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

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-C_(18)(50mm×2.1mm, 2.7μm)分离,在多反应监测(multiple reactionmonitoring, 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范围内线性兲系良好,检出限为0.4μg/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。

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-Cl8 （50 mm×2.1 mm, 2.7μm） 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.