超高效液相色谱-四极杆-静电场轨道离子阱高分辨率质谱法快速筛查和确证动物源性食品中9种β-受体激动剂残留量

Rapid screening and confirming of 9 kinds of β-agonists in animal-derived food by ultra performance liquid chromatography-quadrupole-orbitraphigh resolution mass spectrometry

中文关键词:  超高效液相色谱-四极杆-静电场轨道阱高分辨质谱法  动物源性食品  β-受体激动剂类药物  残留量

英文关键词:ultra performance liquid chromatography-quadrupole-orbitrap high resolution mass spectrometry  animal-derived food  β-agonists  residues

中文摘要:

      目的 建立超高效液相色谱-四极杆-静电场轨道阱高分辨质谱法(ultra performance liquid chromatography-quadrupole-orbitraphigh resolution mass spectrometry, UPLC-Q-Orbitrap)筛查和确证动物源性食品中9种β-受体激动剂残留量的分析方法。方法 样品经乙腈提取, 150 mg PSA(乙二胺-N-丙基填料)粉末、50 mg C18粉末和500 mg无水硫酸镁进行净化, 正己烷去脂, 用Waters Acquity BEH C18 柱(2.1 mm×50 mm, 1.7 μm)分离, 以0.1%甲酸-乙睛(V/V)和0.1%甲酸-水(V/V)进行梯度洗脱, 在全扫描(Full MS)-数据依赖扫描(data dependent MS2)模式下进行检测。结果 9种β-受体激动剂残留量的精确质量相对偏差小于1.0×10?6, 在0.5~10 ng/mL范围内线性关系良好, 相关系数均大于0.997; 检出限范围为0.2~0.5 μg/kg; 加标水平为0.5~5 μg/kg时, 方法回收率在74.3%~110.8%范围内, 相对标准偏差低于12%。结论 该方法简便、快速、准确, 适用于动物源性食品中9种β-受体激动剂类药物的快速筛查和定量分析。

英文摘要:

      Objective To establish a method for screening and validation of 9 kinds of β-agonists residuesin animal-derived food by ultraperformance liquid chromatography-quadrupole-orbitrap high resolution mass spectrometry(UPLC-Q-Orbitrap). Methods The sample was extracted by acetonitrile, purified by 150 mg PSA, 50 mg C18, 500 mg MgSO4 and the fat in the sample was degreased with N-hexane. The extract was separated by Waters Acquity BEH C18 column(2.1 mm×50 mm, 1.7 μm) using agradient elution program of 0.1% formic acid-acetonitrile(V/V) and 0.1% formic acid-water(V/V)as mobile phases, and detected in full scan-data dependent scan mode. Results The results showed that 9 kinds of β-agonists residues had good linear relationships in the range of 0.5?10 ng/mL with correlation coefficients better than 0.997. The accurate mass relative deviation was less than 1.0×10?6, and the limit of determination(LOD) were 0.2?0.5 μg/kg. The recovery of the method ranged from 74.3% to 110.8% at spiked levels of 0.5?5 μg/kg, with the relative standard deviations were less than 12%. Conclusion This method is simple, rapid and accurate, which is suitable for the rapid screening and quantitative analysis of 9 kinds of β-agonist drugs in animal-derived food.