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建立了测定烟用香精香料中18种氨基酸的液相色谱-串联质谱(LC-MS/MS)方法。以L-正缬氨酸(Nva)为内标,样品经10%甲醇-水溶液(盐酸浓度为0.1 mol/L)萃取、0.22μm水相滤膜过滤后直接进行LC-MS/MS分析。结果表明:18种氨基酸在0.1~10μmol/L范围内,线性相关系数均≥0.9990,3个加标水平的回收率在85.4%~110.0%之间,相对标准偏差(RSD)为1.3%~4.9%。方法的检出限(LOD)和定量限(LOQ)分别为0.00005~0.1和0.0002~0.3μmol/L。该方法准确、灵敏,适合用于烟用香精香料样品中氨基酸的测定。
A liquid chromatography-tandem mass spectrometry (LC-MS / MS) method was developed for the determination of 18 amino acids in tobacco flavor and fragrance. The sample was extracted with 10% methanol-water solution (hydrochloric acid concentration 0.1 mol / L) using L-norvaline (Nva) as an internal standard. LC-MS / MS analysis was performed directly after filtration through a 0.22 μm aqueous filter. The results showed that the linear correlation coefficients of 18 kinds of amino acids in the range of 0.1 ~ 10μmol / L were all ≥ 0.9990. The recoveries of three spiked levels were between 85.4% and 110.0% with relative standard deviations (RSDs) of 1.3% ~ 4.9 %. The limit of detection (LOD) and limit of quantitation (LOQ) of the method were 0.00005 ~ 0.1 and 0.0002 ~ 0.3μmol / L, respectively. The method is accurate, sensitive and suitable for the determination of amino acids in flavor and fragrance samples for tobacco.