超高效液相色谱–串联质谱法测定动物源性食品中氯霉素类药物与氯丙嗪残留量

Determination of chloramphenicols and chlorpromazine residues in animal derived foods by ultra performance liquid chromatography tandem mass spectrometry

中文关键词:  动物源性食品  氯霉素类药物  氯丙嗪  固相萃取  超高效液相色谱–串联质谱法

英文关键词:animal derived food  chloramphenicol  chlorpromazine  solid phase extraction  ultra performance liquid chromatography tandem mass spectrometry

中文摘要:

      目的 建立超高效液相色谱–串联质谱法测定动物源性食品中氯霉素类药物与氯丙嗪残留量的分析方法。方法 样品经酸性乙腈溶液提取, 多孔聚苯乙烯/二乙烯基苯(polar enhanced polymer, PEP)固相萃取柱净化, 采用ACE Ultra Core Super C18色谱柱(2.1 mm×100 mm, 2.5 μm)分离, 以10 mmol/L甲酸铵(含0.1%甲酸)/乙腈作为流动相进行梯度洗脱, 电喷雾正、负(electron spray ionization, ESI+、ESI–)多反应监测, 外标法进行定量分析。结果 3种氯霉素类药物与氯丙嗪在1~100 ng/mL浓度范围内, 呈良好线性关系, r均大于0.992。样品在添加浓度分别为0.2、2、20 μg/kg时, 平均回收率为80.3%~94.7%, 相对标准偏差(relative standard deviation, RSD)为0.7%~2.2% (n=6)。方法的检出限为0.03~0.1 μg/kg, 定量限为0.1~0.3 μg/kg。结论 该方法具有简便、环保、准确、灵敏的特点, 适用于动物源性食品中氯霉素类药物与氯丙嗪残留量的分析检测, 可用于大批量快速筛查工作, 有效提高工作效率。

英文摘要:

      Objective To establish a method for the determination of chloramphenicol and chlorpromazine residues in animal derived food by ultra performance liquid chromatography tandem mass spectrometry. Methods The samples were extracted by acid acetonitrile solution and purified by polar enhanced polymer (PEP) solid phase extraction cartridge. And then the samples were separated by ACE Ultra Core Super C18 column (2.1 mm×100 mm, 2.5 μm), 10 mmol/L ammonium formate (including 0.1% formic acid)/acetonitrile was used as the mobile phase for gradient elution, using electrospray positive and negative multi-reaction monitoring. Quantitative analysis was carried out by external standard method. Results Chloramphenicol and chlorpromazine had good linear relationships in the concentration range of 1–100 ng/mL (r>0.992). When the concentration of the sample was 0.2, 2 and 20 μg/kg, the average recovery was 80.3%–94.7%, and the relative standard deviation (relative standard deviation, RSD) was 0.7%–2.2%. The detection limit of the method was 0.03–0.1 μg/kg, and the quantitative limit is 0.1–0.3 μg/kg. Conclusion This method is simple, environmentally friendly, accurate and sensitive, and is suitable for the analysis and determination of chloramphenicol and chlorpromazine residues in animal-derived foods, which can be used for mass and rapid screening and effectively improves the work efficiency.