QuEChERS-超高效液相色谱-大气压化学电离-串联质谱法测定多种动物源性食品中的地塞米松残留

Determination of dexamethasone residues in various animal derived foods by QuEChERS-ultra performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry

中文关键词:  QuEChERS  超高效液相色谱-串联质谱法  动物源性食品  地塞米松  大气压化学电离源  正负离子同扫  基质效应

英文关键词:QuEChERS  ultra performance liquid chromatography tandem mass spectrometry  animal derived food  dexamethasone  atmospheric pressure chemical ionization source  simultaneous scanning of positive and negative ions  matrix effect

中文摘要:

      目的 建立QuEChERS-超高效液相色谱-串联质谱法测定多种动物源性食品中地塞米松残留量的分析方法。方法 样品经含1%甲酸的乙腈提取, QuEChERS方法净化后, 以乙腈-0.1%甲酸水溶液为流动相, 经Phenomenex Kinetex F5色谱柱(100 mm×3.0 mm, 2.6 μm)分离, 采用大气压化学电离源(atmospheric pressure chemical ionization, APCI), 正、负模式同时扫描的离子化模式, 多反应监测(MRM)模式采集, 外标法定量。 结果 地塞米松在0.5~100 ng/mL浓度范围内线性良好, 相关系数(r)为0.99946, 检出限为0.10 μg/kg; 在3个加标水平下, 平均回收率为73.2%~95.9%, 精密度(n=6)为4.1%~10.7%。结论 该方法简单、快速、稳定性高、重现性好, 可满足多种动物源性食品中地塞米松残留量的检测。

英文摘要:

      Objective To establish a method for the determination of dexamethasone residues in various animal-derived foods by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with acetonitrile containing 1% formic acid, purified by QuEChERS method, and separated by Phenomenex Kinetex F5 column (100 mm×3.0 mm, 2.6 μm) with acetonitrile-0.1% formic acid aqueous solution as mobile phase. Using atmospheric pressure chemical ionization, the positive and negative modes were simultaneously scanned by ionization mode and multiple reaction monitoring (MRM) mode. The samples were collected and quantified by external standard method. Results The linearity of dexamethasone was good in the range of 0.5–100 ng/mL, the correlation coefficient (r) was 0.99946, and the detection limit was 0.10 g/kg. Under the 3 standard addition levels, the average recovery rate was 73.2%–95.9%, and the precision (n=6) was 4.1%–10.7%. Conclusion This method is simple, rapid, stable and reproducible, and can meet the requirements for the detection of dexamethasone residues in various animal-derived foods.