吸附热脱附-气质联用技术分析烟丝中挥发及半挥发性成分

卷烟致香成分是卷烟质量的重要指标,利用吸附热脱附-气相色谱-质谱技术分析了烟丝中挥发及半挥发性成分79种,其中酸性物质17种,碱性物质5种,中性物质57种,为烟草化学研究提供了简单快速的分析方法.     

近红外光谱技术在快速检验制丝过程中烟丝质量均一性上的应用北大核心CSCD

采用近红外光谱技术结合主成分分析-马氏距离法研究了卷烟制丝工艺过程中掺配、加香、贮丝及喂丝等4个工序段中烟丝样品的质量均一性。用主成分分析法提取近红外光谱所包含的特征信息,较全面地反映制丝过程4个不同取样点样本的离散程度,马氏距离可反映制丝过程中烟丝质量的波动情况。此外,采用成品烟丝的模型预测了取样点D处烟丝样品中6种化学成分(总植物碱、总糖、还原糖、总氮、钾和氯)的含量,使不同批次的烟丝样品中化学成分的差异控制在合理范围,降低批次间卷烟产品化学成分含量的波动,能有效稳定品牌香烟的特征风格。     

近红外光谱技术在快速检验制丝过程中烟丝质量均一性上的应用

采用近红外光谱技术结合主成分分析-马氏距离法研究了卷烟制丝工艺过程中掺配、加香、贮丝及喂丝等4个工序段中烟丝样品的质量均一性。用主成分分析法提取近红外光谱所包含的特征信息,较全面地反映制丝过程4个不同取样点样本的离散程度,马氏距离可反映制丝过程中烟丝质量的波动情况。此外,采用成品烟丝的模型预测了取样点D处烟丝样品中6种化学成分(总植物碱、总糖、还原糖、总氮、钾和氯)的含量,使不同批次的烟丝样品中化学成分的差异控制在合理范围,降低批次间卷烟产品化学成分含量的波动,能有效稳定品牌香烟的特征风格。     

硅烷化GC-MS指纹图谱在卷烟品牌分析中的应用

采用硅烷化衍生化法结合气相色谱-质谱(GC-MS)法对卷烟烟丝中的主要化学成分进行检测,获得了21个卷烟样品的烟丝硅烷化GC-MS指纹图谱数据,并应用聚类分析和主成分分析法对烟丝硅烷化GC-MS指纹图谱数据进行综合评价。结果表明,该方法可用于不同品牌卷烟的比较和区分,硅烷化成分的含量分布特征能反映不同品牌卷烟的特性,可为卷烟品牌的风格表征、品质维护和真伪鉴别提供参考。     

几种保润剂对卷烟烟气化学成分的影响

考察了不同类别的保润剂(丙二醇、甘油、27664号保润剂、木糖醇和山梨醇)对卷烟烟气化学成分的影响,包括对烟气总粒相物、烟碱、水分、焦油含量及卷烟烟气中致香成分组成和有害物质含量的变化。结果表明:①加入不同种类的保润剂后对卷烟烟气的化学成分有明显的影响,而且其影响随着添加量的变化而变化。②随着各种保润剂的加入,卷烟烟气中致香成分总量均比空白卷烟烟气显著增大,同时烟气中苯类和胺类有害物质含量也增大。     

应用近红外光谱技术分析烟丝总糖和还原糖的研究

应用傅立叶变换近红外漫反射光谱仪,对同一品牌通过选择不同批号代表性好的卷烟烟丝样品,建立了卷烟烟丝总糖和还原糖的近红外定量分析数学模型,并对不同批号的分析样品进行检验,近红外预测值的平均相对误差为1.01%和0.77%,接近实测值,说明近红外光谱分析技术可用于卷烟烟丝生产质量指标的检测.     

卷烟原料的保润性能研究

采用烘箱法、动态水分吸附分析系统、气相色谱-质谱联用仪(GC-MS)以及电子扫描显微镜技术比较了卷烟原料保润性的差异。结果表明:1原料烟丝平衡含水率为12.68%,膨胀丝为12.45%,混合丝为12.07%,梗丝为11.99%,而且依据不同原料自身结构的不同,填充值差异性明显。2由于原料微结构存在明显性差异,烟丝失水率为7.24%,膨胀丝为7.61%,混合丝为8.37%,梗丝为11.95%,表明了烟丝的物理保润性效果较好。3综合分析原料挥发性成分及含量,烟丝与膨胀丝致香成分含量较多,混合丝次之,梗丝较少。     

“Eclipse”卷烟的热重/差热分析

为了对新型卷烟产品进行剖析,利用热重/差热分析研究了空气氛围下典型性碳加热卷烟"Eclipse"各组成成分的热行为,并计算了主要失重温度段的活化能。结合热失重数据和组成结构对其分解机理进行初步推断和验证。结果表明:1碳棒在356~560℃燃烧放热,失重65%,活化能为149.44 k J/mol,热重/差热分析显示含有碳酸钙成分,空气氛围下碳棒燃烧热解更完全;2200~380℃为卷烟纸主要的热解失重阶段,失重62%,主要是纤维素热解造成。其中碳酸钙含量为12%左右,金属箔为铝箔;3薄片1在191~364℃失重49%,可能是单糖、小分子物质以及纤维素热分解。薄片2在97~253℃失重51%,保润剂、水分和挥发性物质受热分解以及纤维素晶体单糖和其他一些小分子物质因热裂解。薄片1和薄片3结构和成分相似,都接近传统卷烟烟丝,薄片2含更多的单糖和水分。本研究为新型卷烟材料和热源的研发积累详实数据,为进一步研制烟叶原料加热非燃烧状态下化学成分释放和烟丝配比的实验装置和分析方法奠定基础。     

关键制丝工艺对烟气成分中挥发性成分的影响

采用气相色谱-质谱联用仪(GC-MS)测定了不同制丝工艺参数(松散回潮的热风温度、切丝宽度、HT工作蒸汽流量、烘丝热风温度和排潮风门开度)条件下制成的卷烟样品烟气成分中的挥发性成分。结果表明:酯类物质的释放总量在这些工艺参数条件下存在极显著差异的水平,说明酯类物质的释放总量在5种工艺参数不同条件下的变化是极明显的。综合分析部分致香成分和简单酚类的释放总量,选取样品2与样品4的工艺参数条件进行对比可知较高的松散回潮热风温度和烘丝热风温度更加有利于增加卷烟烟气中挥发性成分的释放量;在增加卷烟香吃味方面样品4的工艺参数条件为最佳生产条件,在该工艺条件下生产出的卷烟样品其烟气成分中致香成分的释放总量最多。     

气相色谱-质谱/选择离子监测法分析烟叶中的香味成分

烟草中的致香成分主导着烟草品质的优劣,而烟草的感官香气质量取决于其内在的香味物质组成及其之间复杂的相互作用,因此,准确测定烟草中香味物质的差异对配方设计、加香加料和稳定卷烟产品质量有重要的实际意义.     

一种测定主流卷烟烟气中固相自由基总量的新方法

研究了一种准确测定主流卷烟烟气中固相自由基总量的新方法. 通常人们采用剑桥滤片来捕集主流卷烟烟气中的固相自由基, 但它并不适合用于准确测定主流卷烟烟气中的固相自由基的总量, 研究发现有超过20%的主流卷烟烟气中的固相自由基可以透过剑桥滤片. 找到了一种电子顺磁共振波谱(EPR)信号很小的、适合用来捕集主流卷烟烟气中的固相自由基总量的过滤片. 采用了以在相同条件下测得的1,1-二苯基-2-苦基肼基(1,1-Diphenyl-2-picryl-hydrazyl, 简称DPPH)的EPR信号强度与强煤的EPR信号强度相比得到的相对EPR信号强度与自由基的自旋数建立校准曲线的方法来计算烟气固相自由基的量, 降低了使用不同的电子自旋共振波谱仪造成的对同一种检测样品测定结果的差异. 通过不同实验室内和实验室间的验证实验, 证明了此方法有很好的重复性和重现性.     

固相萃取-超高效液相色谱法测定卷烟主流烟气中丙烯酰胺

建立了一种固相萃取-超高效液相色谱法(SPE-UPLC)快速检测主流烟气中丙烯酰胺的方法。使用剑桥滤片和吸收瓶捕集主流烟气后,蒸馏水做萃取溶剂,采用C18固相萃取小柱对样品液进行纯化,用UPLC检测,外标法定量。UPLC方法采用ACQUITY UPLCTMBEH C181.7μm 2.1×50 mm色谱柱,柱温30℃,流动相为V(乙腈)∶V(水)=6∶94,流速为0.15 mL/min,紫外检测器(TUV)检测波长为202 nm,分析时间为6 min。烤烟型香烟主流烟气中丙烯酰胺的含量为4.75μg/cig。方法的线性范围为0.1~10 mg/mL,线性相关系数为0.9999;平均回收率为98.7%;检出限为10 ng/mL(S/N=3);相对标准偏差为2.3%。该方法适合主流烟气中丙烯酰胺的快速检测。     

不同材料滤嘴对卷烟主流烟气中挥发性羰基化合物截滤性能的研究

吸烟是引起肺癌及相关疾病的主要原因[1]。挥发性羰基化合物(如甲醛、乙醛、丙醛、丙酮、丙烯醛、巴豆醛、丁酮和丁醛)是卷烟主流烟气中含量较高的一类有害成分,含量从几十到几百微克不等[2-3]。这些挥发性羰基化合物特别是甲醛、丙烯醛及巴豆醛具有纤毛毒性,与氰化氢和氨一起,     

甲壳素衍生物对烟草抗菌活性影响的研究

研究了不同浓度，不同种类酸溶解和不同脱乙酰度的壳聚糖以及水溶解羧甲基壳聚糖对烟草中主要霉菌的抑菌活性，以及它们对烟丝内在质量，焦油，烟碱等的影响。结果表明：酸溶解壳聚糖和水溶解羧甲基壳聚糖对烟草霉变微生物均具有抑制作用，醋酸溶解的壳聚糖较水溶解的羧甲基壳聚糖效果好，水溶解的羧甲基壳聚糖较柠檬酸溶解的壳聚糖效果好，且随壳聚糖脱乙酰度的升高，抑菌作用增强，使烟草内在品质有所改善，其主流烟气焦油，烟碱释放量也略有降低。     

卷烟烟气总粒相物中氟节胺含量的检测方法

建立了气相色谱电子捕获器法检测卷烟抽吸过程中氟节胺向主流烟气总粒相物中转移量的方法,卷烟在标准条件下抽吸,用剑桥滤片捕集主流烟气总粒相物,经乙腈提取、石墨碳黑固相萃取柱或自制混合层析柱净化、GC/ECD检测后,外标法定量.氟节胺在0.02 ～20 mg/L范围内线性关系良好,检出限为9.14×10-6 g/L.加标量为...     

Determination of the elemental distribution in cigarette components and smoke by instrumental neutron activation analysis

Cigarette smoking is a major source of particles released in indoor environments. A comprehensive study of the elemental distribution in cigarettes and cigarette smoke has been completed. Specifically, concentrations of thirty elements have been determined for the components of 15 types of cigarettes. Components include tobacco, ash, butts, filters, and cigarette paper. In addition, particulate matter from mainstream smoke (MS) and sidestream smoke (SS) were analyzed. The technique of elemental determination used in the study is instrumental neutron activation analysis. The results show that certain heavy metals, such as As, Cd, K, Sb and Zn, are released into the MS and SS. These metals may then be part of the health risk of exposure to smoke. Other elements are retained, for the most part, in cigarette ash and butts. The elemental distribution among the cigarette components and smoke changes for different smoking conditions.     

Analysis of aromatic amines in cigarette smoke

A method for the analysis of o-toluidine, o-anisidine, 2-naphthylamine, and 4-aminobiphenyl in cigarette mainstream smoke has been developed, which combines the sensitivity of their pentafluoropropionyl (PFP) derivatives in negative ion chemical ionization (NICI) mode with the selectivity of the gas chromatography/tandem mass spectrometry (GC/MS/MS) technique. The use of four deuterated analogues as internal standards along with the application of the standard addition method results in accurate and precise results; the interday precision for the aromatic amines was 3-10% and the accuracy ranged from 97-100%. This method was applied to two American-blend University of Kentucky reference cigarettes, eight American-blend market cigarettes, a bright (flue-cured) tobacco cigarette, and an electrically heated cigarette smoking system (EHCSS). For the American-blend cigarettes there was a linear correlation between aromatic amine yields and mainstream smoke 'tar' ('tar' = total particulate matter - (nicotine + water)), whereas the bright tobacco cigarette and the EHCSS demonstrated significantly lower aromatic amine yields on an equal 'tar' basis. The results support the hypothesis that the nitrogen content of the tobacco, and above all the cigarette combustion temperature, are determining factors for the yields of aromatic amines in smoke.     

Puff-by-puff resolved characterisation of cigarette mainstream smoke by single photon ionisation (SPI)-time-of-flight mass spectrometry (TOFMS): comparison of the 2R4F research cigarette and pure Burley, Virginia, Oriental and Maryland tobacco cigarettes

Soft single photon ionisation (SPI)-time-of-flight mass spectrometry (TOFMS) is applied for the characterisation and comparison of puff-by-puff resolved and total yields of cigarette mainstream smoke from single tobacco type cigarettes (Virginia, Oriental, Burley, and Maryland) and the 2R4F University of Kentucky research cigarette. Puff-by-puff characteristics of various smoke components within one cigarette type as well as between different cigarette types can differ tremendously. This is demonstrated by means of a few selected compounds. Puff yields vary between 15 and 106 μm for acetaldehyde, 6 and 57 μm for NO, and between 1 and 8 μm for butadiene. Thereby, cigarettes containing 100% Oriental and Burley tobacco exhibit a very unique behaviour for the first and last puff. Different cultivation and processing methods as well as burning characteristics are most likely responsible for this. Since the 2R4F cigarette contains all four tobacco types it combines features of all of them. However, for some smoke constituents, smoking of the 2R4F reference cigarette results in exceptionally high yields which might not be attributable to the four pure tobacco types, but to other factors. In addition, comparison of the different cigarettes was also carried out by normalising the yields to puff resolved particulate matter. This procedure minimises effects caused by unequal smoke formation and represents another approach in evaluating the data.     

Investigation,by single photon ionisation (SPI)–time-of-flight mass spectrometry (TOFMS), of the effect of different cigarette-lighting devices on the chemical composition of the first cigarette puff

Soft single-photon ionisation (SPI)–time-of-flight mass spectrometry (TOFMS) has been used to investigate the effect of different cigarette-lighting devices on the chemical composition of the mainstream smoke from the first cigarette puff. Lighting devices examined were a Borgwaldt electric lighter, a propane/butane gas lighter, a match, a candle, and the burning zone of another cigarette. To eliminate the effects of the different masses of tobacco burnt by use of the different lighting methods a normalisation procedure was performed which enabled investigation of changes in the chemical patterns of the resulting smoke. When another cigarette was used as the lighting device, elevated levels of ammonia and other nitrogen-containing substances were observed. These are high in the sidestream smoke of the cigarette used for lighting and would be drawn into the mainstream smoke of the cigarette being lit. In contrast, smoke from the cigarette lit by the electric lighter contained slightly higher normalised amounts of isoprene. Lighting the cigarette by use of a candle resulted in larger amounts of substances, e.g. benzene, which most probably originated from thermal decomposition of wax. The composition of the first puff of smoke obtained by use of the three lighting methods with open flames (gas lighter, match, and candle) was usually similar whereas the composition of the smoke produced by use of the electric lighter and the cigarette as the lighter were more unique. The chemical patterns generated by the different lighting devices could, however, be separated by principal-component analyses. Two additional test series were also studied. In the first the cigarette was lit with an electric lighter, then extinguished, the ash was cut off, and the cigarette was re-lit. In the second the cigarette was heated in an oven to 80 °C for 5 min before being lit. These treatments did not result in changes in the chemical composition compared with cigarettes lit in the ordinary way. Figure Time-of-flight mass spectrometry (TOFMS) has been used to investigate the effect of different cigarette-lighting devices on the chemical composition of the mainstream smoke from the first cigarette puff     

New insights into the formation of volatile compounds in mainstream cigarette smoke

A sampling system has been set up to monitor a group of volatile smoke analytes (nitric oxide, acetaldehyde, acetone, benzene, toluene, 1,3 butadiene, isoprene and carbon dioxide) from mainstream cigarette smoke on a puff-resolved basis. The system was able to record gas evolution profiles during puffing and interpuff periods without interruption (e.g. taking clearing puffs). Gas phase smoke analytes were sampled as close to the mouth end of the cigarette filter as possible in order to minimise any dead volume effect. The results revealed that, for some volatile species, a significant fraction (e.g. up to 30% for benzene) in the cigarette mainstream smoke had been generated during the preceding smoulder period. These species were trapped or absorbed within the cigarette rod and then subsequently eluted during the puff. The identification of the two sources of the mainstream smoke, a smouldering source and a puffing source, has not been reported before. The observation contributes to the fundamental knowledge of the cigarette smoke formation and may have implications on wider smoke chemistry and associated effects.