采用自主研制的新型空气动力辅助离子化质谱技术(AFAI—MS)及其装置,对违法饲料添加的未知药片进行了快速实时质谱分析,并对其中的药效成分进行了结构鉴定研究。通过本技术快速、高效地获取了药片中有效成分的一级质谱、二级质谱、分子离子的精确质量数等关键结构信息。在此基础上,结合“抗胆碱”的药理作用以及网络数据库搜索结果,分析推断出该药效成分为山莨菪碱;并结合对照品比对分析,最终确定该未知药片为山莨菪碱片。本方法为药物相关领域中复杂样品的快速实时检测提供了有效的分析途径,并为打击药品违法添加提供了重要的分析依据。
A procedure was described for the fast and direct structural identification of active ingredients in an unknown tablet, which was illegally used as feed additive. The mass spectra, product ion spectra and accurate mass measurement results were acquired by the fast and direct MS analysis of the tablet with a homemade air flow assisted ionization (AFAI) coupling with commercial available mass spectrometers. From these results, the key structure information (molecular weight and formula) of the active ingredient was proposed, and then "cholinolytic effect" and "molecular weight 305" were used as the key word for the information search on the internet. The search results indicated that the active ingredient is raceanisodamine. Finally, the comparison between the MS/MS spectra of the unknown tablet and that of reference raceanisodamine was carried out, and it was confirmed that the unknown tablet is raceanisodamine. The results provided an important evidence to deal with the illegal usage pharmaceuticals as feed additive. AFAI-MS would be a rapid and effective method for the analysis of complex mixture in the field related to pharmaceuticals.