固相萃取结合气相色谱-串联质谱法测定烟草制品中23种酯类香料

利用固相萃取结合气相色谱-串联质谱(SPE-GC-MS/MS)检测技术建立了烟草制品中23种酯类香料的定量分析方法。样品以乙酸乙酯为提取溶剂,经NH₂固相萃取柱(依次用甲醇和水活化)净化,用4 mL乙酸乙酯洗脱,在多反应监测(MRM)模式下进行检测。结果表明,23种香料在20.0~500.0 μ g/L范围内线性关系良好(r² > 0.996),检出限(LOD, S/N=3)及定量限(LOQ, S/N=10)分别为1.9~13.6 μ g/kg及6.3~45.3 μ g/kg,在1、1.5、2倍定量限的加标水平下,平均回收率为62.1%~91.4%,相对标准偏差(RSD)均小于7%。该方法准确可靠、灵敏度好,适用于烟草制品中23种常用酯类香料的快速筛查与定性、定量分析。该方法为烟草中酯类物质的检测开拓了平台。

Analysis of 23 esters of flavor additive in tobacco products by gas chromatography-tandem mass spectrometry coupled with solid-phase extraction

An analytical method for the simultaneous determination of 23 esters of flavor additive in tobacco products was established based on optimized solid-phase extraction (SPE) with gas chromatography-tandem mass spectrometry (GC-MS/MS). The samples were extracted with ethyl acetate, cleaned up by an amino SPE column. After conditioning step, the extracts were eluted by 4 mL ethyl acetate, and then were determined by GC-MS/MS in multi-reaction monitoring (MRM) mode. The results showed that all the 23 ester flavor additives had good linearity in the range of 20.0-500.0 μ g/L, with the correlation coefficients (r²) better than 0.996. The limits of detection (LODs) and limits of quantitation (LOQs) of these additives were in the ranges of 1.9-13.6 μ g/kg and 6.3-45.3 μ g/kg, respectively. The average recoveries of the 23 analysts were in the range of 62.1%-91.4% at the spiked levels of 1, 1.5, 2 times LOQ with relative standard deviations (RSDs) typically lower than 7%. The accurate, reliable and sensitive method can be applied to the determination of the 23 esters of flavor additive in tobacco products for rapid screening and quantitative analysis. The method also offered an opportunity to detect more ester additives that may be added in tobacco products.