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高效液相色谱法测定卷烟滤嘴中截留的主要酚类化合物

Determination of Major Phenolic Compounds Retained by Cigarette Filter with High Performance Liquid Chromatography

  • 摘要: 为准确测定卷烟滤嘴截留主流烟气中的主要酚类化合物,通过考察滤嘴切割方式、萃取液、萃取方式、萃取时间等前处理条件,建立了一种快速、准确测定卷烟滤嘴中对苯二酚、间苯二酚、邻苯二酚、苯酚、对甲酚、间甲酚和邻甲酚7种酚类化合物截留量的高效液相色谱(HPLC)方法,并采用该方法在6家实验室对7种不同滤嘴卷烟样品进行了比对实验。结果表明:①将卷烟抽吸后的滤嘴从烟支端向近嘴端纵向划开后,用50 mL萃取液(1%乙酸+79%甲醇+20%水,体积分数)在室温下超声萃取30 min时,可将卷烟滤嘴中截留的7种主要酚类化合物萃取完全。②7种酚类化合物在0.04~4.00μg/mL浓度范围内线性关系良好(R2均大于0.999),回收率为93.35%~104.50%,相对标准偏差(RSD)小于7.3%。③6家实验室对7种卷烟样品滤嘴截留的7种酚类化合物检测结果的RSD均小于15%,其中5种酚类化合物在10%以下。该方法适用于卷烟滤嘴截留主流烟气中7种酚类化合物的测定。

     

    Abstract: In order to accurately determine the major phenolic compounds(hydroquinol, resorcinol, catechol, phenol, p-cresol, m-cresol, o-cresol) retained by cigarette filters, a rapid and accurate high performance liquid chromatography(HPLC) method was developed by investigating sample pretreatment conditions, such as filter-slitting means, extraction solvent, extraction method, and extraction time. A comparative experiment on seven filter cigarette samples was performed with the developed method among six laboratories. The results showed that: 1) By slitting the filter longitudinally from the tobacco end to the mouth end, then subjecting it to ultrasonic extraction with 50 m L solution(1% acetic acid, 79% methanol and20% water, V/V) for 30 minutes at room temperature, the said phenolic compounds retained in the filter could be completely extracted. 2) Within the concentration of 0.04-4.00 μg/m L, the said phenolic compounds exhibited good linear relations with R2 > 0.999, the recoveries ranged from 93.35% to 104.50% with relative standard deviations(RSDs) < 7.3%. 3) The RSD of the six laboratories in resorcinol and phenol determination was less than 15%, in the other five phenolic compounds determination was less than 10%. This method is suitable for determining the said phenolic compounds in mainstream cigarette smoke retained by cigarette filter.

     

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