QuEChERS净化结合超高效液相色谱-串联质谱法测定豆芽中57种抗生素残留量

Determination of 57 kinds of antibiotic residues in bean sprouts by QuEChERS purification combined with ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  豆芽  抗生素  残留

英文关键词:UPLC-MS/MS  bean sprouts  antibiotic  residue

中文摘要:

      目的 建立QuEChERS净化结合超高效液相色谱-串联质谱法（ultra performance liquid chromatography-tandem mass spectrometry， UPLC-MS/MS）同时测定豆芽中57种抗生素残留的方法。方法 样品经过甲酸乙腈提取，氯化钠分层，上清液经N-丙基乙二胺、C18吸附剂净化，UPLC-MS/MS测定，基质曲线外标法定量。结果 57种抗生素在1～150 μg/L范围内线性关系良好，相关系数在0.9963～0.9999之间, 定量限为0.03～2.78 μg/kg, 平均回收率为70.3%～111.9%，相对标准偏差为1.5%～7.9%。采用该方法筛查60批豆芽，发现一批检出恩诺沙星，另一批检出环丙沙星；本方法实测值与标准方法实测值｜Z｜＜2在可接受范围内。结论 该方法操作简单、高效，灵敏度高，准确性好，适用于豆芽中硝基咪唑类、磺胺类及喹诺酮类等多种类抗生素残留批量筛查检测。

英文摘要:

      ABSTRACT: Objective To establish a QuEChERS purification with ultra performance liquid chromatography-tandem mass spectrometry method for the simultaneous determination of 57 kinds of antibiotic residues in bean sprouts. Methods The samples were extracted with acetonitrile-formic acid, layered with sodium chloride, the supernatant was purified with N-propylethylenediamine and C18 adsorbent purification, UPLC-MS/MS determination, and quantified by the matrix curve external standard method. Results The linear relationships of 57 kinds of antibiotics were good within the range of 1~150 μg/L. The correlation coefficients between 0.9963-0.9999. The limit of quantitation was 0.03~2.78 μg/kg. The average recoveries of 70.3%~111.9%, and the relative standard deviations were 1.5%~7.9%. This method was then used to screening 60 batches of bean sprouts, it was found that enrofloxacin was detected in one batch and ciprofloxacin was detected in another batch; the measured value of this method and the measured value of the standard method | Z | < 2 are within the acceptable range.?Conclusion This method is simple to operate, efficient, has high sensitivity and good accuracy, it is suitable for batch screening and detection of various antibiotic residues such as nitroimidazole, sulfonamides and quinolones in bean sprouts.