气相色谱-串联质谱法同时测定卷烟滤嘴中15种多环芳烃

Simultaneous determination of 15 polycyclic aromatic hydrocarbons in cigarette filter by gas chromatography-tandem mass spectrometry

建立了气相色谱-串联质谱同时检测卷烟滤嘴中15种多环芳烃的方法。卷烟滤嘴用二氯甲烷振荡萃取后,经0.22μm有机相滤膜过滤,采用DB-5MS色谱柱(30 m×0.25 mm,0.25μm)进行分离,电子轰击源、正离子模式下以多反应监测模式进行检测,内标法进行定量。15种多环芳烃(苊烯、苊、芴、菲、蒽、荧蒽、芘、苯并[a]蒽、屈、苯并[b]荧蒽、苯并[k]荧蒽、苯并[a]芘、二苯并[a,h]蒽、苯并[g,h,i]苝和茚并[1,2,3-c,d]芘)的线性关系良好,相关系数(R^2)为0.991 4~0.999 9。15种多环芳烃在低、中、高3个添加水平下的平均回收率为81.6%~111.2%;除了芴在低添加水平时相对标准偏差为19.2%外,其他相对标准偏差均小于16%。15种多环芳烃的检出限为0.02~0.24 ng/滤嘴,定量限为0.04~0.80 ng/滤嘴。方法前处理简便,具有快速、准确、灵敏度高及重复性好的优点,适用于卷烟滤嘴中多环芳烃的分析。

A method for the simultaneous determination of15polycyclic aromatic hydrocarbons in cigarette filter was developed by isotope internal standard combined with gas chromatography-tandem mass spectrometry.The cigarette filters were extracted with dichlo-romethane,and the extract was filtered with0.22um organic phase membrane.The samples were isolated by DB-5MS column(30mx0.25mm,0.25um)and detected using multiple reac-tion monitoring mode of electron impact source under positive ion mode.The linearities of the15polycyclic aromatic hydrocarbons(acenapthylene,acenaphthene,fluorene,phenanthrene,anthracene,fluoranthene,pyrene,ben[a]anthracene,chrysene,benzo[b]fluoranthene,benzo[k]fluoranthene,benzo[a]pyrene,dibenzo[a,h]anthracene,benzo[g,h,i]perylene and indeno[1,2,3-c,d]pyrene)were good,and the correlation coefficients(R2)ranged from0.9914to0.9999.The average recoveries of the15polycyclic aromatic hydrocarbons were81.6%-109.6%at low,middle and high spiked levels,and the relative standard deviations were less than16%,except that the relative standard deviation of fluorene at the low spiked level was19.2%.The limits of detection of the15polycyclic aromatic hydrocarbons were0.02to0.24ng/filter,and the limits of quantification were0.04to0.80ng/filter.The method is sim-ple,rapid,accurate,sensitive and reproducible.It is suitable for the quantitative analysis of the15polycyclic aromatic hydrocarbons in cigarette filters.