河南农业大学烟草学院
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Pyrolysis Analysis on New Latent Fragrant N-(2,3-Pyrazinediformyl) Alanine Methyl Ester by Gas Chromatography-Mass Spectrometry. [J]. 33(8):887-892(2014)
采用在线热裂解-气相色谱-质谱联用技术(Py-GC-MS)分析了潜香吡嗪类化合物N-(2,3-吡嗪二甲酰基)-丙氨酸甲酯的热裂解行为。首先通过对2,3-吡嗪二羧酸酰胺化反应合成了新型目标化合物N-(2,3-吡嗪二甲酰基) 丙氨酸甲酯,其结构经X射线单晶衍射(XRD),1H NMR,13C NMR,IR和HR-MS证实,然后在空气氛围中,对目标化合物分别在300,600,900 ℃下进行热裂解,并通过GC-MS对其挥发性热裂解产物进行定性和半定量分析。结果表明:①裂解形成了包括具有香味特征的吡嗪类、大茴香醇和大茴香醛在内的裂解产物共48种。不同温度下挥发性热裂解产物的类型和相对含量不同,300 ℃和600 ℃时相对含量最高的均为乙酸,而900 ℃时相对含量最高的为吡嗪,且与300 ℃和600 ℃裂解条件相比所形成的吡嗪类衍生物种类较多,相对含量较高。②在具有香味特征的裂解产物中,大茴香醇的相对含量随温度升高而升高,而大茴香醛和苯甲醛的相对含量则呈现随着温度升高而降低的趋势。基于目标化合物的热裂解产物的定性及定量变化情况,初步探讨了该物质可能的裂解机理。
The pyrolysis behavior of latent fragrant compound N-(2,3-pyrazinediformyl) alanine methyl ester was investigated by on-line pyrolysis-gas chromatography-mass spectrometry(Py-GC-MS).Firstly,the new compound N-(2,3-pyrazinediformyl) alanine methyl ester was synthesized by amidation using 2,3-pyrazinedicarboxylic acid as material,and its structure was confirmed by X-ray single crystal diffractometry(XRD),1H NMR,13C NMR,IR and HR-MS.In air atmosphere,the compound was pyrolyzed at 300,600 and 900 ℃,respectively.The pyrolysis products were directly introduced into GC-MS to analyse qualitatively and semi-quantitatively.The results indicated that 48 pyrolysis products were detected,including the flavorous substances such as pyrazines,4-methoxy-benzenemethanol and 4-methoxy-benzaldehyde.The pyrolysis temperature affected the pyrolysis pattern and the relative content of the products.The relative content of acetic acid was the highest at 300 ℃ and 600 ℃,and that of pyrazine was the highest at 900 ℃.Compared with that of the pyrolysis at 300 and 600 ℃,the generated pyrazine derivatives sort and the relative content of pyrazine were the highest when pyrolyzing at 900 ℃.On the other hand,in the pyrolysis products with aroma characteristics,the relative contents of 4-methoxy-benzenemethanol increased monotonically with increase of pyrolysis temperature,while the relative content of 4-methoxy-benzaldehyde and benzaldehyde showed a decreasing tendency with a rise of temperature.The possible pyrolysis mechanism of N-(2,3-pyrazinediformyl) alanine methyl ester was preliminarily discussed based on the determined pyrolysates and quantitative changes with the temperature.It is a simple and rapid way to use Py-GC-MS technology in the separation and identification of pyrolysis products.
热裂解-气相色谱-质谱潜香化合物N-(23-吡嗪二甲酰基) 丙氨酸甲酯热裂解行为
pyrolysis-gas chromatography-mass spectrometry(Py-GC-MS)latent fragrant compoundN-(23-pyrazinediformyl) alanine methyl esterpyrolysis behavior
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