卷烟主流烟气中部分成分在滤嘴中的截留效率研究
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摘要
卷烟主流烟气成分非常复杂,含有多种有害物质,由于卷烟滤嘴能选择性地截留某些有害成分,因此研究卷烟滤嘴的截留效率是卷烟减害降焦的一个重要方面。本论文分析了卷烟滤嘴对低分子醛酮化合物、多环芳烃中的苯并[a]芘及氰化氢的截留效率、针对不同材料滤嘴、不同抽吸方式对烟气中的这些成分的截留效率影响进行了研究,以此为滤嘴选材、成型改性和降焦减害等提供科学的理论依据和数据支撑。具体研究内容如下：
(1)利用高效液相色谱检测法研究了滤嘴对卷烟主流烟气中低分子醛酮化合物的截留效率。主流烟气用加有2,4-二硝基苯肼(DNPH)的剑桥滤片捕集,采用2%(V/V)吡啶-乙腈作为萃取剂,振荡后上样。滤嘴用DNPH-甲醇溶液作萃取剂,振荡后取萃取液经滤膜过滤,用高效液相色谱分析。结果表明：甲醛、乙醛、丙酮、丙烯醛、丙醛、巴豆醛、2-丁酮及丁醛检出限为0.06～0.15μg/cig,定量限为0.20-0.51μg/cig;回收率为85.7%～92.4%,相对标准偏差为1.79%～5.74%。滤嘴截留低分子醛酮化合物的效率在1.2%～27.4%之间。该方法定量准确可靠,重现性好,可行性高。
(2)用GC/MS分析了滤嘴截留卷烟主流烟气中苯并[a]芘的效率。滤嘴和滤片处理方法一致：用加有内标的环己烷作为萃取液,超声萃取后过固相萃取柱,经洗脱、纯化和收集后旋转蒸发,浓缩至约0.5mL,转移至色谱瓶中,待GC/MS分析。苯并[a]芘的线性方程为：y=1.197e+003x-7.340e+003,相关系数为0.9999,检出限和定量限分别为0.9ng/mL、3.0ng/mL。结果显示,滤嘴截留苯并[a]芘的效率为18.3%～45.8%。
(3)采用超高效液相色谱(UPLC)的方法分析滤嘴对主流烟气中苯并[a]芘的截留效率。滤嘴和滤片采用同样方法同时处理：用环己烷作为萃取液,超声萃取,萃取液旋转蒸发至干,残渣用乙腈溶解后上样。抽吸不同的滤嘴的卷烟及在不同的抽吸方式下得出滤嘴截留效率的范围。苯并[a]芘线性方程为：y=1.9479x+39800,相关系数为0.9999。苯并[a]芘的最低检测限为0.10ng/g,定量限为0.36ng/g。用UPLC方法所得的截留效率比GC/MS分析法测定的数据稍低。
(4)研究了滤嘴截留卷烟主流烟气中氰化氢的效率。主流烟气粒相组分中的氰化氢捕集在滤片中,气相部分为氢氧化钠-乙二胺水溶液吸收。合并粒相萃取液和气相吸收液后经IC色谱分析。滤嘴也用氢氧化钠-乙二胺作为萃取液,振荡后上离子色谱分析。氰化氢线性方程为：y=8.7433x+1.4891,相关系数为0.9992,其检测限为0.05μg/mL,定量限为0.17μg/mL。滤嘴截留氰化氢的效率为9.0%～20.3%。该方法具有分析速度快、定量准确可靠,重现性好的优点。
The mainstream cigarette smoke is very complex; including many harmful components. Due to the selectively filter some harmful components in the mainstream cigarette smoke by the cigarette filter, the research on the filtration efficiencies of cigarette filters is a important aspect of the less harmful and lower tar cigarette. This paper mainly studies the filtration efficiencies of cigarette filters for low molecular aldehydes and ketones, Benzo (a) Pyrene of Polycyclic Aromatic Hydrocarbons and hydrogen cyanide. Filtration effieiencies of these components in cigarette filters by different filters and smoking style are studied.to giving a scientific basis and technological support of the selection of filter. The study results as follow:
(1)The filtration efficiencies of cigarette filters for low molecular aldehydes and ketones was detected by high performance liquid chromatography. The cigarette smoke was collected using a Cambridge pad and treated with acidic solution of2,4-dinitrophenylhydrazine. The eight low molecular aldehydes and ketones were extracted from the Cambridge filter with2%pyridine acetonitrile solution, the samples were analysed by high performance liquid chromatography and after shaked. The cigarette filtes were extracted by DNPH-method. The result shows that:The recovery tapped in different filters ranged from85.7%to92.4%with relative standard deviations (RSD) of less than5.74%and the detection limits range from0.06μg/cig to0.15μg/cig while the Limit of quantification of eight compounds range from0.20μg/cig to0.51μg/cig. This method is accurate, stable and with good reproducibility, high feasibility.
(2)The efficiencies of the Benzo (a) Pyrene of mainstream cigarette trapped in cigarette filters were analyzed by gas chromatography/mass spectrometry (GC/MS). The Pretreatment method of the filters was the same as the Cambridge pad. All samples were extracted ultrasonically with internal-standard added cyclohexane, purified by solid-phase extract culoum and condensed to0.5mL, transfered to bottle then analyzing by GC/MS. The Linear Equation of Benzo (a) Pyrene is:y=1.197e+003x-7.340e+003and correlation coefficient is0.9999, the limit of detection and the limit of quantification is0.9ng/mL,3.0ng/mL respectively. The results showed that:The filtration efficiencies of cigarette filters ranged from18.3%to45.8%.
(3)The filtration efficiencies of cigarette filters for the Benzo (a) Pyrene in mainstream cigarette smoke were analyzed by ultra-high performance liquid chromatography. The Cambridge pad and the filter's treatment were the same at the same time:extracted ultrasonically by cyclohexane, the extraction was dry up and resolved by acetonitrile then analyzed by ultra-high performance liquid chromatography instrument, the interception efficiency of filters for different filters and smoking regime whose influencing factors were studied. The linear equation of Benzo (a) Pyrene is:y=1.9479x+39800and correlation coefficient is0.9999, the limit of detection and the limit of quantification is0.10ng/g,0.36ng/mL respectively. The results determinded by UPLC were lower than by GC-MS.
(4)The efficiencies of the hydrogen cyanide of mainstream cigarette trapped in ciga rette filters were studied. The hydrogen cyanide in particle part was trapped in Cambrid-ge pad and the gas part was absorbed by Ethylenediamine-Oxyhydrogen sodium solu-tion. quantitative transferred5mL extraction and absorb liquid from particle part and gas part respectively to mix then analyzed by Ion chromatography instrument.The filters were also extracted by Ethylenediamine-Oxyhydrogen sodium solution, then analyzed by Ion chromatography instrument after shaked. The linear equation of hydrogen cyanide is:y=8.7433x+1.4891and correlation coefficient is0.9992, the limit of detection and the limit of quantification is0.05ng/mL and0.17ng/mL respectively.This method has the advantages including rapid analysis, high accuracy, good reproductivity.
(1)利用高效液相色谱检测法研究了滤嘴对卷烟主流烟气中低分子醛酮化合物的截留效率。主流烟气用加有2,4-二硝基苯肼(DNPH)的剑桥滤片捕集,采用2%(V/V)吡啶-乙腈作为萃取剂,振荡后上样。滤嘴用DNPH-甲醇溶液作萃取剂,振荡后取萃取液经滤膜过滤,用高效液相色谱分析。结果表明：甲醛、乙醛、丙酮、丙烯醛、丙醛、巴豆醛、2-丁酮及丁醛检出限为0.06～0.15μg/cig,定量限为0.20-0.51μg/cig;回收率为85.7%～92.4%,相对标准偏差为1.79%～5.74%。滤嘴截留低分子醛酮化合物的效率在1.2%～27.4%之间。该方法定量准确可靠,重现性好,可行性高。
(2)用GC/MS分析了滤嘴截留卷烟主流烟气中苯并[a]芘的效率。滤嘴和滤片处理方法一致：用加有内标的环己烷作为萃取液,超声萃取后过固相萃取柱,经洗脱、纯化和收集后旋转蒸发,浓缩至约0.5mL,转移至色谱瓶中,待GC/MS分析。苯并[a]芘的线性方程为：y=1.197e+003x-7.340e+003,相关系数为0.9999,检出限和定量限分别为0.9ng/mL、3.0ng/mL。结果显示,滤嘴截留苯并[a]芘的效率为18.3%～45.8%。
(3)采用超高效液相色谱(UPLC)的方法分析滤嘴对主流烟气中苯并[a]芘的截留效率。滤嘴和滤片采用同样方法同时处理：用环己烷作为萃取液,超声萃取,萃取液旋转蒸发至干,残渣用乙腈溶解后上样。抽吸不同的滤嘴的卷烟及在不同的抽吸方式下得出滤嘴截留效率的范围。苯并[a]芘线性方程为：y=1.9479x+39800,相关系数为0.9999。苯并[a]芘的最低检测限为0.10ng/g,定量限为0.36ng/g。用UPLC方法所得的截留效率比GC/MS分析法测定的数据稍低。
(4)研究了滤嘴截留卷烟主流烟气中氰化氢的效率。主流烟气粒相组分中的氰化氢捕集在滤片中,气相部分为氢氧化钠-乙二胺水溶液吸收。合并粒相萃取液和气相吸收液后经IC色谱分析。滤嘴也用氢氧化钠-乙二胺作为萃取液,振荡后上离子色谱分析。氰化氢线性方程为：y=8.7433x+1.4891,相关系数为0.9992,其检测限为0.05μg/mL,定量限为0.17μg/mL。滤嘴截留氰化氢的效率为9.0%～20.3%。该方法具有分析速度快、定量准确可靠,重现性好的优点。
The mainstream cigarette smoke is very complex; including many harmful components. Due to the selectively filter some harmful components in the mainstream cigarette smoke by the cigarette filter, the research on the filtration efficiencies of cigarette filters is a important aspect of the less harmful and lower tar cigarette. This paper mainly studies the filtration efficiencies of cigarette filters for low molecular aldehydes and ketones, Benzo (a) Pyrene of Polycyclic Aromatic Hydrocarbons and hydrogen cyanide. Filtration effieiencies of these components in cigarette filters by different filters and smoking style are studied.to giving a scientific basis and technological support of the selection of filter. The study results as follow:
(1)The filtration efficiencies of cigarette filters for low molecular aldehydes and ketones was detected by high performance liquid chromatography. The cigarette smoke was collected using a Cambridge pad and treated with acidic solution of2,4-dinitrophenylhydrazine. The eight low molecular aldehydes and ketones were extracted from the Cambridge filter with2%pyridine acetonitrile solution, the samples were analysed by high performance liquid chromatography and after shaked. The cigarette filtes were extracted by DNPH-method. The result shows that:The recovery tapped in different filters ranged from85.7%to92.4%with relative standard deviations (RSD) of less than5.74%and the detection limits range from0.06μg/cig to0.15μg/cig while the Limit of quantification of eight compounds range from0.20μg/cig to0.51μg/cig. This method is accurate, stable and with good reproducibility, high feasibility.
(2)The efficiencies of the Benzo (a) Pyrene of mainstream cigarette trapped in cigarette filters were analyzed by gas chromatography/mass spectrometry (GC/MS). The Pretreatment method of the filters was the same as the Cambridge pad. All samples were extracted ultrasonically with internal-standard added cyclohexane, purified by solid-phase extract culoum and condensed to0.5mL, transfered to bottle then analyzing by GC/MS. The Linear Equation of Benzo (a) Pyrene is:y=1.197e+003x-7.340e+003and correlation coefficient is0.9999, the limit of detection and the limit of quantification is0.9ng/mL,3.0ng/mL respectively. The results showed that:The filtration efficiencies of cigarette filters ranged from18.3%to45.8%.
(3)The filtration efficiencies of cigarette filters for the Benzo (a) Pyrene in mainstream cigarette smoke were analyzed by ultra-high performance liquid chromatography. The Cambridge pad and the filter's treatment were the same at the same time:extracted ultrasonically by cyclohexane, the extraction was dry up and resolved by acetonitrile then analyzed by ultra-high performance liquid chromatography instrument, the interception efficiency of filters for different filters and smoking regime whose influencing factors were studied. The linear equation of Benzo (a) Pyrene is:y=1.9479x+39800and correlation coefficient is0.9999, the limit of detection and the limit of quantification is0.10ng/g,0.36ng/mL respectively. The results determinded by UPLC were lower than by GC-MS.
(4)The efficiencies of the hydrogen cyanide of mainstream cigarette trapped in ciga rette filters were studied. The hydrogen cyanide in particle part was trapped in Cambrid-ge pad and the gas part was absorbed by Ethylenediamine-Oxyhydrogen sodium solu-tion. quantitative transferred5mL extraction and absorb liquid from particle part and gas part respectively to mix then analyzed by Ion chromatography instrument.The filters were also extracted by Ethylenediamine-Oxyhydrogen sodium solution, then analyzed by Ion chromatography instrument after shaked. The linear equation of hydrogen cyanide is:y=8.7433x+1.4891and correlation coefficient is0.9992, the limit of detection and the limit of quantification is0.05ng/mL and0.17ng/mL respectively.This method has the advantages including rapid analysis, high accuracy, good reproductivity.
引文
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