分散液液微萃取/气相色谱-质谱法同时测定烟用添加剂中8种烷基苯类香味有害物

建立了超声溶剂提取和分散液液微萃取(DLLME)相结合的提取、净化前处理技术,采用气相色谱-质谱法分析了烟用添加剂中的黄樟素、侧柏酮、龙蒿脑、胡薄荷酮、甲基丁香酚、香豆素、6-甲基香豆素和7-甲氧基香豆素8种烷基苯类香味有害物。对分散液液微萃取溶剂及其体积、分散剂及其体积、萃取时间等条件进行了优化。在最佳实验条件下,8种有害物的线性范围为0.4～928μg/L(r2≥0.998 9),检出限为0.04～0.24μg/L,定量下限为0.13～0.80μg/L,富集倍数为140～208倍,方法的加标回收率为90%～100%,相对标准偏差为2.4%～6.7%。与行业推荐的测定方法相比,该方法具有灵敏度高、富集效果好、回收率高等优点。

Simultaneous Determination of Alkenylbenzenes and Other Flavor-related Compounds in Tobacco Additives by Dispersive Liquid-Liquid Micro-extraction and GC-MS

A new ultrasonic-assisted extraction followed by dispersive liquid-liquid micro-extraction(DLLME) and GC-MS analysis method was developed for the simultaneous determination of eight alkenylbenzenes and other flavor-related compounds including safrole,coumarin,6-methylcoumarin,7-metheoxycoumarin,estragole,methyleugenol,pulegone and thujone in tobacco additives.The different parameters affecting the whole process such as the type and volume of extraction and disperser solvents,the salt addition and the extraction time were studied.Under the optimum conditions,the enrichment factors(EF) ranged from 140 to 208.The linear relationships of eight alkenylbenzenes and other flavor-related compounds were obtained in the range of 0.4-928 μg/L,with correlation coefficients(r2) over 0.998 9.The limits of detection(LOD) and the limits of quantitation(LOQ) were in the ranges of 0.04-0.24 μg/L and 0.13-0.80 μg/L,respectively.The average recoveries were in the range of 90%-100% with relative standard deviations(RSDs) of 2.4%-6.7%.The method was successfully applied in the analysis of real tobacco flavor additive samples.Compared with the industry recommended standard method,lower concentrations of detection were achieved due to the high enrichment power of DLLME.Therefore,this method shows tremendous potential in trace analysis of alkenylbenzenes and other flavor-related compounds in real samples.