在线裂解气相色谱/质谱联用法研究4-氧代-β-大马酮的热裂解行为  

Investigation of the Pyrolysis Behavior of 4-Oxo-β-Damascone by On-Line Pyrolysis Gas Chromatography-Mass Spectrometry

作　　者：吴亿勤[1] 杨柳 刘芳[1] 缪明明 朱洪友[1] 冒德寿[1] 

机构地区：[1]云南大学化学科学与工程学院,云南昆明650091 [2]红塔烟草(集团)有限责任公司技术中心,云南玉溪653100

出　　处：《色谱》2007年第3期408-412,共5页Chinese Journal of Chromatography

摘　　要：用在线裂解气相色谱/质谱法(PyGC/M S)研究了4-氧代-β-大马酮的热裂解行为。在氦气氛围中,将4-氧代-β-大马酮分别在350,450,550,650,700和750℃下进行热裂解,并以GC/M S对其裂解产物进行定性和半定量分析。结果表明,不同的裂解温度直接影响生成产物的类型和相对含量。4-氧代-β-大马酮可裂解出β-大马酮、4-氧代-β-紫罗兰酮、3,4,4-三甲基-环己-2-烯-1-酮和2,5,5-三甲基-环己-3-烯-1-酮等54种裂解产物。在550℃以下时,只有少量4-氧代-β-大马酮发生裂解;在750℃时,几乎完全裂解,转移率达99.74%,裂解产物达45种之多。随着裂解温度的升高,裂解产物越来越复杂,并出现有害物质如苯、甲苯、蒽和菲等。根据4-氧代-β-大马酮裂解产物相对含量的变化规律,对其裂解产物的形成机理进行了探讨,认为4-氧代-β-大马酮可能按照4种途径发生裂解。The pyrolysis behavior of an essence, 4-oxo-β-damascone, was investigated using an on-line pyrolysis gas chromatography-mass spectrometry （PyGC/MS）. In helium atmosphere, the compound was pyrolyzed at 350, 450, 550, 650, 700, and 750 ℃, separately. The pyrolysis products were directly introduced into GC/MS with 1. 03 × 10^6 Pa He and were qualitatively and semi-quantitatively analyzed. At the six pyrolysis temperatures mentioned above, 3, 7, 15, 33, 42 and 45 products were detected and their relative contents were 96.25%, 85.44%, 87.18%, 78.37%, 78.29% and 83.13%, respectively. The results indicated that the pyrolysis temperature directly affected the pyrolysis pattern and the relative content of the products. A total of 54 products were identified, including β-damascone, 4-oxo-β-ionone, 3,4,4-trimethyl-2-cyclohexen-1-one and 2,5,5-trimethyl-cyclohex-3-en-l-one. At 550℃, only a small portion of the parent compound was pyrolyzed. At 750 ℃, the compound was completely pyrolyzed, with a conversion of 99.74% and 45 products were given. Moreover, with the elevation of the pyrolysis temperature, complex pyrolysis products were formed, and harmful substances, such as benzene, toluene, anthracene and phenanthrene were identified. According to the relative content and the category of the pyrolysis products, the pyrolysis mechanism of 4-oxo-β-damascone is further discussed with the conclusion that the pyrolysis of this compound might take place via 4 different pathways. The investigation gave an exemplification for the transfer behavior of tobacco essence in the cigarette burning process, and provided a reliable theoretical foundation for the perfume reinforcement technology in tobacco products, contributing to the development of cigarette products with better aroma and taste.

关 键 词：裂解气相色谱/质谱 4-氧代-β-大马酮 热裂解行为 烟草添加剂 

分 类 号：O658[理学—分析化学]