硅烷化衍生/气相色谱法测定烟草中的脱氧果糖嗪

目的]以2,5-脱氧果糖嗪为标样,采用气相色谱方法准确测定烟草中脱氧果糖嗪的含量。方法]以吡啶与二甲基亚砜（V/V=1∶1）的混合溶剂为衍生溶剂,双（三甲基硅烷基）三氟乙酰胺（BSTFA）为衍生试剂对脱氧果糖嗪进行硅烷化衍生,衍生后的烟草样品以2,5-脱氧果糖嗪为标样,用气相色谱进行定量分析。结果]80℃下衍生60 min后,脱氧果糖嗪标准曲线的线性回归系数为0.999 4,线性范围7.08~70.80μg/ml。脱氧果糖嗪的检出限为1.42μg/ml,回收率为93.0%,RSD值为5.95%。结论]该方法可靠,具有良好的分析效果,可用于准确测定烟草中脱氧果糖嗪的含量。

Study on Determination of Deoxyfructosazine in Tobacco Using Silylation Derivatization Coupled with Gas Chromatography

Objective]Based on the synthesis of 2,5-deoxyfructosazine,a method for the determination of deoxyfructosazine was researched to analyze tobacco samples.Method]Using the mixture of Pyridine with DMSO(V/V=1∶1) as the solvent and N,O-bis(trimethylsilyl)-trifluoroacetamide as derivatization reagent,DOF in tobacco samples was quantitatively analyzed by gas chromatography according to the standard curve of 2,5-deoxyfructosazine.Result]After the samples reacted with BSTFA at 80 ℃ for 60 min,the samples were determined.The results showed the linearity correlation was 0.999 4,the linearity range of calibration curve was 7.08-70.80 μg/ml,the relative standard deviation of DOF was 5.95%,the recovery was 93.0%,and the detection limit was 1.42 μg/ml respectively.Conclusion]An effective GC method was developed to analyze the DOF compounds in tobacco.The method was suitable to accurately determine the contents of DOF compounds in tobacco.