超高效液相色谱-串联质谱法同时测定禽产品和水产品中酰胺醇类药物残留

Simultaneous determination of amide alcohol drug residues in poultry and aquatic products by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  禽产品,水产品,国标优化,酰胺醇类

英文关键词:poultry product  aquatic product  ultra performance liquid chromatography-tandem mass spectrometry  amide alcohol drugs

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时检测禽产品与水产品中酰胺醇类药物的分析方法。方法 匀浆均匀的试样经3%氨化乙酸乙酯充分提取, 正己烷除脂, Waters Acquity UPLC BEH C18色谱柱分离, 以0.02%的氨水溶液和乙腈梯度洗脱, 使用UPLC-MS/MS, 在正负离子多反应监测(multiple reaction monitoring, MRM)模式下同时测定, 采用基质标准曲线及内标法进行定性和定量分析检测。结果 酰胺醇类药物在0.05~20.00 ng/mL质量浓度范围内均呈良好线性关系(r2≥0.997); 4种酰胺醇类药物的检出限和定量限均为0.05 μg/kg和0.15 μg/kg, 对阴性样品进行2倍定量限、5倍定量限和10倍定量限的添加回收, 回收率在85.3%~103.3%之间, 相对标准偏差为0.2%~4.2%。结论 优化后的方法操作简单、准确性高、回收率和重现性好, 能够适用于大批量样品中酰胺醇类药物的测定。

英文摘要:

      Objective To establish a method for the simultaneous detection of amide alcohol drugs in poultry and aquatic products by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The homogenized samples were fully extracted by 3% ammoniated ethyl acetate, delipidized by n-hexane, separated by Waters Acquity UPLC BEH C18 column, then eluted with 0.02% ammonia solution and acetonitrile gradient using UPLC-MS/MS. Positive and negative ion multiple reaction monitoring (MRM) mode was used for simultaneous determination, and matrix standard curve and internal standard method were used for qualitative and quantitative analysis. Results The amide alcohol drugs showed a good linear relationship (r2≥0.997) within the mass concentration range of 0.05–20.00 ng/mL; the limits of detection and limits of quantification of 4 kinds of amide alcohol drugs were 0.05 μg/kg and 0.15 μg/kg, respectively. Negative samples were added and recovered at 2 times, 5 times and 10 times the quantification limits, with recovery rates ranging from 85.3% to 103.3% and relative standard deviations of 0.2% to 4.2%. Conclusion The optimized method has the advantages of simple operation, high accuracy, good recovery and reproducibility, and can be used for the determination of amphenicols in large quantities of samples.