加速溶剂/固液固萃取-气相色谱/质谱法分析卷烟烟气中苯并a芘

摘要

A novel sample preparation method for trace benzo[a] pyrene (BaP) in tobacco cigarette smoke by accelerated solvent/solid-liquid-solid extraction (AS/SLSE) has been developed,which integrated extraction and purification in one step.The tobacco cigarette samples were trapped,then extracted and purified by AS/SLSE.The extracts were concentrated before analysis by chromatography.The extraction conditions such as adsorbents,extraction temperature,flush volume,static extraction time and static cycles,were optimized.Under the optimized condition (5 g silicon magnesium sorbent,extraction temperature at 100 ℃,flush volume of 40％,static extraction time of 3 min and for 2 static cycles,the extraction process was repeated three times),the limit of detection was 1.0 μg/L and the average recovery was 97.1％ for determination of benzo [a] pyrene in tobacco cigarette smoke by AS/SLSE coupled with gas chromatography/mass spectrometry (GC/MS).The relative standard deviation was 2.5％.The developed method was successfully applied to the analysis of tobacco cigarette smoke sample,the analytical results accord with those obtained by current national standards recommended method.%建立了集萃取与净化于一体的加速溶剂/固液固萃取(AS/SLSE)卷烟烟气中痕量苯并[a]芘(BaP)的样品前处理方法.卷烟烟气经捕集后,用AS/SLSE提取和净化,萃取液浓缩后进行色谱分析.优化了AS/SLSE吸附剂、萃取温度、吹扫体积、静态萃取时间及循环次数等条件.在优化条件下(5 g硅镁型吸附剂、萃取温度100℃、吹扫体积40％、静态萃取时间3 min循环2次,样品连续萃取3次),AS/SLSE-气相色谱/质谱法(GC/MS)分析卷烟烟气中苯并[a]芘方法的检出限为1.0μg/L,回收率为97.1％,相对标准偏差(RSD)为2.5％.方法成功用于卷烟烟气样品的分析,测定结果与国家标准推荐方法吻合.