多壁碳纳米管QuEChERS结合超高效液相色谱-串联质谱法测定鸡蛋中兽药多残留残留

Determination of veterinary drug residues in eggs by multiwalled carbon nanotube QuEChERS combined with ultra-high performance liquid chromatography-tandem mass spectrometry

中文关键词:  多壁碳纳米管  QuEChERS  超高效液相色谱-串联质谱法  兽药残留  鸡蛋

英文关键词:multiwalled carbon nanotube  QuEChERS  high performance liquid chromatography-tandem mass spectrometry  veterinary drugs residues  eggs

中文摘要:

      目的 基于改良的多壁碳纳米管QuEChERS方法, 建立超高效液相色谱-串联质谱法快速筛查和测定鸡蛋中38种兽药残留量。方法 样品以70%乙腈提取, 结合多壁碳纳米管、十八烷基键合硅胶、乙二胺-N-丙基硅烷混合吸附剂净化提取液, 以1%甲酸水和1%甲酸甲醇为流动相, 经CAPCELL PAK C18 MGⅢ (2.0 mm×100 mm, 1.1 μm)分离, 采用电喷雾正负离子多反应监测模式检测, 基质匹配外标法进行定量。结果 38种化合物在0.1~100.0 μg/L范围内线性关系良好(r＞0.99); 在3个添加水平下, 平均回收率为80.1%~113.8%, 相对标准偏差为1.1%~9.8%, 定量限为0.014~1.100 μg/kg。结论 该方法简便, 基质干扰小, 可用于鸡蛋中磺胺类、氯霉素类、氟虫腈类以及硝基咪唑类药物快速筛查和定量分析。

英文摘要:

      Objective To establish a method for rapidly screening and determination of 38 veterinary drugs residues in eggs by ultra performance liquid chromatography-tandem mass spectrometry, based on the modified multi-walled carbon nanotubes QuEChERS method. Methods The sample was extracted with 70% acetonitrile and the extract was purified by multi-walled carbon nanotubes, octadecyl bonded silica gel, ethylenediamine-N-propylsilane mixed adsorbent. The samples were separated by CAPCELL PAK C18 MGIII (2.0 mm×100 mm, 1.1 μm) using 1% formic acid water and 1% formic acid methanol as mobile phase, then detected by electrospray positive and negative ion multiple reaction monitoring mode, and quantified by matrix-matched external standard method. Results The 38 compounds had good linear relationships in the range of 0.1?100.0 μg/L (r＞0.99). The average recoveries of 3 different spiked levels were 80.1%?113.8%, with the relative standard deviations of 1.1%?9.8%. The limits of quantitation were 0.014?1.100 μg/kg. Conclusion This method is simple and has low matrix interference, which can be used for rapid screening and quantitative analysis of sulfonamides, chloramphenicol, fluorozoanitrile and nitroimidazoles in eggs.