高效液相色谱-串联质谱法测定水产品中大环内酯类兽药残留

Determination of Macrolide Antibiotics Residue in aquatic products by high performance liquid chromatography- electrospray ionization tandem mass spectrometry

关键词:  大环内酯、兽药残留、检测、高效液相色谱-串联质谱

Key words:  Macrolide  Veterinary medicine Residue  Detection  HPLC-MS/MS.

摘要:

本文建立了水产品中10种大环内酯类抗生素的高效液相色谱-电喷雾串联质谱检测方法。对比几种检测方法后，最终采用乙腈进行提取的方法。在5.0～200.0 μg/L 范围内，10种大环内酯类抗生素的线性相关系数均大于0.99。通过实际样品的添加回收试验，方法的定量下限(S/N=10)为1.0 μg/kg，检出限（S/N=3）为0.2 μg/kg，3个添加水平中，龙虾、鮰鱼的加标回收率分别为69.4%～115.3%和63.1%～100.9%，日内相对标准偏差（RSD）分别为0.73%～3.39%及0.8%～4.44%。结果表明，该法简单、灵敏、特异性强，适用于水产品中大环内酯类药物残留的分析确证。

Abstract:

Determination of 10 kinds of Macrolide durgs by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) in aquatic products has been studied in this research. Contrast several extraction methods，samples finally were extracted by acetonitrile. In the range of 5.0~200.0μg/L，the linear correlation coefficients for the determination for the above ten kinds of macrolide antibiotics were greater than 0.99. The detection quality (S/N=10) and the detection limit (S/N = 3) were 1.0 μg/kg and 0.2 μg/kg，respectively. Recoveries for the lobster，catfish of fish，honey and milk were 69.4% ~ 115.3%，63.1% to 100.9%，RSD in the day were 0.73% ~3.39% and 0.8%~ 4.44%. Results indicated that the established method is simple，sensitive，and specific for the determination of macrolide residues in aquatic products.