超高效液相-串联质谱法测定速冻调理肉制品中18种喹诺酮类药物残留量

Determination of the residues of 18 quinolones in quick-frozen prepared meat products by ultra-high performance liquid phase tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  喹诺酮类药物  速冻调理肉制品

英文关键词:ultra high performance liquid phase tandem mass spectrometry  quinolones  frozen meat products

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra high performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时检测速冻调理肉制品中18种喹诺酮类药物的含量。方法 速冻调理肉制样品用酸化乙腈溶液提取净化, 采用乙腈-甲酸水体系作为流动相进行梯度洗脱, 样品在电喷雾离子源正离子多反应监测模式下进行测定, 内标法定量。结果 18种喹诺酮类药物在2.5~20 μg/L浓度范围内线性关系良好, 相关系数均大于0.990。检出限和定量限分别为0.5、1.5 μg/kg, 在3个不同添加水平下的平均回收率为72.5%~110.7%, 相对标准偏差为1.5%~11.4%(n=6)。结论 该方法操作简单、快速, 灵敏度高, 能够适用于速冻调理肉制品等肉制品的测定。

英文摘要:

      Objective To establish a method for simultaneous determination of quinolones in frozen processed meat products by ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The quick-frozen conditioning meat sample was extracted and purified with acidified acetonitrile solution, and the gradient elution was carried out using acetonitrile-formic acid water system as mobile phase. It was measured in the electrospray ion source positive ion multiple reaction monitoring mode, and quantified by internal standard method. Results The 18 quinolones had a good linear relationship within the concentration range of 2.5? 20 μg/L, and the correlation coefficients were all greater than 0.990. The limit of detection and quantification were 0.5 and 1.5 μg/kg, respectively. The average recoveries at 3 different levels of addition were 72.5%?110.7%, and the relative standard deviations were 1.5%?11.4% (n=6). Conclusion The method is simple, rapid and sensitive, and can be applied to the determination of frozen meat products.