| 摘要: |
| 建立了一种测定鸡蛋及牛奶中四环素类药物残留 液相色谱-串联质谱的方法。样品经Mcllvaine-Na2EDTA缓冲液提取，经快速滤纸过滤，并经加脱脂棉的HLB固相萃取柱净化，洗脱液氮气吹至小于1 mL，加30%甲醇至1mL并混匀，液相色谱-串联质谱法检测，基质匹配标液外标法定量。结果表明，四环素类药物在5 μg/kg~100 μg/kg的浓度范围内呈现良好的线性关系。在鸡蛋及牛奶中四环素类药物的检测限均为2 μg/kg，定量限均为5 μg/kg。在LOQ~2MRL(多西环素为LOQ-10LOQ)添加浓度范围内，四环素类药物的回收率均在81.2~110.0%之间，批内批间变异系数均小于11.4%。该方法各项技术指标均能满足残留检测要求，且方法的重现性良好，满足国内外兽药残留检测的相关规定。 |
| 关键词: 鸡蛋 牛奶 四环素类 残留 液相色谱-串联质谱 |
| DOI： |
| 投稿时间：2021-11-08修订日期：2022-02-28 |
| 基金项目: |
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| Determination of tetracyclines residues in eggs and milk by liquid chromatography-mass spectrometry |
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| (Henan Institute of Veterinary Drug and Feed Control) |
| Abstract: |
| To establish a method for testing the tetracyclines residues in eggs and milk by liquid chromatography-tandem mass spectrometry. The samples were extracted with Mcllvaine-Na2EDTA buffer, filtered through fast filter paper, and purified by HLB solid phase extraction column with absorbent cotton. The eluent was blown with nitrogen to less than 1 mL, then added with 30% methanol solution to 1 mL and mixed, and tested by liquid chromatography-mass spectrometry, matrix matching solution external standard method for quantification. The results showed a good linear relationship between the range of 5 to 100 μg/kg concentrations. The detection limit and the limit of quantification of tetracyclines were 2 μg/kg, and 5 μg/kg, respectively both in eggs and in milk. The recoveries of tetracyclines were all between 81.2% and 110.0%, and the coefficients of variation within and between the batches were less than 11.4% when the concentraion was at the range of LOQ to 2MRL(doxycycline:LOQ to 10LOQ). The technical indicators of this method can meet the requirements of residue testing, and the method has good reproducibility, and meets the relevant regulations of home and abroad on testing residues of veterinary drugs. |
| Key words: egg milk tetracycline residues high performance liquid chromatographytandem mass spectrometry |
