抽吸方式对卷烟主流烟气氨释放量的影响

为考察抽吸方式对卷烟主流烟气中氨释放量的影响,采用ISO、Massachusetts和Health Canada 3种抽吸方案分别抽吸了15种国产卷烟,然后采用离子色谱法测定了这些卷烟主流烟气中氨的释放量.结果表明:①对于滤嘴打孔卷烟,与ISO抽吸方案相比,采用Massachusetts抽吸方案,混合型卷烟主流烟气中氨...     

两种抽吸模式下卷烟主流烟气中主要酚类的释放量比较

为了解不同抽吸方式对卷烟主流烟气中主要酚类化合物释放量的影响,建立了一种利用超高效液相色谱(UPLC)快速分析卷烟主流烟气中邻-苯二酚、对-苯二酚、间-苯二酚、苯酚、邻-甲酚、间+对-甲酚的方法,并采用该方法测定了ISO模式和加拿大卫生部(Health Canada)深度抽吸模式下38个卷烟样品烟气中这7种主要酚类的释放量。结果表明:①方法检测限为16～43 ng/支,回收率94%～102%,RSD4%;②与ISO抽吸模式相比,在HC深度抽吸模式条件下卷烟主流烟气中主要酚类化合物释放量显著提高。     

抽吸方式对卷烟主流烟气中氢氰酸释放量的影响

为考察不同抽吸方式对卷烟主流烟气中氢氰酸(HCN)释放量的影响,采用ISO、Massachusetts和Health Canada 3种抽吸方式分别抽吸了15种市售卷烟,采用连续流动法测定了主流烟气中的HCN释放量.研究表明:与ISO方案相比,采用Massachusetts或Health Canada深度抽吸方式,HCN释放量均有显著提高;抽吸方式的改变对低焦油卷烟、高滤嘴通风率的卷烟的HCN释放量影响更为显著.     

抽吸方式对卷烟主流烟气烟草特有亚硝胺释放量的影响

为考察抽吸方式对卷烟主流烟气中烟草特有N-亚硝胺(TSNAs)释放量的影响,采用ISO、Massachusetts和Health Canada 3种抽吸方案分别抽吸了15种国产卷烟,而后采用GC/TEA法测定了这些卷烟主流烟气粒相物中的NNN、NAT、NAB、NNK释放量.结果表明:与ISO方案相比,采用Massachusetts方案(50%封闭滤嘴通风孔)或Canada深度抽吸方案(100%封闭滤嘴通风孔),滤嘴打孔卷烟烟气TSNAs总释放量增加100%以上,高通风率卷烟样品的增幅达200%以上;滤嘴不打孔卷烟烟气TSNAs总释放量增加50%左右.     

离子色谱法测定卷烟主流烟气中氨含量的方法改进

为准确测定主流烟气中的氨含量,对离子色谱(IC)测定方法进行了改进,并采用该方法测定了59种卷烟在ISO和加拿大卫生部(Health Canada,HC)深度抽吸条件下主流烟气中的氨含量.结果表明:①烟气样品经捕集、萃取和石墨化炭黑柱(GCB)净化后,以甲基磺酸(MSA)为淋洗液,采用CS16阳离子交换柱分离.②在0～1 μg/mL范围内,线性相关系数为0.9992,方法检出限为0.0067 μg/mL,相对标准偏差为2.8％ ～ 4.5％,回收率为96％ ～ 104％.③HC深度抽吸条件下卷烟主流烟气中NH4+含量是ISO抽吸条件下的173％ ～ 378％.改进后的测定方法较好地解决了样品溶液不稳定、色谱系统易被污染的问题.     

冷阱捕集-气相色谱-质谱法测定卷烟主流烟气中的呋喃

建立了测定卷烟主流烟气中呋喃的冷阱捕集-气相色谱-质谱(GC/MS)法。主流烟气中的呋喃用含有氘代内标(呋喃-d4)的冷甲醇吸收后在选择离子监测模式下进行GC/MS 分析;考察了11 个不同品牌卷烟在ISO 抽吸模式与加拿大深度抽吸模式下主流烟气呋喃的释放量。结果表明:方法的线性相关系数为0.999 7,检出限为0.028 μg/mL,加标回收率和相对标准偏差(RSD)分别为94.2%~98.5%和3.3%~4.6%。加拿大深度抽吸模式下卷烟主流烟气中呋喃的释放量为ISO 抽吸模式下的两倍以上,ISO抽吸模式下卷烟主流烟气呋喃释放量与实测焦油量显著线性相关。该方法适用于测定卷烟主流烟气中呋喃的释放量。      

卷烟烟气中烟草特有亚硝胺的滤嘴截留效率测定

为考察烟草特有亚硝胺(TSNAs)的滤嘴截留效率(FE),建立了采用GC-TEA测定卷烟滤嘴中TSNAs截留量的方法,并采用该方法测定了同一醋纤滤嘴卷烟样品在ISO,Massachusetts,WG9-A,WG9-B,WG9-C和Health Canada 6种抽吸方案下的FEs,以及在ISO方案下醋酸纤维滤嘴、聚丙烯纤维滤嘴和活性炭+醋酸纤维复合滤嘴的FEs。结果表明:①不同类型滤嘴中截留的TSNAs的回收率均在90%～110%之间,相对标准偏差(RSD)均小于8%;②随着抽吸方案由ISO转变为其他抽吸方案,主流烟气TSNAs释放量和滤嘴截留量增加,而4种TSNAs的滤嘴截留效率则相对稳定,RSD均5%;③3种不同类型的滤嘴对TSNAs的截留效率比较接近。     

两种抽吸模式对卷烟主流烟气测量方法与结果精密度的影响

为了解吸烟机抽吸模式对卷烟主流烟气相关测量方法与结果精密度的影响,针对卷烟主流烟气的常规指标(抽吸口数、总粒相物、焦油、烟碱、CO)、烟草特有亚硝胺[TSNAs,N-亚硝基降烟碱(NNN)、4-(N-甲基-N-亚硝氨基)-1-(3-吡啶基)-1-丁酮(NNK)]、苯并[a]芘、羰基化合物(甲醛、乙醛、丙烯醛、巴豆醛)、苯酚、氢氰酸、氨、挥发性有机化合物(VOCs,1,3-丁二烯、苯)等17个测试指标,在ISO和加拿大深度抽吸(HCI)两种模式下开展了卷烟主流烟气系列测量方法的协同试验,按照GB/T 6379.2—2004/ISO 5725-2:1994的统计方法进行分析,获得了9个测量方法 6个测试水平(m)下的重复性限(r)和再现性限(R),并确立了r、R与m的线性拟合函数关系。结果表明:焦油、烟碱、CO的测量精密度显著优于其他测试指标,相对重复性限(r%)和相对再现性限(R%)分别约为10%和20%,其他指标的r%和R%分别为20%和45%左右;与ISO抽吸模式相比,HCI抽吸模式下卷烟主流烟气释放量显著增加,但测量方法的精密度对于绝大多数测量指标并没有明显改善;HCI抽吸模式下相关测试指标的精密度对m的依赖性显著较弱,部分指标的两种吸烟机型测试结果差异较大;烟气在HCI抽吸模式下的捕集过程中,吸烟机卷烟抽吸参数(如抽吸口数)稳定性相对较差。因此,当前典型的吸烟机设计并不能较好地满足深度抽吸条件下卷烟主流烟气相关分析物的稳健测量。     

卷烟主流烟气中氨测定方法的改进及不同抽吸模式下的氨释放量比较

为了提高卷烟主流烟气中氨(NH3)的测定效率,对现行标准YC/T 377—2010的离子色谱(IC)测定方法进行了改进,并考察了ISO和加拿大深度抽吸(HC)模式下卷烟主流烟气中NH3释放量变化。结果表明:①采用Ion Pac CS16分析柱、等度洗脱、0.60 mL/min流速和50 mmol/L甲烷磺酸(MSA)淋洗液,15 min内即可完成单个卷烟样品中NH3的测定;②NH3的加标回收率为97.53%～99.13%,相对平均标准偏差(RSD)<5%;③HC模式下主流烟气中NH3含量明显高于ISO抽吸模式下的含量。     

不同抽吸模式卷烟主流烟气中常规成分和某些有害成分释放研究

对比研究了ISO抽吸模式和加拿大深度抽吸模式下不同卷烟主流烟气中焦油、烟碱和水分3种常规成分释放量及一氧化碳、氨和苯酚3种有害成分释放量。结果表明, 加拿大深度抽吸模式下, 卷烟主流烟气中焦油、烟碱和水分3种常规成分及一氧化碳、氨和苯酚3种有害成分释放量远远高于ISO抽吸模式下的释放量;随着滤嘴通风率的增加, 主流烟气常规成分和某些有害成分释放量的增加幅度越来越大;主流烟气中水分释放量的增加幅度远远大于焦油、烟碱、一氧化碳、氨和苯酚释放量的增加幅度。     

两种抽吸模式下吸烟机型对卷烟主流烟气总粒相物及7种化学成分检测结果的影响

为研究不同抽吸模式下吸烟机型对卷烟主流烟气总粒相物(TPM)和7种化学成分释放量检测结果的影响,以典型的不同焦油量(1.0~13.3 mg/支)的9种烤烟型和11种混合型卷烟样品为研究对象,考察了ISO和加拿大深度抽吸(HCI)模式下直线型(L)和转盘型(R)吸烟机对卷烟主流烟气总粒相物(TPM)和一氧化碳(CO)、4-(N-甲基-N-亚硝氨基)-1-(3-吡啶基)-1-丁酮(NNK)、苯并[a]芘(B[a]P)、巴豆醛、苯酚、氰化氢(HCN)、氨(NH₃)释放量测试结果的影响。结果表明:①HCI抽吸模式下两种吸烟机型测试结果的一致性弱于ISO抽吸模式; TPM、巴豆醛和HCN在HCI抽吸模式下两种吸烟机型测试结果的差异明显。②两种抽吸模式下卷烟主流烟气NNK、B[a]P和苯酚重复检测结果标准偏差(SD,n=5)与检测水平均值(m)的相关性总体上较CO、巴豆醛、HCN和NH₃高,但HCI抽吸模式下检测结果SD与检测水平m的相关性弱于ISO抽吸模式。③在两种抽吸模式下,卷烟主流烟气相关指标不同吸烟机型测试结果总体精密度差异基本一致,即R型吸烟机对于20个不同烟气释放量水平样品重复测试结果的平均变异系数(CV)大多低于L型。      

Analysis of hydrogen peroxide in cigarette smoke from selected Chinese cigarette brands under conventional and intense machine smoking conditions

The purpose of the present work was to investigate the concentration ranges of H₂O₂ generated from cigarette smoke of selected Chinese brands and the effect of different smoking behaviors on the deliveries of H₂O₂. A simple, rapid and reliable fluorescence assay was developed for the measurement of H₂O₂ based on the catalytic activity of hemoglobin using 10-acetyl-3, 7-dihydroxyphenoxazine (Amplex Red) as the substrate. The proposed method was applied to determine the H₂O₂ deliveries from mainstream cigarette smoke of 30 Chinese (5 blended and 25 Virginia) and two reference cigarettes (3R4F and 1R5F) under two machine smoking regimes. Results showed that, under ISO smoking conditions, Chinese blended cigarettes had lower H₂O₂ yields than Chinese flue-cured cigarettes (mean value 2.41 vs. 4.69?μg?cig^?1, p?<?0.05). As expected, the deliveries of H₂O₂ for all cigarettes analyzed were higher under Canadian intense smoking conditions than those under ISO conditions (ISO mean 4.31?μg?cig^?1 vs. Canadian mean 5.96?μg?cig^?1, p?<?0.05). In addition, the ratios of H₂O₂ to nicotine yields were utilized to show the relative differences in yields among brands tested in this work and more than a twofold difference was found for most of selected Chinese blended and flue-cured cigarettes.     

Revising the machine smoking regime for cigarette emissions: implications for tobacco control policy

Background

The WHO Framework Convenion on Tobacco Control includes provisions for testing and regulating cigarette emissions. However, the current international standard for generating cigarette emissions—the ISO machine smoking regime—is widely acknowledged to be inappropriate for purposes of setting regulatory restrictions.

Objective

To review alternatives to the ISO machine smoking regime and the extent to which they: 1) Represent human smoking behaviour, 2) Reduce the potential for industry exploitation, particularly in the area of risk communication, and 3) Serve as suitable measures for product regulation.

Methods

Emissions data from 238 Canadian cigarette brands tested under the ISO and “Canadian Intense” machine smoking regimes.

Results

None of the alternative smoking regimes, including the Canadian Intense method, are more “representative” of human smoking behaviour and none provide better predictors of human exposure.

Conclusions

Given that alternatives such as the Canadian Intense regime are subject to the same fundamental limitations as the ISO regime, key questions need to be addressed before any smoking regime should be used to set regulatory limits on smoke emissions. In the meantime, regulators should remove quantitative emission values from cigarette packages and more work should be done on alternative machine smoking methods.The issue of how to test and regulate conventional cigarettes represents a critical challenge for tobacco control. To date, the primary means of testing cigarette toxicity has been to machine smoke the cigarettes according to a standard puffing regime and to measure the chemical emissions in the mainstream smoke. In many jurisdictions, these cigarette “yields” are printed on packages and represent the only source of information on constituents or toxicity available to consumers. Cigarette emissions also serve as a regulatory standard in several of jurisdictions, including the European Union, where brands that generate emissions >10 mg of tar, 1 mg of nicotine or 10 ppm of carbon monoxide are prohibited. The puffing regime used to machine smoke the cigarettes—the International Organization for Standardization (ISO) regime¹—is widely recognised to be inadequate for the purposes of product regulation or consumer information. The ISO regime constitutes a set of puffing parameters that systematically underestimate smoking behaviour in humans.^2,3,4 Tobacco manufacturers have also designed cigarette brands to perform one way under the machine smoking conditions, but to deliver much greater smoke constituents to humans.^5,6 As a result, the emissions generated under the ISO smoking regime have little relationship with actual measures of human exposure, and exaggerate the differences between brands in a manner that has proved deceptive to both consumers and regulators.^7,8,9 Overall, the emissions from the ISO regime have served as more of an industry marketing tool to falsely reassure health‐concerned smokers, rather than as a valid measure of cigarette toxicity.^2,10,11,12There is a growing movement to develop a more meaningful machine testing method. The World Health Organization''s Framework Convention on Tobacco Control (FCTC)—the world''s first international public health treaty—includes provisions for testing and regulating cigarette emissions under Article 9.¹³ These provisions will need to be specified now that the FCTC has come into force. After discussions with the WHO, the ISO convened a working group (ISO TC 126 WG9) to develop recommendations for “…a robust and practical smoking regime that as far as possible is representative of smokers'' behaviour”. Meanwhile, the World Health Organization''s Study Group on Tobacco Product Regulations (WHO TobReg) has developed its own set of recommendations, which were under consideration by the ISO Working Group.¹⁴ There are also concerns that the ISO committee structure responsible for setting tobacco standards is dominated by the tobacco industry.¹²Before any new testing regime is implemented, it is critical to ensure that the new standards will serve the interests of public health rather than the tobacco industry. The purpose of this paper is to review the smoking regimes that are under consideration by the ISO Working Group, and to examine the implications for tobacco control policy and product regulation. In particular, we examine the extent to which the proposed regimes will: (1) succeed in “representing” smoking behaviour in humans and generate better predictors of human exposure; (2) reduce the potential for industry exploitation, particularly in the field of risk communication; and (3) help to establish more effective regulatory limits on cigarette toxicity.     

婴幼儿配方乳粉中维生素A、E检测方法的比较研究

目的 以国家标准GB5009.82-2016第一法(GB方法)和AOAC 2012.10/ ISO20633:2015 (AOAC/ISO方法)为例,通过文本分析和实验数据比较反相液相色谱法(RF-HPLC)和正向液相色谱法(NP-HPLC)检测婴幼儿配方粉中维生素A和维生素E的差异,分析可能导致方法结果产生差异的原因,提出科学建议。方法 通过标准方法文本原理比对,分析两种方法的原理及技术步骤差异;通过质控样检测,分析两组结果的标准偏差、变异系数、95%重复性限、相对重复性限值、平均值、回收率等指标,比对两种方法的精密度和准确度差异;通过市售样品检测,分析两种方法检测结果的系统偏差和比例偏差,判别两种方法对婴幼儿配方乳粉的结果一致性。结果 从方法文本上看,AOAC/ISO方法较 GB方法的步骤更为简便,且标明了方法的适用浓度范围、重复性、重现性等关键指标,标注的检出限及定量限值也较GB方法更低;精密度方面,采用AOAC/ISO方法测得的重复性和重现性标准偏差、变异系数、95%重复性限、相对重复性限值结果,均低于GB方法测得的同类指标。准确度方面,AOAC/ISO方法和GB方法测定维生素AE时均表现出较好的回收率(100±5%);样品对比检测结果表明,维生素A两种方法的检测结果不存在系统偏差和比例偏差,结果一致;维生素E两种方法的结果既有系统偏差也有比例偏差,结果不一致。结论 AOAC/ISO 方法和GB方法原理及操作步骤存在明显不同,可能导致两种方法在测定维生素E含量时,结果呈现统计学显著差异。建议加强国内外检测标准的沟通协调,在检测目标物,样品称量方式,样品适用浓度范围等方面做进一步改进和完善。     

ISO 12863卷烟引燃倾向标准评价方法的改进

为解决ISO 12863标准方法测试成本高、测试效率低的问题,结合样品抽样方案设计和统计学算法建立了一种测试支数动态调节的卷烟引燃倾向评价方法,并通过全长燃烧百分比（P-FLB）的二项分布计算分析了该指标偏差较大的原因。结果表明:①本文方法与ISO标准方法的准确性和重复性基本一致。②P-FLB仅是测定结果置信区间中置信度最高的一点,但其置信度仍然较低,导致理论上可产生10%~20%的最大偏差。③当全燃支数较少时（0~4支）,ISO方法更稳定,当全燃支数较多时（5~10支）,本文方法更稳定,当全燃支数超过6支时,卷烟产品的防火安全性能存在潜在风险。④80个LIP样品测试结果显示,与ISO方法相比,本文方法的平均检测时间和专用滤纸使用量均下降了59.65%,取得了较好的节支效果,提高了检测效率。