranging from 1.0 μg/kg to 10.0 μg/kg were added to samples, recovery rates for chloramphenicol ranged from 87.4 % to 103.4 %, with relative standard deviations (RSDs) between 2.1 % and 5 %. This developed method was applied to test twenty batches of samples in which one batch of Laminaria japonica was found to contain a chloramphenicol concentration of approximately 2.0 μg/kg. The developed method, which uses simple and cost-effective sample pretreatment techniques, is suitable for qualitative determination. It satisfies the experimental requirements in terms of accuracy and sensitivity when monitoring large quantities of marine algae products containing CAPs.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1260 ","pages":"Article 124632"},"PeriodicalIF":2.8000,"publicationDate":"2025-05-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Development and validation of a QuEChERS extraction-UPLC-MS/MS method for the simultaneous determination of chloramphenicol drugs in Laminaria japonica and Porphyra yezoensis\",\"authors\":\"Kaili Gao , Kunming Zheng , Juan Yuan , Qian Huang , Ruiqi Liu , Jiamin Tian , Xiaoping Wu , Xingang Meng\",\"doi\":\"10.1016/j.jchromb.2025.124632\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><div>The analysis of the content of chloramphenicol (CAPs) in Laminaria japonica and <em>Porphyra yezoensis</em> samples is crucial for quality control of seaweed products. In this study, the analytical method using QuEChERS combined with Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry (UPLC-MS/MS) was established to separate and detect residues of chloramphenicol, thiamphenicol, and florfenicol in Laminaria japonica and <em>Porphyra yezoensis</em>. The extraction solvent used was acetonitrile, and a 1:1 mixture of graphitized carbon black (GCB) and C18 was employed as the purifying agent. Electrospray ionization (ESI) in negative ion mode with multiple reaction monitoring (MRM) was employed, coupled with the isotope internal standard quantification method. The results demonstrated good linearity within a range of 0.0005–0.050 μg/mL for chloramphenicol, thiamphenicol, and florfenicol with correlation coefficient (r) of 0.999. The method detection limit was 0.4 μg/kg, while the quantitation limit was 1.0 μg/kg. Furthermore, during validation experiments where concentrations ranging from 1.0 μg/kg to 10.0 μg/kg were added to samples, recovery rates for chloramphenicol ranged from 87.4 % to 103.4 %, with relative standard deviations (RSDs) between 2.1 % and 5 %. This developed method was applied to test twenty batches of samples in which one batch of Laminaria japonica was found to contain a chloramphenicol concentration of approximately 2.0 μg/kg. The developed method, which uses simple and cost-effective sample pretreatment techniques, is suitable for qualitative determination. It satisfies the experimental requirements in terms of accuracy and sensitivity when monitoring large quantities of marine algae products containing CAPs.</div></div>\",\"PeriodicalId\":348,\"journal\":{\"name\":\"Journal of Chromatography B\",\"volume\":\"1260 \",\"pages\":\"Article 124632\"},\"PeriodicalIF\":2.8000,\"publicationDate\":\"2025-05-02\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of Chromatography B\",\"FirstCategoryId\":\"1\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S1570023225001862\",\"RegionNum\":3,\"RegionCategory\":\"医学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q2\",\"JCRName\":\"BIOCHEMICAL RESEARCH METHODS\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Chromatography B","FirstCategoryId":"1","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S1570023225001862","RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"BIOCHEMICAL RESEARCH METHODS","Score":null,"Total":0}
Development and validation of a QuEChERS extraction-UPLC-MS/MS method for the simultaneous determination of chloramphenicol drugs in Laminaria japonica and Porphyra yezoensis
The analysis of the content of chloramphenicol (CAPs) in Laminaria japonica and Porphyra yezoensis samples is crucial for quality control of seaweed products. In this study, the analytical method using QuEChERS combined with Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry (UPLC-MS/MS) was established to separate and detect residues of chloramphenicol, thiamphenicol, and florfenicol in Laminaria japonica and Porphyra yezoensis. The extraction solvent used was acetonitrile, and a 1:1 mixture of graphitized carbon black (GCB) and C18 was employed as the purifying agent. Electrospray ionization (ESI) in negative ion mode with multiple reaction monitoring (MRM) was employed, coupled with the isotope internal standard quantification method. The results demonstrated good linearity within a range of 0.0005–0.050 μg/mL for chloramphenicol, thiamphenicol, and florfenicol with correlation coefficient (r) of 0.999. The method detection limit was 0.4 μg/kg, while the quantitation limit was 1.0 μg/kg. Furthermore, during validation experiments where concentrations ranging from 1.0 μg/kg to 10.0 μg/kg were added to samples, recovery rates for chloramphenicol ranged from 87.4 % to 103.4 %, with relative standard deviations (RSDs) between 2.1 % and 5 %. This developed method was applied to test twenty batches of samples in which one batch of Laminaria japonica was found to contain a chloramphenicol concentration of approximately 2.0 μg/kg. The developed method, which uses simple and cost-effective sample pretreatment techniques, is suitable for qualitative determination. It satisfies the experimental requirements in terms of accuracy and sensitivity when monitoring large quantities of marine algae products containing CAPs.
期刊介绍:
The Journal of Chromatography B publishes papers on developments in separation science relevant to biology and biomedical research including both fundamental advances and applications. Analytical techniques which may be considered include the various facets of chromatography, electrophoresis and related methods, affinity and immunoaffinity-based methodologies, hyphenated and other multi-dimensional techniques, and microanalytical approaches. The journal also considers articles reporting developments in sample preparation, detection techniques including mass spectrometry, and data handling and analysis.
Developments related to preparative separations for the isolation and purification of components of biological systems may be published, including chromatographic and electrophoretic methods, affinity separations, field flow fractionation and other preparative approaches.
Applications to the analysis of biological systems and samples will be considered when the analytical science contains a significant element of novelty, e.g. a new approach to the separation of a compound, novel combination of analytical techniques, or significantly improved analytical performance.