QuEChERS-UPLC-MS/MS测定鱼肉中3种抗病毒药物残留

Determination of Three Kinds of Antiviral Drugs Residue in Fish by UPLC–MS/MS after QuEChERS Preparation

关键词:  QuEChERS  超高效液相色谱串联三重四极杆质谱法  鱼肉  抗病毒药物  残留

Key words:  QuEChERS  ultra-high liquid chromatography tandem mass spectrometry(UPLC-MS/MS)  fish  antiviral drug  residue

摘要:

建立一种超高效液相色谱-串联质谱(UPLC-MS/MS)快速同时测定鱼肉中3种抗病毒药物（金刚乙胺、奥司他韦和帕拉米韦）残留的方法。以鱼肉作为样品，经甲醇直接提取，提取上清液经100 mg C18粉末净化；采用Brownlee SPP C18柱分离，电喷雾电离，正离子多反应监测模式检测，以含2 mmol/L乙酸铵和0.1%甲酸的水溶液与含0.1%甲酸的乙腈溶液为流动性，梯度洗脱，空白基质匹配系列浓度的标准品溶液，外标法定量。结果表明， 3种抗病毒药物在0 ~ 30 ng/mL范围内线性关系良好(R2 ＞0.99)，3种抗病毒药物的检出限（LOD）和定量限（LOQ）分别为0.18～0.48 μg/kg和0.64～1.5 μg/kg；三个梯度水平加样回收率和RSD分别在66.1%～119.4%和1.9%～4.9%之间。提示该方法操作简便、灵敏度高，适用于鱼肉中抗病毒药物的检测。

Abstract:

A fast method for determination of three kinds of antiviral drugs residue in fish by ultra high liquid chromatography-tandem mass spectrometry was developed. The analytes included peramivir, rimantadine and oseltamivir. The analytes were extracted from fish using methanol, the supernatant was removed by the power of 100 mg C18. The Brownlee SPP C18 column was used to separate the analytes under a gradient elution program, with aqueous solution of 2 mmol/L ammonium acetate and 0.1% formic acid, and acetonitrile containing 0.1% formic acid. The analytes were detected by the positive electrospray ionization modes of mass spectrometry under multiple reaction monitoring mode (MRM). Blank matrix matching standard solution was quantified by external standard method. Good linearities (R2＞0.99) were obtained in the range of 0 – 30 ng/mL, the LOD and LOQ of all analytes were in the ranges of 0.18 – 0.48 and 0.64 – 1.5 μg/kg, respectively. The recoveries of spiked levels were in the range of 66.1 % – 119.4%, and the ralative standard deviation were in the range of 1.9% – 4.9%. This method is simple, sensitive, and can be applied to the detection of antiviral drugs in fish.