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20.0~500.0μg／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1.9~13.6μg／kg及6.3~45.3μg／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。
An analytical method for the simultaneous determination of 23 esters of flavor addi-tive 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 lin-earity in the range of 20. 0-500. 0 μg/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 μg/kg and 6. 3-45. 3 μg/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 rel-ative 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 prod-ucts for rapid screening and quantitative analysis. The method also offered an opportunity to detect more ester additives that may be added in tobacco products.
参考文献
| [1] | Carmines EL;Carmines EL.Evaluation of the potential effects of ingredients added to cigarettes. Part 1: cigarette design, testing approach, and review of results.[J].Food and Chemical Toxicology,20021(1):77-91. |
| [2] | Dempsey R;Coggins CR;Roemer E.Toxicological assessment of cigarette ingredients.[J].Regulatory Toxicology and Pharmacology: RTP,20111(1):119-128. |
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