气袋-热脱附-气/质联用法分析卷烟主流烟气中的气相全成分 |
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引用本文: | 郑赛晶,刘百战,徐中一,孙文梁,吴达.气袋-热脱附-气/质联用法分析卷烟主流烟气中的气相全成分[J].中国烟草学报,2014,20(2):9-0. |
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作者姓名: | 郑赛晶 刘百战 徐中一 孙文梁 吴达 |
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作者单位: | 上海烟草集团有限责任公司 |
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摘 要: | 为了分析比较不同卷烟的气相成分的差异,以及减害降焦过程中卷烟气相成分的变化情况,本文建立了气袋-热脱附-气/质联用法分析卷烟主流烟气中的气相全成分的方法。此方法采用Tedler气袋收集20支卷烟的主流烟气,并用针筒式注射泵定量转移一定体积烟气入Carbotrap300吸附采样管,利用热脱附技术-气/质联用仪(ATD-GC/MS)法进行定性和定量分析。通过方法优化和验证,结果表明:(1)由于针筒式注射泵的取样时间、速率及体积高度可控,大大改进了重复性,气相全成分中,大部分被测物的相对标准偏差都在5%以下,重复性显著优于文献报道;(2)此方法可较完全地捕集卷烟主流烟气气相成分;(3)可定性鉴定出卷烟烟气中的67种成分;(4)采用氘代内标法,准确定量分析了13种气相成分;(5)13种定量成分的回收率在80%~120%之间,结果令人满意。对不同卷烟样品进行分析测试,结果如下:(1)2R4F的测试结果和文献报道值相符;(2)混合型卷烟的气相成分中,含N的气体成分比烤烟型的相对高些;(3)对卷烟滤嘴添加了活性炭材料前后的卷烟分析,可发现,添加了活性炭材料后,大部分气相成分呈不同程度地下降。综合比较认为此方法方便可靠,可应用于日常分析以及对减害材料的评价研究。
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关 键 词: | 气袋 热脱附 气/质联用 主流烟气 气相成分 |
收稿时间: | 2013-04-23 |
Analysis of Vapour Phase Componets inMainstream Smoke by Bag Sample-Thermal Desorption-Gas Chromatography/Mass Spectrometry |
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Abstract: | A method for the analysis of vapour phase (VP) compounds in mainstream smoke (MSS) was described. Cigarettes were smoked on a rotary smoking machine under the standard ISO smoking conditions and the VP that passes through the Cambridge filter pad collected in a Tedlar? bag. On completion of smoking, the bag contents were sampled onto Two Carbotrap 300 adsorption tube containing 3 beds of adsorbents (Carbopack C, Carbopack B and Carboxen III). The tube was subsequently analyzed on an automated thermal desorption (TD) system coupled to a gas chromatography- mass spectrometry (GC/MS) using a VOCOL column. The ATD and GC operating parameters were optimized. The VP of MSS produced by reference cigarette 2R4F and 4 other cigarettes were determined. The results indicated that: 1) the VP compounds in MSS were basically completely trapped by Carbotrap 300. 2) 67 components were identified; 3) The response of GC/MS was found to be linear with the concentration of 13 analytes in the different range; 4) The relative standard deviation (RSD) of 67 components were less than 10%; 5) Satisfactory recoveries were obtained with independent check standards; 6) The Results for the University of Kentucky reference cigarette 2R4F were in good agreement with reported values; 7) The delivery of Propanenitrile and Acetonitrile in MSS of blend type cigarette was higher than which of flue-cured type cigarette; 8)The VP compounds in MSS could be selective filtered by activated carbon. |
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