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绿原酸的梯度热裂解分析

Gradient Pyrolysis of Chlorogenic Acid

  • 摘要: 为准确了解绿原酸的裂解过程,测定了绿原酸的热失重特性,并根据绿原酸的热重曲线和裂解特性将其裂解历程分为10个温度段,采用GC/MS法测定了这10个梯度温度段绿原酸的热裂解产物。结果表明:①绿原酸的热失重至少可分为6个温度段,各阶段的热失重分别为2.94%,0.61%,8.55%,20.29%,34.32%和9.43%;②绿原酸在10个温度段的热裂解产物为:30~120℃,裂解产物是水;120~190℃,没有裂解产物产生;190~260℃,裂解产物是水、二氧化碳和奎宁内酯类化合物;260~325℃,裂解产物是二氧化碳、苯酚、儿茶酚、对苯二酚和奎宁内酯类化合物、水;325~400℃,与260~325℃相比,新裂解产生了3-羟基苯甲酸、苯甲酸、4-乙基儿茶酚;400~500℃,共检出27种主要组分,包括初级裂解产物和1,3-环戊二烯、呋喃、烷基苯酚、甲基儿茶酚、苯甲酸类、芳香烃和多苯环化合物等二次裂解产物;500~600℃,裂解产物中含量较高的是二氧化碳、水和一氧化碳,其次是苯酚、儿茶酚和3-甲基苯酚;600~700℃,主要的挥发性成分是水、二氧化碳和一氧化碳,还有少量的苯、甲苯、苯酚和3-甲基苯酚;700~800℃和800~900℃,裂解产物只有水、二氧化碳和一氧化碳。因此,结合热重分析的梯度裂解产物分析能够为研究绿原酸的裂解过程提供更多的信息。

     

    Abstract: In order to accurately reveal the pyrolysis process of chlorogenic acid (CGA),the pyrolysates of CGA were analyzed at ten temperature ranges,which were divided on the basis of thermogravimetric curve and pyrolytic characteristics of CGA,by an online gas chromatography/mass spectrometry (GC/MS).The results indicated that:1) The pyrolysis process of CGA could be divided into at least 6 temperature ranges,at which the weight-loss of CGA were 2.94%,0.61%,8.55%,20.29%,34.32% and 9.43%,respectively.2) The major components produced at the ten temperature ranges were as follows:Only water was observed at 30-120℃; no products were detected at 120-190℃; water,carbon dioxide and quinide-like compounds were formed at 190-260℃; carbon dioxide,phenol,catechol,hydroquinone,water and quinide-like compounds were released at 260-325℃; comparing with the products at 260-325℃,3-hydroxy benzoic acid,benzoic acid and 4-ethyl catechol were new at 325-400℃; 27 major pyrolysates were identified at 400-500℃, besides primary products,these were secondary products,such as 1,3-cyclopentadienes,furan,alkyl phenols,methyl catechols,benzoic acids,aromatic hydrocarbons and multi-benzene ring compounds; the concentrations of carbon dioxide,water and carbon monoxide were higher,which followed by phenol,catechol and 3-methyl phenol at 500-600℃; the main volatile components were water,carbon dioxide and carbon monoxide,and there were also a small quantity of benzene,toluene,phenol and 3-methyl phenol at 600-700℃; only water,carbon dioxide and carbon monoxide were observed at 700-800℃ and 800-900℃.The gradient pyrolysate analysis combining with thermogravimetric analysis could provide more information for investigating the pyrolysis process of CGA.

     

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