全自动固相萃取-超高效液相色谱-串联质谱法测定鸡肉中的金刚烷胺和利巴韦林

Determination of amantadine and ribavirin in chicken by automatic solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱串联质谱  金刚烷胺  利巴韦林  鸡肉

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  amantadine  ribavirin  chicken

中文摘要:

      目的 建立全自动固相萃取-超高效液相色谱-串联质谱法(ultra performance liquid chromatography- tandem mass spectrometry, UPLC-MS/MS)同时测定鸡肉中金刚烷胺和利巴韦林含量的分析方法。方法 样品加入同位素内标后用三氯乙酸和乙酸铵缓冲液提取, 经PBA/PCX复合固相萃取柱净化后, 用Acquity UPLC? HSS T3柱(3.0 mm×150 mm, 1.8 μm)分离, 以乙腈和0.2%甲酸作为流动相进行梯度洗脱, 电喷雾正离子模式(ESI+)电离, 多反应监测模式(multiple reaction monitoring, MRM)进行检测。结果 金刚烷胺在0.2~10 ng/mL范围内线性关系良好, 方法的检出限为(S/N=3)0.02 μg/kg, 在0.6、2.4和12 μg/kg添加水平的平均回收率分别为92.2%、99.2%和99.2%, 相对标准偏差(n=6)为6.2%、4.3%和1.5%。利巴韦林在1.0~50 ng/mL范围内线性关系良好, 方法的检出限为(S/N=3)0.1 μg/kg, 在3.0、12和60 μg/kg添加水平的平均回收率分别为99.0%、97.5%和97.2%, 相对标准偏差(n=6)为4.9%、2.8%和1.4%。结论 该方法简单、灵敏、准确可靠, 适用于鸡肉中金刚烷胺和利巴韦林含量的同时测定。

英文摘要:

      Objective To establish a method for simultaneous determination of amantadine and ribavirin in chicken by automatic solid phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Method The target in the samples was extracted by trichloroacetic acid and ammonium acetate buffer after joining isotope internal standard. Then the extract was purified by PBA/PCX composite solid phase extraction column, and separated by Acquity UPLC? HSS T3 column (3.0 mm×150 mm, 1.8 μm) with acetonitrile and 0.2% formic acid as mobile phase for gradient elution. Samples were detected by UPLC-MS/MS under the electrospray ionization (ESI+) positive ion mode with multiple reaction monitoring (MRM). Results Amantadine had a good linearity in the range of 0.2~10 ng/mL, and the limit of detection (S/N=3) was 0.02 μg/kg. The average recoveries were 92.2%, 99.2% and 99.2% at the spiked levels of 0.6, 2.4 and 12 μg/kg, while the relative standard deviations (n=6) were 6.2%, 4.3% and 1.5%. Ribavirin had a good linearity in the range of 1.0~50 ng/mL, and the limit of detection (S/N=3) was 0.1 μg/kg. The average recoveries were 99.0%, 97.5% and 97.2% at the spiked levels of 3.0, 12 and 60 μg/kg, while the relative standard deviations (n=6) were 4.9%, 2.8% and 1.4%. Conclusion The method is simple, sensitive and accurate, which is suitable for the determination of amantadine and ribavirin content in chicken.