超高效液相色谱-串联质谱法测定动物源食品中肾上腺素和去甲肾上腺素的残留

Determination of epinephrine and norepinephrine residues in animal derived food by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  动物源食品  肾上腺素  去甲基肾上腺素

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  animal derived food  epinephrine  norepinephrine

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)测定动物源食品中肾上腺素和去甲肾上腺素残留的方法。方法 样品经乙腈-1%三氯乙酸溶液提取, 用Bond Elut PBA固相萃取柱净化后, 以0.1%甲酸溶液与乙腈作为流动相, 经金刚烷基柱Capcellpak ADME色谱柱(150 mm×4.6 mm, 5 μm)分离, 采用多反应监测模式, 以13C2,15N-肾上腺素和去甲肾上腺素-D6为内标进行定量测定。结果 肾上腺素和去甲肾上腺素在0~200.0 ng/mL范围内线性关系良好(r>0.998), 定量限为10 μg/kg。当肾上腺素和去甲肾上腺素添加水平为10、20和100 μg/kg时, 平均回收率为96.0%~109.5%, 相对标准偏差在1.23%~5.71%之间。结论 该方法前处理提取率高、重复性好, 适用于动物源性食品中肾上腺素和去甲肾上腺素的检测, 可为动物源性食品中非法添加的检测提供技术支持。

英文摘要:

      Objective To establish a method for the determination of epinephrine and norepinephrine residues in animal derived food by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The sample were extracted with acetonitrile-1% trichloroacetic acid solution, purified by Bond Elut PBA solid phase extraction column, and separated on a Capcell Pak ADME chromatographic column (150 mm×4.6 mm, 5 μm) with 0.1% formic acid solution and acetonitrile as mobile phases, the multiple reaction monitoring mode was adopted for the quantitative determination with 13C2,15N-epinephrine and norepinephrine-D6 as internal standards. Results The epinephrine and norepinephrine had good linear relationships in range of 0?200.0 ng/mL (r>0.998), the limit of quantification was 10 μg/kg. When the addition levels were 10.0, 20.0, and 100.0 μg/kg, the average recoveries were 96.0%?109.5%, and the relative standard deviations were 1.23%?5.71%. Conclusion This method has high extraction efficiency and good repeatability, and is suitable for the detection of epinephrine and norepinephrine residues in foodstuffs of animal origin, which can provide an technical sports for determination of illegal additives.