摘要
建立了基于液相色谱-同位素稀释质谱法(LC-IDMS)的牛肉粉中恩诺沙星和磺胺嘧啶残留测定的高准确度分析方法,采用同位素稀释单点校准定量,恩诺沙星和磺胺嘧啶的加标回收率分别为(99.0±0.8)%和(100.4±1.2)%,基质效应因子分别为0.9991和1.0119。采用添加法制备牛肉粉中恩诺沙星和磺胺嘧啶标准物质候选物,进行了标准物质均匀性检验、稳定性检验和定值,评定了不确定度。标准物质均匀性、稳定性良好,恩诺沙星特性量值为729 ng/g,扩展不确定度为42 ng/g(k=2),磺胺嘧啶特性量值为413 ng/g,扩展不确定度为31 ng/g(k=2)。该标准物质的研制能够应用于食品中恩诺沙星和磺胺嘧啶等相关兽药残留检测的质量控制、方法开发和验证等领域,进而保障相关检测结果的准确性、可比性。
A liquid chromatography-isotope dilution mass spectrometry(LC-IDMS)method was established for the precise determination of enrofloxacin and sulfadiazine in bovine powder.Isotope dilution single point calibration method was applied for quantification.The matrix spiked recoveries of enrofloxacin and sulfadiazine were found to be(99.1±0.8)%and(100.4±1.2)%,respectively,with corresponding matrix effect factors of 0.9991 and 1.0119.To prepare the reference material,enrofloxacin and sulfadiazine standard solution were spiked into bovine muscle samples.Subsequently,the developed LC-IDMS method was utilized in homogeneity testing,stability testing,and value assignment.With an evaluation of the uncertainty of the reference material.The results indicated remarkable homogeneity and stability of enrofloxacin and sulfadiazine in bovine powder,characterized by values of 729 ng/g with uncertainty of 42 ng/g(k=2),and 413 ng/g with uncertainty of 31 ng/g(k=2),respectively.This reference material can paly a pivotal role in quality control,method development,and validation of veterinary drug residue detection in food,thereby ensuring the accuracy and comparability in related detection outcomes.
作者
李瑶瑶
杨吉双
李秀琴
时玲
高燕
张庆合
LI Yao-yao;YANG Ji-shuang;LI Xiu-qin;SHI Ling;GAO Yan;ZHANG Qing-he(Division of Chemical Metrology and Analytical Science,National Institute of Metrology,Beijing 100029,China;College of Chemical Engineering and Environment,China University of Petroleum(Beijing),Beijing 102249,China;China Academy of Information and Communications Technology,Beijing 100191,China)
出处
《化学试剂》
CAS
2024年第5期93-99,共7页
Chemical Reagents
基金
国家市场监督管理总局科技计划资助项目(2021MK156)
中央级公益性科研院所基本科研业务费资助项目(AKYZZ2117)。
关键词
牛肉粉
恩诺沙星
磺胺嘧啶
同位素稀释质谱法
标准物质
bovine powder
enrofloxacin
sulfadiazine
isotope dilution mass spectrometry
reference material
