农业执法案件中未知粉末的分析研究

Analysis of Unknown Powder in Agricultural Law Case

为了对农业执法案件中缴获的未知粉末进行分析研究,采用超高效液相色谱-飞行时间高分辨质谱(UPLC-TOF-HRMS)获得未知物分子离子峰的精确质量数、天然同位素及高质量二级碎片信息,并应用SCIEX PeakView及MasterView软件进行分析。经过靶向及非靶向筛查,同时参考文献报道,推导出未知粉末中的疑似化合物,并采用高效液相色谱-二极管阵列检测器(HPLC-PDA)法及UPLC-TOF-HRMS法进行了双重确证。结果显示该未知粉末中含克仑特罗(16 g/kg)及其合成中间体克仑特罗杂质B(455 g/kg)。研究中详述的分析技术可为未知添加物的筛查、确证提供思路和技术参考。

A study about the screening,analysis and confirmation of unknown compounds in agricultural law case had been implemented.First,the screening of the sample through ultra-performance liquid chromatography coupled with time of flight high resolution mass spectrometry(UPLC-TOF-HRMS)was carried out.Accurate mass of the precursor ion,isotopic intensity ratio,and characteristics of secondary ion fragments of two unknown substances were detected in the positive ion modes of mass spectrometry.Then this information was imported into SCIEX PeakView and MasterView software.Using targeted and non-targeted analysis technology combined with literature reports,unknown substances were presumed.Finally,double confirmation was accomplished by HPLC with photodiode array detector(HPLC-PDA)and UPLC-TOF-HRMS.Clenbuterol and clenbuterol impurity B as the unknown compounds were identified and detected at 16 g/kg and 455 g/kg respectively in this sample.The research may provide a technical reference for the screening and identifying of unknown additives.