在线甲基衍生化-气相色谱-质谱法测定烟用香精香料中油酸  

GC-MS Determination of Oleic Acid in Tobacco Flavor with On-Line Pyrolytic Methylation

作　　者：汤晓东[1] 陈晓水[1] 蒋佳磊[1] 杨艳芹[1] 潘力[1] 陆明华[1] 朱书秀[1] 

机构地区：[1]浙江中烟工业有限责任公司,杭州310024

出　　处：《理化检验（化学分册）》2017年第8期950-953,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：提出了在线甲基衍生化-气相色谱-质谱法测定烟用香精香料中油酸的方法。烟用香精香料样品与四甲基氢氧化铵溶液(衍生化试剂)同时进样,在280℃气相进样口瞬间生成油酸甲酯。在气相色谱分离中用DB-5MS毛细管色谱柱为固定相,在质谱分析中采用选择离子监测模式,以萘为内标物。油酸的线性范围为25~1 000mg·kg^(-1),方法的检出限(3S/N)为0.35mg·kg^(-1),测定下限(10S/N)为1.10 mg·kg^(-1)。以空白样品为基体进行加标回收试验,所得回收率为92.6%~98.8%,测定值的相对标准偏差(n=6)为3.2%~6.3%。A method of GC-MS for the determination of oleic acid in tobacco flavor with on-line pyrolytic methylation was proposed.The sample of tobacco flavor was injected together with TMAH solution（derivation agent）,and immediately methyl oleate was produced in gas injector port of 280 ℃.The DB-5MS capillary chromatographic column was used for GC separation and the selected ion monitoring mode was adopted in MS determination.Naphthalene was used as internal standard.Linearity range of oleic acid was found between 25mg·kg^（-1） and 1 000mg·kg^（-1）,with detection limit（3S/N）of 0.35mg·kg^（-1） and lower limit of determination（10S/N）of 1.10mg·kg^（-1）.On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 92.6%-98.8%,with RSD′s（n=6）in the range of 3.2%-6.3%.

关 键 词：气相色谱-质谱法 在线甲基衍生化 油酸 烟用香精香料 

分 类 号：O657.63[理学—分析化学]