液相色谱-质谱联用测定鸡蛋中4-乙酰氨基苯甲酸的残留

Residual determination of p-acetylamino-benzoic acid in eggs by liquid chromatography-mass spectrometry

中文关键词:  异丙肌苷  4-乙酰氨基苯甲酸  鸡蛋  残留  液相色谱-质谱法

英文关键词:inosiplex  p-acetylamino-benzoic acid  egg  residue  liquid chromatography-mass spectrometry

中文摘要:

      目的 建立液相色谱-质谱法检测鸡蛋中4-乙酰氨基苯甲酸残留的方法。方法 样品经乙腈提取, 通过式吸附净化和阴离子交换固相萃取净化, 液相色谱分离, 四极杆-静电场轨道阱质谱定性定量测定, 平行反应监测模式检测, 外标法定量。结果 4-乙酰氨基苯甲酸保留时间为5.6 min, 在2.5~50 μg/kg范围内呈现良好的线性关系, 日内、日间精密度均小于15%, 回收率为70%~80%, 定量限为2.5 μg/kg。结论 此方法快速、准确且灵敏度高, 为监测异丙肌苷的非法使用及鸡蛋中的残留监控提供了快速准确的技术手段。

英文摘要:

      Objective To establish a method for the determination of p-acetaminobenzoic acid residues in eggs by liquid chromatography-mass spectrometry. Methods The samples were extracted by acetonitrile, purified by pass-through cleanup and solid phase extraction with anion exchange, separated by liquid chromatography, qualitatively and quantitatively determined by quadrupole- orbitrap mass spectrometry, detected by parallel reaction monitoring mode, and quantified by external standard method. Results The retention time of p-acetylamino-benzoic acid was 5.6 min, and showed a good linear relationship in the range of 2.5?50 μg/kg. The precisions of intra-day and inter-day were less than 15%. The recoveries were 70%?80% and the limit of quantitation was 2.5 μg/kg. Conclusion This method is fast, accurate and highly sensitive, which provides a fast and accurate technical means for monitoring the illegal use of isopropyl inosine and monitoring the residues in eggs.