通过式净化-液相色谱-串联质谱快速筛查水产品中15类107种兽药多残留的方法研究

Simultaneous determination of 15 categories and 107 kinds of veterinary drugs in aquatic products by pass-through purification and liquid chromatography-tandem mass spectrometry

中文关键词:  水产品  兽药  多残留  快速筛查  液相色谱-串联质谱法

英文关键词:aquatic products  veterinary drugs  multi-residue  rapid screening  liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立水产品基质中15类包含107种药物多残留的快速筛查方法。方法 通过多溶剂分步提取-通过式净化, 结合液相色谱-串联质谱仪, 在MRM模式下正、负离子同时扫描监测水产品, 实现水产品中15类107种药物多残留的快速筛查, 并用于实际水产样品中药物残留含量的测定。结果 所有药物在35 min内分离良好, 方法线性范围为0.1~200 ng/mL, 相关系数均大于0.995; 检出限为0.1~5.0 μg/kg (S/N>3), 定量限为0.3~10 μg/kg (S/N>10); 回收率为40.0%~120%, 相对标准偏差均小于15%。结论 方法的准确性和灵敏度较高, 重现性好, 适合水产基质中药物多残留的高通量、快速筛查, 能够满足国家限量法规的要求。

英文摘要:

      Objective To establish a rapid screening method for 15 categories containing 107 drug residues in aquatic product substrates. Methods The aquatic products were extracted by multi-solvent step and pass-through -purified, combined with liquid chromatography-tandem mass spectrometer, and the positive and negative ions were scanned and monitored simultaneously in MRM mode. The rapid screening of 15 categories and 107 kinds of drug residues in aquatic products were realized and applied to the determination of drug residues in actual aquatic samples. Results All the drugs were well separated within 35 mins. The linear ranges of the method were 0.1-200 ng/mL, and the correlation coefficients were greater than 0.995. The limits of detection were 0.1-5.0 μg/kg (S/N>3), and the limits of quantitation were 0.3-10 μg/kg (S/N>10). The recoveries were 40.0%-120%, and the relative standard deviations were less than 15%. Conclusion The method has high accuracy, sensitivity and good reproducibility, which is suitable for high throughput and rapid screening of drug residues in aquatic substrate, and can meet the requirements of national limit regulations.