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

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5.0～200.0μg/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1.0μg/kg,检出限(S/N=3)为0.2μg/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。

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

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 p,g/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.