超高效液相色谱-串联质谱法测定猪肉中儿茶酚胺类的残留

Determination of the catecholamines residue in pork 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  猪肉  儿茶酚胺类  残留

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  pork  catecholamine  residues

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, UPLC-MS/MS)检测猪肉中肾上腺素、去甲肾上腺素、多巴胺等儿茶酚胺类药物残留量方法的检测方法。方法 样品经乙腈+水(95+5,V/V)提取, 经正己烷脱脂后, 过PBA固相萃取小柱纯化, 采用0.1%甲酸和乙腈作为流动相按比例进行梯度洗脱, 采用电喷雾正离子化质谱(positive electrospray mass spectrometry, ESI+)和多反应监测(multiple reaction monitoring,MRM)技术对肾上腺素、去甲肾上腺素、多巴胺进行定量和定性检测。结果 本方法在6 min内完成了3种目标化合物的分离分析。3种目标化合物在1~50 ng/mL线性范围内, r2均大于0.995。肾上腺素、去甲肾上腺素、多巴胺的检出限分别为0.2、0.4、0.3 μg/L, 定量限分别为为0.7、1.3、1.0 μg/L。在20、40和100 μg/kg 3个加标水平下, 平均回收率为78.2%～89.6%, 相对标准偏差为2.2%～4.9%(n=6)。 结论 该方法具有快速准确、灵敏度高等优点, 适用于猪肉中儿茶酚胺类残留量的测定。

英文摘要:

      Objective To establish a method for determination of the residue of catecholamines including epinephrine, norepinephrine and dopamineresidues in pork by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods After extracting the sample with a mixture of acetonitrile and water (95+5,V/V), samples were degreased by n-hexane and purified by PBA solid-phase extraction column. The gradient elution was carried out with 0.1% formic acid and acetonitrile as mobile phases in proportion. Positive electrospray mass spectrometry (ESI+) and multiple reaction monitoring (MRM) were used for quantitative and qualitative analysis for epinephrine, norepinephrine and dopamineresidues. Results The 3 target compounds were separated and analyzed within 6 min. In the linear range of 1-50 ng/mL, r2 of the three target compounds were all greater than 0.995. The detection limits of epinephrine, norepinephrine and dopamine were 0.2, 0.4 and 0.3 μg/L, respectively, and the limits of quantification were 0.7, 1.3 and 1.0 μg/L, respectively. The average recoveries were 78.2%–89.6% and the relative standard deviations were 2.2%–4.9% (n=6) at 3 spiked levels of 20, 40 and 100 μg/kg. Conclusion The method is rapid, accurate, sensitive and suitable for the determination of catecholamine residues in pork.