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  

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

作　　者：郑阳[1,2] 许秀丽[1] 纪顺利 袁飞[1] 黄志强 杨丙成[2] 张峰[1] 

机构地区：[1]中国检验检疫科学研究院烟草安全与控烟技术中心/食品安全研究所,北京100176 [2]华东理工大学药学院,上海200237 [3]湖南省南检验检疫科学技术研究院,湖南长沙410004

出　　处：《色谱》2016年第5期512-519,共8页Chinese Journal of Chromatography

基　　金：质检公益性行业科研专项(201410088,201310134);中国检验检疫科学研究院基本科研业务费项目(2016JK009,2015JK008);国家质检总局科研计划项目(2014IK084);国家重大仪器设备开发专项(2012YQ14000806)~~

摘　　要：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(r^2>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 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 μg/L,with the correlation coefficients（r-2）better than0. 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 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 op-portunity to detect more ester additives that may be added in tobacco products.

关 键 词：固相萃取 气相色谱-串联质谱 酯类香料 烟草制品 

分 类 号：O658[理学—分析化学]