QuEChERS EMR-Liqid-超高效液相色谱-串联质谱法测定动物源食品中的安眠酮

Determination of methaqualone residues in animal-derived food by QuEChERS EMR-Liqid-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  QuEChERS EMR-Liqid技术  安眠酮  超高效液相色谱-串联质谱法  动物源食品

英文关键词:QuEChERS EMR-Liqid  methaqualone  ultra performance liquid chromatography-tandem mass spectrometry  animal-derived food

中文摘要:

      目的 建立QuEChERS EMR-Liqid-超高效液相色谱-串联质谱法测定动物源食品中的安眠酮残留的分析方法。方法 样品用1%甲酸乙腈提取, 经过QuEChERS EMR-Lipid萃取净化后, 采用在电喷雾正离子模式下以质谱多反应监测(multiple reaction monitoring, MRM)方式检测。结果 安眠酮在0.1~100 ng/mL浓度范围内线性良好, 相关系数为0.9997, 方法检出限0.03 μg/kg, 定量限为0.1 μg/kg, 在0.1、0.2和0.5 μg/kg 3个加标水平下的回收率为85.5%~98.6%, 相对标准偏差(relative standard deviations, RSDs)为2.07%~4.56%。 结论 该方法简便快捷、灵敏可靠, 适用于动物源食品中的安眠酮药物的快速检测。

英文摘要:

      Objective To establish a method for determination of methaqualone residues in animal-derived food by QuEChERS EMR-Liqid-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Samples were extracted with acetonitrile with 1% formic acid, then purified by QuEChERS EMR-Lipid extraction column. The UPLC-MS/MS (ESI+) with multiple reactions monitoring (MRM) was used for detection. Results Methaqualone had a good linear relationship in the range of 0.1-100 ng/mL, and the correlation coefficient was 0.9997. The limit of detection was 0.03 μg/kg, and the limit of quantization was 0.1 μg/kg. The recoveries were ranged from 85.5%-98.6% for methaqualone at 3 spiked levels of 0.1, 0.2 and 0.5 μg/kg. The relative standard deviations (RSDs) were from 2.07%-4.56%. Conclusion The method is easy, rapid, accurate and sensitive, which is suitable for detecting methaqualone in animal-derived food.