超高效液相色谱-串联质谱测定配合饲料中10种抗病毒类药物

Determination of 10 antiviral drugs in compound feed by ultra-high performance liquid chromatography tandem mass spectrometry

实验旨在建立超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测配合饲料中10种抗病毒类药物的分析方法。样品用1%甲酸水、乙腈溶液提取后,经PRIME HLB固相萃取柱净化,PC HILIC色谱柱分离,以10mmol/L乙酸铵(含0.2%甲酸)和乙腈为流动相进行洗脱,基质匹配标准工作曲线定量。结果显示:10种抗病毒类药物在浓度1.0~100 ng/mL内线性关系良好,50、100、500μg/kg 3水平的加标回收率为87.5%~106.3%,相对标准偏差1.2%~10.6%,本方法检出限为20μg/kg,定量限为50μg/kg。

A method for detecting 10 kinds of anti-viral drugs in compound feed was established by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The samples were extracted by 1% formic acid and acetonitrile solution and purified by PRIME HLB solid phase extraction column.The 10 kinds of anti-viral drugs were separated by PC HILIC column and gradiently eluted using acetonitrile and 10 mmol/L ammonium acetate solution(containing 0.2% formic acid).The quantitative analysis was conducted using the matrix matching external standard method.The results showed that the calibration curves were in good linear relationship in the range of 1.0 ~ 100 ng/mL.The recoveries of the 10 kinds of antiviral drugs at three spiked levels(50,100,500 μg/kg) were 87.5% ~ 106.3%,and the relative standard deviations were 1.2% ~ 10.6%.The detection limit was 20 μg/kg and the quantitative limit was 50 μg/kg.