超声萃取-快速HPLC法测定卷烟主流烟气中的苯酚、甲酚和苯二酚

Determination of Phenol,Cresols,and Dihydroxybenzenes in Mainstream Cigarette Smoke with Ultrasonic Extraction and Fast HPLC

建立了超声萃取-快速高效液相色谱同时测定卷烟主流烟气中的苯酚、甲酚和苯二酚的方法。即用1%的醋酸水溶液于室温下对捕集了烟气粒相物的剑桥滤片超声萃取20min,将萃取液用0.45μm滤膜过滤后,滤液直接用配置荧光检测器的快速分离柱-高效液相色谱进行分析。并应用该法测定了10种国产烤烟型和10种混合型卷烟主流烟气中的挥发酚,结果表明:①该法的相对标准偏差为1.92%～4.62%,回收率97.9%～100.3%,检测限5.74～14.70ng/支,分析时间6min;②烤烟型卷烟主流烟气中苯二酚、苯酚的含量明显高于混合型卷烟,而甲酚的含量整体上略高于混合型;③同类型卷烟主流烟气中挥发酚含量高低的次序为p-苯二酚>o-苯二酚>苯酚>(m、o)-甲酚>p-甲酚>m-苯二酚。该法适合批量卷烟主流烟气中苯酚、甲酚和苯二酚的快速分析。

A method based on ultrasonic extraction combined with fast high performance liquid chromatography for simultaneously determining phenol, cresol, and dihydroxybenzene in mainstream cigarette smoke （MS） was developed. The total particulate matter collected on Cambridge filter pad was extracted with 1% acetic acid under ultrasonic for 20 minutes. The extract was filtrated with 0.45 μm filter membrane, then separated and detected by HPLC with a fast separation column and a fluorescence detector. The volatile phenols in MS of 10 brands of domestic Virginia type and 10 brands of blended type cigarettes were determined with this method. The results indicated that： 1 ）the recoveries of the method were from 97.9% to 100.3% with RSD of 1.92% -4.62% and the limit of detection of 5. 74 to 14. 70 ng/cig, the analyzing took 6 minutes; 2） the contents of dihydroxybenzenes and phenol were much higher in MS of Virginia type cigarettes than in MS of blended type cigarettes, while the content of total cresols was slightly higher in MS of Virginia type cigarettes; and 3 ） in MS of same type cigarettes, the volatile phenols in order of content were p - dihydroxybenzene 〉 o - dihydroxybenzen 〉 phenol 〉 m, o - cresol 〉 p - cresol 〉 m - dihydroxy- benzene. The method is suitable for the fast analysis of volatile phenols in batches of MS samples.