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建立了在线液相-气相二维色谱测定卷烟主流烟气中的苯并[a]芘方法。采用剑桥滤片捕集烟气粒相物,环己烷萃取,以D12-苯并[a]芘为内标,然后用在线液相-气相二维色谱测定:样品直接进样进入液相色谱,经微型硅胶柱分离,含苯并[a]芘的部位切割进入气相色谱,排干溶剂后启动气相色谱升温,经毛细管柱进行分离,用质谱检测。本方法将烟气苯并[a]芘测定中的硅胶柱层析和气相色谱-质谱分析在线连接起来,可不经样品前处理净化直接进样分析;而且每次进样可达40#L,与常规气相色谱-质谱分析最大进样2.0#L相比,分析灵敏度提高了20倍。方法线性范围达0.08~50 ng/L,相关系数为r2=0.999,回收率为94.2%~105.5%;检出限和定量限分别为0.09和0.30 ng/支,应用本方法对14个不同类型市售卷烟和2R4F标准烟进行了测定,结果与GB/T21130-2007测定结果相符合。
A method for the determination of benzo [a] pyrene in mainstream cigarette smoke by on-line liquid-gas two-dimensional chromatography was established. Coulomb particulate matter was collected by Cambridge filter and extracted with cyclohexane. D12-benzo [a] pyrene was used as an internal standard and then measured by on-line liquid-gas two-dimensional chromatography. The sample was directly injected into liquid chromatography , Separated by micro-silica gel column, and the parts containing benzo [a] pyrene were cut into gas chromatograph, the solvent was drained, and the temperature was increased by gas chromatography. The sample was separated by capillary column and detected by mass spectrometry. In the method, the silica gel column chromatography and the gas chromatography-mass spectrometry analysis in the determination of benzo [a] pyrene in the flue gas are online connected and can be directly purged without sample pretreatment; furthermore, the injection can reach 40 # The analytical sensitivity is increased by a factor of 20 over the conventional GC-MS maximum injection of 2.0 # L. The linear range of the method was 0.08-50 ng / L with the correlation coefficient of r2 = 0.999 and the recovery of 94.2% -105.5%. The limits of detection and quantification were 0.09 and 0.30 ng / Commercial cigarettes and 2R4F standard smoke were measured and the results were in accordance with the results of GB / T21130-2007.