固相萃取净化-双填料反萃取-GC/MS法分析卷烟烟气中甲基丁香酚  

Analysis of methyleugenol in mainstream cigarette smoke by solid phase extractiondouble packing reverse extraction coupled with GC/MS

作　　者：廖惠云[1] 吴洋[1] 孙海平[1] 叶远青 王晨辉[1] 曹毅[1] 张华[1] 朱怀远[1] LIAO Huiyun;WU Yang;SUN Haiping;YE Yuanqing;WANG Chenhui;CAO Yi;ZHANG Hua;ZHU Huaiyuan(China Tobacco Jiangsu Industrial Co.,Ltd.,Nanjing 210019,China)

机构地区：[1]江苏中烟工业有限责任公司,南京市210019

出　　处：《烟草科技》2021年第4期66-73,共8页Tobacco Science & Technology

基　　金：江苏中烟工业有限责任公司科技创新项目“细支卷烟用爆珠对逐口烟气中主要香味物质释放量影响研究”(201703)和“细支卷烟中香精料液代表性组分释放转移分析及应用研究”(201704)。

摘　　要：为定量分析卷烟主流烟气中的甲基丁香酚,采用固相萃取净化-双填料反萃取-气相色谱/质谱法进行检测,研究了主流烟气中目标物的捕集方式;甄选出合适的净化用固相萃取柱,并优化了固相萃取淋洗条件;设计了双填料的洗脱液除水反萃取装置,确定了合适填料用量;优化了色谱仪器分离和分析条件。结果表明:(1)在优化条件下,目标物在10~400 ng/mL范围内线性良好(R^(2)为0.9995),日内和日间相对标准偏差(RSD)分别为6.86%和8.73%,样品加标回收率在97.2%~114.5%之间,方法的检出限和定量限分别为0.24和0.81 ng/支,明显优于现有文献结果。(2)采用该方法分析部分市售卷烟,混合型和烤烟型卷烟烟气中甲基丁香酚的释放量范围分别为2.46~3.52和2.24~5.13 ng/支,前者的单位焦油释放量远高于后者。An analytical method was developed for analyzing methyleugenol in mainstream cigarette smoke by using solid-phase extraction purification-double packing reverse extraction coupled with gas chromatography/mass spectrometry.The trapping method of target compound in mainstream smoke was studied,and the suitable solid-phase extraction condition was selected and optimized successively.By optimizing the amount of packings,a device with double packings was prepared for back extracting from water-organic solvent system.The influence on the chromatographic peak of target compound with different chromatographic injection mode was discussed,and the mass spectra ion parameters were finally decided.The results showed that:(1)under the optimized condition,the method presented good linear relationship(R^(2)=0.9995)in the range of 10-400 ng/mL.The intra-day and inter-day relative standard deviations(RSD)were 6.86%and 8.73%respectively,and the rate of spiked recovery was between 97.2%and 114.5%.The limit of detection(LOD)was 0.24 ng/cig,while the limit of quantization(LOQ)was 0.81 ng/cig,which were obviously better than the existing literature results.(2)By analyzing some cigarettes selected from the market,the yields of methyl eugenol in blended type cigarettes was in the range of 2.46-3.52 ng/cigarette,while 2.24-5.13 ng/cigarette in Virginia type cigarettes.In addition,the release amount of methyl eugenol per tar of the former was far higher than the latter.

关 键 词：固相萃取 双填料反萃取 气相色谱/质谱 卷烟主流烟气 甲基丁香酚 

分 类 号：TS411.2[农业科学—烟草工业]