{"title":"Determination of nitrofuran metabolites in sausage casings and crawfish using LC-Q-Orbitrap HRMS: Method development and validation","authors":"Omar Khaled , Lamia Ryad , Nermine Gad , Fawzy Eissa","doi":"10.1016/j.toxrep.2025.102076","DOIUrl":null,"url":null,"abstract":"<div><div>This study developed and validated an analytical method for determining four nitrofuran (NF) metabolites in sausage casings and crawfish matrices. The method utilizes liquid chromatography coupled with quadrupole-Orbitrap high-resolution mass spectrometry (LC-Q-Orbitrap HRMS) to analyze these metabolites. The validation of the developed method was carried out in accordance with the Commission Implementing Regulation (CIR) EU 2021/808, using three concentration levels ranging from 0.25 to 0.75 μg/kg. The recoveries ranged from 77 % to 109 %, while both repeatability and reproducibility remained consistently below 15 %. The calibration curves exhibited good linearity, with correlation coefficients (R) exceeding 0.9978. The limits of detection (LOD) ranged from 0.0218 to 0.0596 μg/kg, while the limits of quantification (LOQ) ranged from 0.0719 to 0.1966 μg/kg. The decision limit (CCα) and detection capability (CCβ) values ranged from 0.30 to 0.39 μg/kg and 0.29–0.35 μg/kg, respectively. Out of 30 crawfish samples collected from local markets in Egypt, 16.66 % contained NF metabolites residues, whereas sausage casings showed no NF metabolite residues. The reliability of the method was further demonstrated through successful participation in two proficiency testing (PT) rounds.</div></div>","PeriodicalId":23129,"journal":{"name":"Toxicology Reports","volume":"15 ","pages":"Article 102076"},"PeriodicalIF":0.0000,"publicationDate":"2025-06-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Toxicology Reports","FirstCategoryId":"1085","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S2214750025001945","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"Environmental Science","Score":null,"Total":0}
引用次数: 0
Abstract
This study developed and validated an analytical method for determining four nitrofuran (NF) metabolites in sausage casings and crawfish matrices. The method utilizes liquid chromatography coupled with quadrupole-Orbitrap high-resolution mass spectrometry (LC-Q-Orbitrap HRMS) to analyze these metabolites. The validation of the developed method was carried out in accordance with the Commission Implementing Regulation (CIR) EU 2021/808, using three concentration levels ranging from 0.25 to 0.75 μg/kg. The recoveries ranged from 77 % to 109 %, while both repeatability and reproducibility remained consistently below 15 %. The calibration curves exhibited good linearity, with correlation coefficients (R) exceeding 0.9978. The limits of detection (LOD) ranged from 0.0218 to 0.0596 μg/kg, while the limits of quantification (LOQ) ranged from 0.0719 to 0.1966 μg/kg. The decision limit (CCα) and detection capability (CCβ) values ranged from 0.30 to 0.39 μg/kg and 0.29–0.35 μg/kg, respectively. Out of 30 crawfish samples collected from local markets in Egypt, 16.66 % contained NF metabolites residues, whereas sausage casings showed no NF metabolite residues. The reliability of the method was further demonstrated through successful participation in two proficiency testing (PT) rounds.