高效液相色谱-串联质谱法测定水产品中喹乙醇残留量

Determination of olaquindox residue in aquatic products by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  喹乙醇  高效液相色谱-串联质谱法  外标法  罗非鱼  水产品

英文关键词:olaquindox  high performance liquid chromatography-tandem mass spectrometry  external standard method  tilapia  aquatic products

中文摘要:

      目的 建立高效液相色谱-串联质谱联用法测定水产品中喹乙醇残留量的方法。方法 以罗非鱼为实验样品, 样品经乙腈提取、正己烷脱脂, 以乙腈-0.5 mmol乙酸铵甲酸溶液(10:90, V:V)为流动相进行等度洗脱、色谱柱Poroshell 120 EC-C18(50 mm×2.1 mm, 2.7 μm)分离, 在多反应监测(multiple reaction monitoring, MRM)模式下进行三重四极杆质谱检测。结果 喹乙醇在0.02~0.4 mg/kg范围内线性关系良好, 检出限为0.4 μg/kg, 加标回收率(n=6)为93.8%~97.0%, 相对标准偏差为2.10%~8.02%。结论 该方法简单、快速、灵敏度高、准确可靠, 可用于批量水产品样品喹乙醇残留量的测定。

英文摘要:

      Objective To establish a method for the determination of olaquindox residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods Tilapia samples were extracted by acetonitrile, and purified by hexane. The obtained target compound were separated by high performance liquid chromatography using Poroshell 120 EC-C18 (50 mm×2.1 mm, 2.7 μm) column with isocratic elution of acetonitrile-0.5 mmol ammonium acetate formic acid solution (10:90, V:V), and were detected by HPLC-MS/MS with multiple reaction monitoring (MRM) mode. Results Olaquindox had good linearity in the range of 0.02-0.4 mg/L. The limit of detection was 0.4 mg/kg, and the standard recovery rates were 93.8%-97.0% (n=6), with the relative standard deviation of 2.10%-8.02%. Conclusion This method is simple, rapid, sensitive, accurate and reliable, which can be used for the determination of residual amount of olaquindox in batches of aquatic products.