超高效液相色谱-串联质谱法检测羊肉中20种大环内酯类和林可胺类药物残留

Determination of 20 kinds of macrolides and lincomasides residues in mutton by ultra performance liquid chromatography-tandem mass spectrometry method

中文关键词:  大环内酯类  林可胺类  超高效液相色谱-串联质谱法  复定溶液  HLB

英文关键词:macrolides  lincomasides  ultra performance liquid chromatography-tandem mass spectrometry  solutions for reconstitution  HLB solid-phase extraction

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)检测羊肉样品中20种大环内酯类和林可胺类兽药残留的方法。方法 试验先用乙腈提取, 上清液浓缩至近干后, 样品再用50%甲醇水溶液提取, 合并两次的提取液, 用pH为8.0的弱碱性缓冲溶液稀释后经HLB固相萃取柱浓缩净化, 甲醇/5 mmol/L乙酸铵溶液(1:1, V:V)定容, 采用正离子多反应监测模式检测, 基质液配制标准曲线。方法对20种化合物的色谱质谱参数进行了优化, 比较了不同流动相和定容液的分离效果, 同时考察了提取溶剂、净化方式对目标化合物的提取效率和净化效果的影响。结果 20种大环内酯类化合物和林可胺类化合物在各自的线性范围内, 线性关系良好, 相关系数(r2)均大于0.999, 回收率为64.7%~94.2%, 相对标准偏差在3.8%~11.0%之间。结论 该方法具有准确、灵敏、高效等特点, 可用于羊肉中20种大环内酯类和林可胺类化合物的同时检测。

英文摘要:

      Objective To develop a method for analysis of 20 kinds of macrolides and lincomasides in mutton by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Samples were initially extracted with acetonitrile, and the supernatant was concentrated to near dryness. The residues were further extracted with 50% methanol, and the 2 extracts were combined and diluted with a weak alkaline buffer solution (pH 8.0). The mixture was then concentrated and purified using an HLB solid-phase extraction cartridge. A methanol/5 mmol/L ammonium acetate solution (1:1, V:V) was used for final dilution. Detection was performed in positive ion multiple reaction monitoring mode. A matrix-matched standard curve was prepared for quantification. Chromatographic and mass spectrometry parameters were optimized for the 20 kinds of target compounds, while the effects of different mobile phases, extraction solvents, and purification methods on extraction efficiency and purification quality were thoroughly investigated. Results The 20 kinds of macrolides and lincomasides demonstrated excellent linearity within their respective ranges, with correlation coefficients (r2) exceeding 0.999. Recoveries ranged from 64.7% to 94.2%, the relative standard deviation was between 3.8% and 11.0%. Conclusion The developed method is sensitive, accurate, and suitable for the simultaneous detection of 20 kinds of macrolides and lincomasides in mutton.