Shi Jiaqin, Liu Baizhan, Xie Wenyan
Technical Center, Shanghai Tobacco (Group) Corporation, Shanghai 200082, China.
Se Pu. 2010 Jun;28(6):623-7. doi: 10.3724/sp.j.1123.2010.00623.
The mid-point restrictor, known as the key spare part of multidimensional gas chromatography (MDGC), was modified and applied in the determination of benzo[a] pyrene in cigarette smoke. The graphite restrictor was replaced by a 0.25 mm i.d. fused silica open tubular and the two-hole graphite ferrule was replaced by a press-fit glass Y-splitter to improve the stability of retention time on the 1st dimensional column and eliminate the carry-over effects of graphite. The cigarette samples were prepared as follows: The mainstream cigarette smoke collected on Cambridge pad was extracted with cyclohexane, then the extractant was analyzed by heart cut MDGC-mass spectrometry (MS) directly with benzo [ a] pyrene-d12 as internal standard. The method was proved to be simple, sensitive, fast and reliable with good linearity (linear range of 1.47-29.4 microg/L, r2 of 0.9999), reproducibility (relative standard deviation (RSD) of 1.94%), recovery (90.74%-101.86%) and low quantitative and qualitative detection limits. Moreover, the amount of benzo [a] pyrene in the 2R4F Kentucky reference cigarette smoke obtained by this method was close to that reported in literature.
中点限流器作为多维气相色谱(MDGC)的关键备件,进行了改进并应用于卷烟烟气中苯并[a]芘的测定。将石墨限流器替换为内径0.25 mm的熔融石英开口管柱,将两孔石墨卡套替换为压配玻璃Y形分流器,以提高一维柱上保留时间的稳定性并消除石墨的残留效应。卷烟样品制备如下:收集在剑桥滤片上的主流卷烟烟气用环己烷萃取,然后以苯并[a]芘-d12为内标,直接通过中心切割MDGC-质谱(MS)分析萃取剂。该方法被证明简单、灵敏、快速且可靠,具有良好的线性(线性范围为1.47 - 29.4 μg/L,r2为0.9999)、重现性(相对标准偏差(RSD)为1.94%)、回收率(90.74% - 101.86%)以及低定量和定性检测限。此外,用该方法测得的2R4F肯塔基参考卷烟烟气中苯并[a]芘的含量与文献报道值相近。