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 chromatographytandem 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,1.8μm)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)0.02μg/kg,在0.6、2.4和12μg/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)0.1μg/kg,在3.0、12和60μg/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。
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×l50 mm, 1.8 μm) with aeetonitrile 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 ktg/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.
出处
《食品安全质量检测学报》
CAS
2018年第1期149-154,共6页
Journal of Food Safety and Quality
关键词
超高效液相色谱串联质谱
金刚烷胺
利巴韦林
鸡肉
ultra performance liquid chromatography-tandem mass spectrometry
amantadine
ribavirin
chicken