烟草及烟草制品中TSNAs分析方法的对比

对目前烟草及烟草制品中烟草特有亚硝胺（TSNAs）的分离纯化和测试方法进行了综述和对比,认为使用液相色谱-质谱-质谱（LC-MS-MS）联用技术测试TSNAs是今后的发展趋势。     

烟草化学分析技术的应用及发展探讨

研究卷烟燃烧条件与烟气中化学成分构成的变化,裂解相色谱模拟分析技术是一种相当有效的手段。为促进该分析技术的发展,本文对裂解气相色谱一质谱法（PY—GC—MS）在国内烟草化学应用研究情况作系统分析总结并对其发展进行了探讨。     

基质固相分散-UPLC-MS/MS法测定吸烟者尿液中的TSNAs

研究了用基质固相分散-高效液相色谱质谱法测定吸烟者尿液中的烟草特有亚硝胺(TSNAs)。尿液样品浓缩后用碱性氧化铝分散处理,然后在带柱层析净化功能的索氏提取器中用氧化铝柱层析净化。经净化后样品中的TSNAs用UPLC-MS/MS分析。在选定条件下,四种烟草特有亚硝胺NAT、NNK、NNN和NAB的检出限分别为0.06,0.07,0.13,0.11 ng/m L,对样品进行7次测定,日内相对标准偏差为3.3%~4.9%;日间相对标准偏差为4.1%~4.9%,方法的回收率在82.3%~91.4%之间,结果令人满意。     

基质固相分散-UPLC-MS/MS法测定吸烟者尿液中的TSNAs

研究了用基质固相分散-高效液相色谱质谱法测定吸烟者尿液中的烟草特有亚硝胺(TSNAs)。尿液样品浓缩后用碱性氧化铝分散处理,然后在带柱层析净化功能的索氏提取器中用氧化铝柱层析净化。经净化后样品中的TSNAs用UPLC-MS/MS分析。在选定条件下,四种烟草特有亚硝胺NAT、NNK、NNN和NAB的检出限分别为0.06,0.07,0.13,0.11 ng/m L,对样品进行7次测定,日内相对标准偏差为3.3%⁴.9%;日间相对标准偏差为4.1%4.9%;日间相对标准偏差为4.1%⁴.9%,方法的回收率在82.3%4.9%,方法的回收率在82.3%⁹1.4%之间,结果令人满意。     

烟草中特有的亚硝胺研究进展

烟叶中烟草特有的亚硝胺（TSNAs）已成为目前世界烟草研究的重点领域之一,综述了近年来国内外有关TSNAs的研究进展,阐述了TSNAs的形成、致癌性,介绍了TSNAs检测方法,并探讨了如何降低烟叶中的TSNAs。     

气相色谱-质谱法测定牙膏中的二甘醇

利用毛细管柱气相色谱-质谱（GC—MS）测定牙膏中二甘醇的量,检出限为5mg／kg,二甘醇的线性范围为5μg／mL－500μg／mL,回收率为95．2％～102．2％,相对标准偏差（RSD）为1．19％～1．54％。     

烟用香精的全二维气相色谱-飞行时间质谱定性分析

针对在一维色谱上分离峰太少或色谱图中有明显重叠峰的烟用香精,采用全二维气相色谱-飞行时间质谱（GC×GC-TOFMS）对烟用香精进行了定性分析,优化分析条件,并与一维色谱分析结果进行比较。最后,比较了不同分析结果所得化学成分和品吸结果之间的对应关系。结果表明,GC×GC-TOFMS比一维气相色谱/质谱（GC/MS）具有更强的分离能力,可定性的组分明显多于一维GC/MS,并且更符合该香精的评吸结果。这种分析方法有利于更全面地认识香精的化学成分,更准确地认识香精的组成与功能之间的关系。为增强加香配方研究的科学性、提高调香工作的效率提供有力的支持。     

金银花浸膏挥发性成分分析

采用气相色谱-质谱分析技术（GC—MS）分析了金银花浸膏的挥发性成分,并对其相对含量进行了分析,共鉴定出67种成分,主要为亚油酸甲酯、棕榈酸、十八碳烯酸甲酯、棕榈酸甲酯、亚麻酸甲酯、芳樟醇、棕榈酸乙酯、亚油酸乙酯、亚油酸、肉豆蔻酸、亚麻酸乙酯等。     

海南油棕果肉中脂肪酸的成分分析

用乙醚萃取海南油棕果肉中的油脂,油脂中的脂肪酸采用氢氧化钾-甲醇溶液进行甲酯化后,利用气相色谱-质谱联用技术（GC—MS）对其中的脂肪酸成分进行分析。结果分离鉴定出4种脂肪酸成分,它们分别是棕榈酸（45．62％）、油酸（37．70％）、亚油酸（8．39％）、硬脂酸（8．29％）。其中不饱和脂肪酸高达46％以上,有进一步开发利用的潜力。     

气相色谱-质谱法测定聚碳酸酯树脂及其成型品中的双酚A

建立了聚碳酸酯树脂及其成型品中双酚A（BPA）的气相色谱-质谱联用（GC—MS）检测方法。样品经丙酮提取后挥发至干，用碳酸钾溶液溶解，再与乙酸酐衍生反应。衍生产物经正已烷提取后，采用GC—MS进行分析。结果表明，方法的线性范围为0．05—1．0mg／L，相关系数为0．9989，线性范围为1．0—10．0mg／L，相关系...     

卷烟主流烟气中烟草特有亚硝胺的测定

建立了一种高效液相色谱-串联质谱联用法测定卷烟主流烟气中烟草特有亚硝胺的方法。采用含10ng.mL-1内标的0.1mol.L-1乙酸铵溶液直接对收集了主流烟气的剑桥滤片进行超声萃取30min,过膜后的萃取液用带电喷雾装置的LC-MS/MS仪进行分析。该方法数据可靠、操作简单、重复性好。     

Absence of volatile N-nitrosamines in margarines

Samples of margarines, butter and vegetable oils were analyzed for volatile N-nitrosamines by the vacuum steam distillation method followed by dichloromethane extraction of the distillate and gas chromatographic-thermal energy analysis (GC-TEA) of the extracts. No volatile nitrosamines in excess of a practical limit of determination of 0.5 ppb were found in any of the samples. The problem of artifact formation during analysis of low levels of nitrosamines and the meaning of a “practical limit of determination” is briefly discussed.     

Nitrosamines Extraction from Frankfurter Sausages by using Superheated Water

An efficient, rapid, and inexpensive method for extraction and clean-up of some selected volatile nitrosamines from frankfurter sausages was developed by using superheated water coupled with solid-phase extraction. Because a coextraction of lipid caused a serious problem during the extraction, a subsequent clean-up step using fat-selective Florisil adsorbent with 60% diethyl ether-dichloromethane was then necessary. Various factors affecting superheated water extraction, such as flow rate, extraction temperature, dynamic time, and static time were optimized by using a full factorial design with three replicates. The optimal extraction temperature was 140°C with dynamic and static time of 10 and 5 min, respectively, and a flow rate of 1.0 mL/min. Separation and quantification of nitrosamines were carried out using GC-FID and GC-MS in selected ion monitoring mode. Direct application of this method to frankfurter samples allowed overall recoveries of N-nitrosamines in the range of 81-106% with < 10% RSD, and the detection limit of the coupling method ranged between 0.47-1.48 ng nitrosamines injected.     

Trapping tobacco specific N-nitrosamines in Chinese-Virginia type tobacco extracting solution by porous material

Liquid adsorption of tobacco specific nitrosamines (TSNA) in the tobacco extracting solution by porous materials is reported, with the monitoring of standard LC–MS/MS technique, in order to reduce the environmental cancerogens in smoke at the source. Three types of adsorbent, zeolite, mesoporous silica and activated carbon are utilized to trap nitrosamines in the extracting solution of Chinese-Virginia type tobacco with low TSNA content, and their performance was measured by spectrophotometric and LC–MS/MS methods. Both measurements gave the same variation tendency on the nitrosamines analysis, enabling the photometric method to be the simple and feasible tool in preliminary tests. The influence of pore size and cations of zeolite along with the organic modification of mesoporous silica with chloroisopropyl triethoxysilane were carefully investigated, and the optimal liquid conditions were determined, in which CaA zeolite and modified mesoporous silica CAM48-10 sample can capture 34 and 46 % of TSNA in the tobacco extracting solution, offering the efficient candidate for controlling the carcinogen like nitrosamines in environment.     

Selective adsorption of zeolite towards nitrosamine in organic solution

Experiments were carried out to study the adsorption of four nitrosamines (N-nitrosohexamethyleneimine (NHMI), N-nitrosopyrrolidine (NPYR), N-nitrosonornicotine (NNN) and N-nirosodiphenylamine (NDPA)) by zeolites in organic solvents. It was found that zeolites of different pore structures and hierarchy exhibited different selectivity towards the nitrosamines. The behavior was generally governed by geometric matching between the adsorbate and adsorbent: zeolites with smaller pores favored the trap of smaller nitrosamines whereas mesoporous zeolites captured more bulky nitrosamines. Nevertheless the adsorption of bulky NDPA and NNN was found to take place on type A zeolite, which has a smaller pore size than the molecular diameter of the two nitrosamines. Meanwhile, the presence of other compounds with nitro group in the system appeared to interfere with the adsorption. Among the zeolites studied, CsA and KA could distinguish the bulky nitrosamines such as N-nitrosodiphenylamine (NDPA) and nitro compounds (nitrobenzene). The influence of the solvent on the adsorption was also studied.     

烟草特有亚硝胺降解技术研究进展

香烟在燃烧期间，烟草中的亚硝胺一部分可能转移进入烟气中，另一部分可能发生降解。本文综述了近几十年来国内外有关烟气中烟草特有亚硝胺的研究进展，阐述了烟气中特有亚硝胺的形成、危害及影响因素，介绍了各种亚硝胺的降解技术和方法。     

Bildung und Nachweis von Nitrosaminen in Lebensmitteln —ein kurzer Überblick

Formation and Analysis of Nitrosamines in Food Products —a Brief Review A brief review has been prepared to illustrate a number of current problems. The formation of nitrosamines in food products and the analysis of volatile nitrosamines in the ppb range and problems of the analysis of non-volatile nitrosamines are briefly discussed.     

Electronic cigarette-generated aldehydes: The contribution of e-liquid components to their formation and the use of urinary aldehyde metabolites as biomarkers of exposure

Electronic cigarettes (e-cigarette) have emerged as a popular electronic nicotine delivery system (ENDS) in the last decade. Despite the absence of combustion products and toxins such as carbon monoxide (CO) and tobacco-specific nitrosamines (TSNA), carbonyls including short-chain, toxic aldehydes have been detected in e-cigarette-derived aerosols up to levels found in tobacco smoke. Given the health concerns regarding exposures to toxic aldehydes, understanding both aldehyde generation in e-cigarette and e-cigarette exposure is critical. Thus, we measured aldehydes generated in aerosols derived from propylene glycol (PG): vegetable glycerin (VG) mixtures and from commercial e-liquids with flavorants using a state-of-the-art carbonyl trap and mass spectrometry. To track e-cigarette exposure in mice, we measured urinary metabolites of 4 aldehydes using ULPC-MS/MS or GC-MS. Aldehyde levels, regardless of abundance (saturated: formaldehyde, acetaldehyde???unsaturated: acrolein, crotonaldehyde), were dependent on the PG:VG ratio and the presence of flavorants. The metabolites of 3 aldehydes – formate, acetate, and 3-hydroxypropyl mercapturic acid (3-HPMA; acrolein metabolite) – were increased in urine after e-cigarette aerosol and mainstream cigarette smoke (MCS) exposures, but the crotonaldehyde metabolite (3-hydroxy-1-methylpropylmercapturic acid, HPMMA) was increased only after MCS exposure. Interestingly, exposure to menthol-flavored e-cigarette aerosol increased the levels of urinary 3-HPMA and sum of nicotine exposure (nicotine, cotinine, trans-3′-hydroxycotinine) relative to exposure to a Classic Tobacco-flavored e-cigarette aerosol. Comparing these findings with aerosols of other ENDS and by measuring aldehyde-derived metabolites in human urine following exposure to e-cigarette aerosols will further our understanding of the relationship between ENDS use, aldehyde exposure, and health risk.

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