摘要
建立了氨基酸硅烷化衍生-气相色谱-质谱联用法测定烟草中18种游离氨基酸的分析方法。烟叶样品用75%乙醇萃取,萃取液真空干燥后在75℃下加入N-叔丁基二甲基甲硅烷基-N-甲基三氟乙酰胺(MTBSTFA)衍生试剂进行硅烷化衍生反应30 min后在选择离子监测(SIM)模式下进行GC/MS分析,采用内标法定量。结果表明:18种氨基酸的定量标准曲线线性良好,R2为0.9990~0.9999,方法的加标回收率为97.4%~114.1%,相对标准偏差为0.17%~3.4%。该方法前处理操作快速简便、检测灵敏度高,适用于烟草中游离氨基酸含量的定量分析。
A method using silylationderivatization followed by GC/MS was established for the quantitative determination of the free amino acids in tobacco, Tobacco sample was extracted by 75 % alcohol and then the extracted solution was dried in vacuum and silylanized with N-methyl-N - （tert- butyldimethylsilyl） trifluoroacetamide （MTBSTFA） in 75℃ for 30 rain before GC/MS analysis with selected ion monitoring （SIM） mode andinternal standard quantitative determination. The results showed that the 18 free amino acids could be satisfactorily separated with an excellent linearity with correlation coefficients in the range of 0. 9990 and 0. 9999. For all the amino acids, the recoveries were 97.4% - 114. 1% and relative standard deviations were 0. 17% - 3.4%. This proposed method was easy-handling, sensitive and suitable for the quantitative determination of the free amino acids in tobacco.
出处
《分析试验室》
CAS
CSCD
北大核心
2017年第11期1341-1346,共6页
Chinese Journal of Analysis Laboratory
