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    基于滤片-吸附管串联捕集的气相色谱-质谱法分析卷烟主流烟气全成分

    Analysis of Total Components of Cigarette Mainstream Smoke by Gas Chromatography-Mass Spectrometry Based on Filter-Adsorption Tube Series Trapping

    • 摘要: 为同时、高效检测卷烟主流烟气全成分,采用自制活性炭吸附管,提出了题示方法,并应用于3R4F参比卷烟的检测。用转盘型吸烟机抽吸卷烟,用直径为92 mm的剑桥滤片捕集卷烟主流烟气粒相物,透过滤片的气相部分通过自制活性炭吸附管(内装0.5 g活性炭)捕集。卷烟抽吸完毕后,收集吸附管及滤片,用二氯甲烷淋洗,加入含2 g·L−1乙酸异丁酯、己酸异丁酯、十一酸乙酯、十七烷酸乙酯的异丙醇溶液(内标),振荡萃取30 min后取上层滤出清液,采用气相色谱-质谱法分析。对检出的未知成分,通过解卷积后采用NIST质谱库检索定性,并辅以保留指数比对确证。结果表明:该方法能够完全捕集卷烟主流烟气全成分,共准确鉴定出257种成分,包括气相成分65种,粒相成分105种,有机蒸汽相(气粒两相共存)成分87种;251种成分的半定量分析结果相对标准偏差(RSD,n=6)不大于10%。建立了19种代表性烟气成分(含气相成分、粒相成分及有机蒸汽相成分)的定量分析方法,19种代表性烟气成分的质量浓度在一定范围内和其峰面积与内标峰面积比值呈线性关系,检出限(3S/N)为3.3~22.4 ng·支−1。按照标准加入法进行回收试验,回收率为79.0%~115%,测定值的RSD(n=6,日内和日间精密度)均小于10%。

       

      Abstract: To simultaneously and efficiently detect the total components of cigarette mainstream smoke, a self-made activated carbon adsorption tube was used, and the method mentioned by the title was proposed and applied to the detection of 3R4F reference cigarettes. Cigarettes were smoked with a rotary smoking machine, using Cambridge filter with a diameter of 92 mm to trap the particulate matter of the mainstream smoke, and the vapor portion passing through the filter was trapped using the self-made activated carbon adsorption tube (containing 0.5 g of activated carbon). After suction of the cigarette, the adsorption tubes and filters were collected and rinsed with dichloromethane, and isopropanol solution containing 2 g·L−1 of isobutyl acetate, isobutyl caproate, ethyl undecanoate, and ethyl heptadecanoate (internal standards) was added. The mixture was extracted for 30 min by oscillation, and the upper layer was filtered out and analyzed by gas chromatography-mass spectrometry. Unknown components detected were qualitatively identified through deconvolution followed by NIST mass spectral library searches, and further confirmed by retention index (RI) comparison. As shown by the results, this method could effectively achieve complete trapping of total components of cigarettes mainstream smoke, accurately identifying 257 components in total, including 65 vapor phase components, 105 particle phase components, and 87 organic vapor phase (coexisting vapor and particle phase) components. The semi-quantitative analysis results for 251 compounds showed RSDs (n=6) were not more than 10%. A quantitative analysis method was established for 19 representative smoke components (including vapor, particle, and organic vapor phase components). Linear relationships between the peak area ratios of 19 representative smoke components to the internal standards and mass concentrations of 19 representative smoke components were found in definite ranges, with detection limits(3S/N) in the range of 3.3−22.4 ng per cigarette. Test for recovery was made by the standard addition method, giving the results in the range of 79.0%−115%, with RSDs (n=6, intra-day and inter-day precision) less than 10%.

       

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