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研究采用高效液相色谱-电喷雾串联质谱法建立了鸡蛋中金刚烷胺、金刚乙胺、利巴韦林和吗啉胍4种抗病毒药物多残留的检测方法。样品经过-26℃低温反复冻融清除蛋白质后,在水饱和的正己烷处理条件下,采用超声法去除脂肪,并通过Cleanert PCX阳离子交换固相萃取柱净化,使用Eclipse Plus C18反相色谱柱(2.1 mm×50 mm,1.8μm)进行分离,以5 mmol/L乙酸铵和乙腈水溶液作为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式电离,多反应监测模式进行定性定量测定。结果表明:金刚烷胺、金刚乙胺、利巴韦林、吗啉胍4种待测物在0.01~200.0 ng/m L浓度范围内均呈良好的线性关系,相关系数均大于0.999,该方法测定鸡蛋中金刚烷胺、金刚乙胺、利巴韦林、吗啉胍的最低检出限(S/N=3)为1.0μg/kg,定量限(S/N=10)为2.0μg/kg,平均回收率多集中于80%~100%,批内和批间变异系数均≤12%。该方法的建立对于监控鸡蛋等动物源性食品中的兽药残留具有积极作用。
A high performance liquid chromatography-electrospray ionization tandem mass spectrometry (ESI-MS / MS / MS) method was established for the detection of four residues of antiviral drugs such as amantadine, rimantadine, ribavirin and moroxydine in eggs. After the sample was repeatedly frozen and thawed at -26 ° C, the protein was removed by sonication under water-saturated n-hexane to remove fat and purified by a Cleanert PCX cation exchange SPE cartridge using Eclipse Plus C18 reversed-phase column 2.1 mm × 50 mm, 1.8 μm). The gradient elution was carried out with 5 mmol / L ammonium acetate and acetonitrile in water as mobile phase, and ionization and electrospray ionization (ESI +) mode. The results showed that the four analytes of amantadine, rimantadine, ribavirin and morpholine guanidine showed a good linearity in the concentration range of 0.01 ~ 200.0 ng / mL with the correlation coefficients greater than 0.999. The detection limit (S / N = 3) of amantadine, rimantadine, ribavirin and moroxydine in eggs was 1.0μg / kg and the limit of quantification (S / N = 10) was 2.0μg / kg, and the average recovery was mostly in the range of 80% -100%. The coefficient of variation (CV) within and between batches was ≤12%. The establishment of this method has a positive effect on the monitoring of veterinary drug residues in animal-derived foods such as eggs.