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

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.