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废弃烟叶中有效成分提取分离与纯化

Extraction,separation and Purification of Effective Components from Waste Tobacco Leaves

【作者】 刘振宇

【导师】 董悦生;

【作者基本信息】 大连理工大学 , 生物工程(专业学位), 2017, 硕士

【摘要】 我国是一个烟草种植大国,烟草种植面积和产量排在世界前列,但是由于缺乏相关的技术手段,卷烟的生产过程中未充分利用而遭废弃的烟叶约占烟叶总量的25%。烟叶中已经测定出含有300多种化合物,有效成分在化工、医药、农业等多个领域有着广泛的应用,如烟碱可用来生产烟碱农药;茄尼醇是生产辅酶Q10和维生素K2等药物的必要原料;绿原酸可以用来作为生物试剂和药物的原料等,将废弃烟叶中有效成分进行提取分离不仅实现这些成分的综合利用,也能够降低废弃物对环境的污染。本论文提供了一种高效利用烟叶有效成分综合利用的方法,以云南废弃烟叶为原料,首先建立了烟碱、茄尼醇、绿原酸的HPLC定量分析方法,测定废弃烟叶中烟碱、茄尼醇和绿原酸的含量分别为31.5±0.3 mg/g,13.1±0.1 mg/g,5.0±0.2 mg/g。确定了烟叶中有效成分的提取方法为热回流提取,最佳工艺条件为pH 2的50%乙醇热回流3次,纯乙醇热回流提取1次,热回流温度为50°C,热回流时间为0.5 h。烟碱、茄尼醇和绿原酸收率分别为75.09%、76.22%、117.4%。将0.12 mol/L Ca(OH)2溶液到加入50%乙醇提取液中,可实现绿原酸和其他成分的分离,绿原酸沉淀使用酸水溶解,乙酸乙酯萃取可获得绿原酸粗品,总收率为88.4%,纯度为25.0%。萃余相调pH 8,使用石油醚反复萃取,可得高纯度烟碱,最终烟碱收率为68.3%,纯度为95.1%。对纯乙醇提取液进行皂化处理可提高茄尼醇的收率,皂化条件为0.45 mol/L Na OH,温度为70°C,时间为3 h,石油醚萃取两次,可以得到纯度为25.3%的茄尼醇,总收率为92.3%。质量分析表明烟碱、茄尼醇和绿原酸中均未见其他两种成分残留。经过放大实验,该工艺收率和产品质量均稳定。本论文开发的工艺,实现了烟碱、茄尼醇和绿原酸的综合利用,具有工艺简单、有效成分的纯度和收率高的特点,为废弃烟叶的综合利用奠定了基础。

【Abstract】 China has large tobacco cultivation area and production,but about 25% of tobacco leaves wasted in the production of cigarettes due to planting management techniques and processing technology.The tobacco leaves contain more than 300 kinds of compounds,the effective component,including nicotine,solanesol,chlorogenic acid are widely used in the chemical industry,medicine,agriculture and other aspects.For example,the nicotine can be used as pesticides;solanesol can be used to as material to produce coenzyme Q10 and vitamin K2;chlorogenic acid is also an important biological reagents and pharmaceutical raw materials.In this paper,a new approach for the efficient use of active ingredients in tobacco leaves is provided.Using the waste tobacco leaves from Yunnan,the research on the extraction and separation method was carried out.The HPLC analytical methods of three substances were established firstly.The contents of nicotine,solanesol and chlorogenic acid were determined as 3.15%,1.31% and 0.50% by Soxhlet extraction,respectively,and were used as criterion to determine the yield for each extraction steps.The extraction method was ethanol hot reflux extraction,the optimum conditions were refluxed at 50% ethanol at p H 2 for 1 time,ethanol extraction for 1 time,hot reflux temperature was set as 50 °C and the hot reflux time was set at 30 min,respectively.The recoveries of nicotine,solanesol and chlorogenic acid were 75.09%,76.22% and 117.4%,respectively.Adding 0.12 mol / L Ca(OH)2 to the 50% ethanol extract,the chlorogenic acid could be obtained in precipitation phase.This precipitation was dissolved and extracted by ethyl acetate,at pH 2 for 5 times to give crude chlorogenic acid.The recovery was 88.4% and the purity was 25.0%,respectively.Extracting the raffinate phase with petroleum ether at pH 8,5 times,will give crude nicotine with recovery of 75.2% and the purity of 95.1%.The ethanol extract was then saponified 0.45 mol / L NaOH,70°C,for 3 h.And solanesol could be separated and obtained from the saponification solution by solvent extraction method.Extracting with ether twice,gave crude solanesol was recovery of 87.86% and purity of 25.3%.Quality analysis indicated that completely separation of one of the components from the other two components was achieved.The recovery and quality of three products were proved to be stable though scale-up experiment.The new approach in the thesis realized the comprehensive utilization of active ingredients in tobacco leaves,with the characters of simple process,high purity and high recovery of the products.It will play solid foundation of utilization of waste tobacco leaves.

  • 【分类号】TQ914.3
  • 【被引频次】12
  • 【下载频次】760
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