牛肉粉中恩诺沙星和磺胺嘧啶高准确度分析方法研究与标准物质研制

Development of an Accurate Determination Method and Reference Material for Enrofloxacin and Sulfadiazine in Bovine Powder

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.