超高效液相色谱-串联质谱法测定动物源食品中克霉唑的残留量

Determination of clotrimazole residue in food of animal origin by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  克霉唑  液相色谱-串联质谱法  动物源食品  残留测定

英文关键词:clotrimazole  ultra performance liquid chromatography-tandem mass spectrometry  food of animal origin  residue determination

中文摘要:

      目的 建立QuEChERS提取和净化、超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定猪肉、牛肉、羊肉、鸡肉等畜禽肉和猪肝、猪肾、羊肝、鸡心等畜禽内脏中克霉唑残留的分析方法。方法 样品经正己烷饱和的乙腈提取, 提取液经乙腈饱和的正己烷液液分配除脂, 并经含PSA和C18粉末的净化管进一步净化。采用0.1%甲酸和乙腈作为流动相进行梯度洗脱, 多反应监测模式(multiple reaction monitoring, MRM)测定, 同位素内标法定量。结果 本方法在 7 min内完成分离分析, 方法在0.2~20.0 μg/L范围内线性关系良好, 相关系数r为0.9999。在0.2、2.0和20 μg/kg添加水平下的回收率为78.5%~111.9%, 相对标准偏差小于11.1%, 方法定量限为0.2 μg/kg。结论 该方法快速、准确、灵敏, 适合动物源食品中克霉唑残留量的测定。

英文摘要:

      Objective To establish a method for the determination of clotrimazole residues in pork, beef, mutton, chicken and other livestock and poultry meat and in pig liver, pig kidney, sheep liver, chicken heart and other livestock and poultry viscera by UPLC-MS/MS after QuEChERS extraction and purification. Methods The sample was extracted by n-hexane saturated acetonitrile, the extract was degreased by acetonitrile saturated n-hexane liquid-liquid distribution, and further purified by a purification tube containing PSA and C18 powder. Using 0.1% formic acid and acetonitrile as mobile phase for gradient elution, multi?reaction monitoring mode (MRM) determination and isotope internal standard method were carried out. Results The separation and analysis were completed within 7 min with a good linear relationship in the range of 0.2?20.0 μg/L, and the correlation coefficient r was 0.9999. The recoveries ranged from 78.5% to 111.9% at spiked levels 0.2, 2.0 and 20 μg/kg, the relative standard deviation was less than 11.1%, and the quantitative limit was 0.2 μg/kg. Conclusion The proposed method is fast, accurate and sensitive, which is suitable for detecting clotrimazole residue in animal muscles and viscera.