同位素稀释法-超高效液相色谱-串联质谱法测定豆芽中6种喹诺酮类药物残留

Determination of 6 quinolones drug residues in bean sprouts by isotope internal standard- ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  豆芽  prime HLB固相萃取小柱  喹诺酮  超高效液相色谱-串联质谱/质谱法

英文关键词:bean sprouts  prime HLB solid phase extraction  quinolones  ultra performance liquid chromatography- tandem mass spectrometry

中文摘要:

      目的 建立通过式固相萃取(solid phase extraction, SPE)柱净化、氘代同位素内标、超高效液相色谱-串联质谱法同时测定豆芽中6种喹诺酮类药物残留的方法。方法 用0.1%甲酸-乙腈作为提取溶剂, 经通过式固相萃取柱净化提取液, 超高效液相色谱-串联质谱测定豆芽中6种喹诺酮药物残留。结果 6种喹诺酮在5.0~200 μg/L范围内线性关系良好, r2≥0.999; 方法检出限(S/N=3)为0.7 μg/kg, 定量限(S/N=10)为2.0 μg/kg; 加标水平为2.0~80 μg/kg时, 平均回收率在85.5%~119.4%, 相对标准偏差(relative standard deviation, RSD) (n=6)为0.13%~9.93%。结论 本方法前处理简单, 定量结果准确, 回收率高, 可以应用于大批次豆芽中喹诺酮药物残留的监测。

英文摘要:

      Objective To establish a method for simultaneous determination of 6 quinolones residues in bean sprouts by ultra performance liquid chromatography-tandem mass spectrometry with solid phase extraction column purification and deuterated isotope internal standard. Methods Using 0.1% formic acid-acetonitrile as extraction solvent, the extraction solution was purified by solid phase extraction column, and 6 quinolones residues in bean sprouts were determined by ultra performance liquid chromatography-tandem mass spectrometry. Results Six quinolones had good linear relationship in the range of 5.0?200 g/L, r2≥0.999. The detection limit (S/N=3) was 0.7 g/kg, and the quantitative limit (S/N=10) was 2.0 g/kg. When the standard addition level was 2.0?80 g/kg, the average recoveries were in the range of 85.5%?119.4% and relative standard deviation (RSD) (n=6) was in the range of 0.13%?9.93%. Conclusion This method is simple and accurate, which can be applied in daily rapid monitoring of 6 quinolones in bean sprouts.