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采用超高效液相色谱串联三重四极杆质谱系统建立了检测抗病毒药物金刚烷胺(Amantadine)的分析方法。猪肉样品经提取金刚烷胺后,采用基于QuEChERS原理的EMR快速分散固相萃取进行净化,使用亚2 μm粒径的反相C_(18)色谱柱进行分离,经配有电喷雾离子源的三重四极杆液质联用仪在正离子模式下监测。该方法在1.0~50ng/mL浓度范围内线性良好,相关系数R~2=0.9992;在1.0,5.0和10.0 μg/kg 3个水平的平均添加回收率为80.6%~90.5%,检出限为0.5 μg/kg,精密度为2.1%~3.1%(n=6)。通过对方法灵敏度、精密度和线性范围等参数进行考察,得到所建立的方法能在10 min内对抗病毒药物金刚烷胺完成快速、准确、高灵敏度的检测分析,完全满足法规监测要求。
An analytical method for the detection of antiviral drug Amantadine was developed using an ultra performance liquid chromatography tandem triple quadrupole mass spectrometry system. The pork sample was extracted with amantadine and purified by EMR rapid dispersion solid phase extraction based on the QuEChERS principle. The separation was performed on a reversed-phase C_ (18) column of sub-2 μm particle size. The triplex Quadrupole LC / MS monitors in positive mode. The method was linear in the range of 1.0 ~ 50 ng / mL with the correlation coefficient of R ~ 2 = 0.9992. The average recoveries at three levels of 1.0, 5.0 and 10.0 μg / kg ranged from 80.6% to 90.5% with a detection limit of 0.5 μg / kg and the precision was 2.1% ~ 3.1% (n = 6). The sensitivity, precision and linearity of the method were investigated. The established method was able to detect amantadine rapidly and accurately and sensitively within 10 min, and fully meet the regulatory requirements.