气相色谱-质谱联用法测定烟用香精中黄樟素及香豆素

GC-MS Determination of Safrole and Coumarin in Tobacco Essence

采用气相色谱-质谱(GC-MS)联用分析技术,提出了烟用香精中香豆素、黄樟素的同时测定方法。色谱柱为DB-1 MS石英毛细管柱,电子轰击离子源,选择香豆素质谱图中m/z89,90,118,146;黄樟素m/z104,131,135,162各4个特征离子用于选择离子检测法检测,根据这4个离子的抽出离子色谱图的峰面积比进行目标物确证,以基峰m/z118,162作两成分的定量分析,方法的检出限(3S/N)均为0.1 mg.kg-1。用色谱保留时间、质谱特征离子同时定性,消除了香精样品中复杂基体的干扰,避免了假阳性结果的出现。

A method of GC-MS in hyphenation was proposed to be used for simultaneous determination of safrole and coumarin in tobacco essence.The DB-1 MS capillary column was used as chromatographic column.Electron ionization（EI） was used as the ion source,and the characteristic ions of m/z 89,90,118,146 for coumarin and m/z 104,131,135,162 for safrole in the respective mass spectrum were selected in SIM mode of detection.Qualification of the essence was attained by the characteristic ions together with the respective retention time and also with the peak area ratio of chromatograms of abstracted ions.Quantification of the essence was attained by using the base peak of m/z 118 as the quantitative ion for coumarin,and of m/z 162 for safrole,as well as using the external standard method.Detection limits（3S/N） found for both the essence were same as 0.1 mg·kg-1.By taking the above mentioned measures in the detection and determination,interferences due to the complex matrixes were effectively eliminated,thus avoiding the possibility of false positive results.