高效液相色谱法测定卷烟主流烟气中的苯并[a]芘

为了测定卷烟主流烟气中苯并a]芘,考察了萃取条件、弗罗里硅土净化条件和色谱分离条件,建立了测定卷烟主流烟气中苯并a]芘的高效液相色谱-荧光检测法,并采用该方法和国标法测定了肯塔基参考卷烟3R4F和国内参比烤烟以及国内50个牌号卷烟样品烟气中的苯并a]芘。结果表明:①用环己烷超声萃取40 min效果较好;②用Agilent ZORBAX Eclipse PAH作色谱柱,乙腈和水为流动相,梯度洗脱,流速2.0 mL/min,30 min内苯并a]芘色谱峰可以和杂质峰有效分开;③该法的平均回收率在98.13%～101.36%之间,RSD在1.29%～4.32%之间;④该方法的测定结果与国标法较为一致,二者不存在显著性差异。该方法适合卷烟主流烟气中苯并a]芘的检测。

Determination of Benzo[a]pyrene in Mainstream Cigarette Smoke by HPLC

A high performance liquid chromatography with fluorescence detection for determining the benzoa]pyrene in mainstream cigarette smoke was developed.The extraction,clean up with Florisil and chromatographic conditions were tested.The Kentucky reference cigarette 3R4F and domestic Virginia type reference cigarette samples and 50 domestic cigarette brands samples were parallel tested with the developed method and national standard method.The results showed that:1)tobacco samples were extracted more effectively with cyclohexane under ultrasonic for 40 minutes;2)benzoa]pyrene was separated effectively in 30 minutes by reversed-phase HPLC with an Agilent ZORBAX Eclipse PAH column under a gradient elution with acetonitrile and water as mobile phase at a flow-rate of 2.0 mL/minute;3)the recoveries of benzoa]pyrene ranged from 98.13% to 101.36% with the relative standard deviation(RSD)of 1.29% to 4.32%;4)there was no significant difference between the results determined with the developed method and national standard method.This method is suitable for determining benzoa]pyrene in mainstream cigarette smoke.