同位素稀释-气相色谱-质谱法同时测定卷烟滤嘴截留烟气中的烟碱和6种挥发酚

Determination of Nicotine and Volatile Phenols Retained by Cigarette Filter by Istope Dilution Gas Chromatography-mass Spectrometry

建立了同位素稀释-气相色谱-质谱联用(GC/MS)测定卷烟滤嘴截留烟气中的烟碱和6种酚(苯酚、对、间-甲酚、邻-甲酚、对-苯二酚、邻-苯二酚和间-苯二酚)的分析方法。在标准抽吸条件抽吸4支卷烟,并收集抽吸后的滤嘴,纵向切开,用含内标苯酚-d5和烟碱-d3的甲醇超声萃取后,采用TG-1MS毛细管柱(30 m×0.25 mm, 0.25μm)分离,选择离子模式方式进样检测,同位素内标法定量。方法经优化后,烟碱和6种酚具有良好线性,r为0.999 0~0.999 9,方法的检出限(LOD)和定量限(LOQ)分别为7.5~25 ng/支和25~50 ng/支,加标回收率为91.7%~102.6%,相对标准偏差为1.9%~6.2%。该方法操作简便、结果准确可靠,可用于测定卷烟滤嘴截留烟气中的烟碱和6种挥发酚。

A method was developed for the simultaneous determination of nicotine and 6 kinds of phenols(phenol,p,m-cresol,o-cresol,p-catechol,o-catechol and m-catechol)retained by cigarette filter with ultrasonic-assisted extraction-isotope dilution-gas chromatography-mass spectrometry.Four cigarettes were smoked under ISO smoking regimes,and the smoked filters were collected and slitted longitudinally.After ultrasonic extraction with methanol solution containing internal standards,phenol-d5 and nicotine-d3,the samples were analyzed by GC/MS in selective ion mode,and quantified by internal standard method.By method optimization,nicotine and 6 kinds of phenols exhibited good linear relationships with r^(2) ranging from 0.9990 to 0.9999.The limits of detection(LOD)and limits of quantitation(LOQ)of the method were 7.5~25 ng/cigarette and 25~50 ng/cigarette,respectively.The recoveries ranged from 91.7%to 102.6%with relative standard deviations(RSDs)ranging from 1.9%to 6.2%.The method was simple,sensitive and suitable for the determination of nicotine and 6 phenols retained by cigarette filters.