解吸-内部沸腾两步法提取植物有效成分工艺及其工艺及其机理的研究
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摘要
在中医药的现代发展史中,中草药的提取生产过程在我国己有很悠久的历史,但是还普遍存在着生产工艺落后,提取得率低等问题。为了提高有效成分的收率,降低生产成本,应当利用中草药的提取过程进行深入的研究和分析。为此,通过对其机理研究,探索其过程,合理制定提取工艺是一个重要课题。
本文提出了解吸-内部沸腾两步提取法,该法是先将植物干物料粉碎,再加入一定量的解吸剂,等充分浸润后再加入沸腾的溶剂提取,过滤分离,提取两次。用该提取法对金银花、银杏叶、肉桂皮和黄连的有效成分进行了提取,同时做了传统法实验与之比较,结果表明该方法与传统回流提取法相比不仅可以大量缩短提取时间,减少有机溶剂的消耗,还提高了提取液和浸膏中有效成分的含量。效果显著,具有良好的应用前景。此外还与文献中的微波预处理提取方法进行了比较,获得了与它相似的提取效果,但却节省了提取设备,更易于实现产业化。
为了对两步法深入了解,本文对提取机理进行了研究,通过改变提取温度来观察提取效果,发现提取温度在解吸剂沸点附近时提取速率有一个突变,因而提出了孔内沸腾传质机理,即通过加入沸腾的热溶剂使预先进入植物细胞内部的解吸剂沸腾汽化,汽化产生的内部汽液对流,夹带有效成分快速离开植物组织的过程,从而加速了提取速
In the phylogeny of Chinese traditional medicine, application of its extraction had a long history in our country, but many problems weren't solved such as old-dated extraction process, low extraction rate and so on. In order to increase ratio of effectual component in extraction succus and decrease production cost, it was necessary to apply modern techniques to research and analyze its extraction process.This paper put forward the extraction method of the two-step of release and internal evaporation of liquid. In Two-step, first, the plant was put into little releasable solvent. And then, after the effectual component in these materials was desorbed by releasable solvent adequately, boiling extraction solvent was added. The boiling extraction solvent was filtrated and separated and then the same process was undertaken to the sedimentation. The result showed that compared with extraction of traditional one, effectual component of Flos Lonicerae, Ginkgo biloba, Chinese cinnamon and Rhizoma Coptidis were extracted by this method, it had many advantages: the extraction time was shorter, the consumption of organic solvent was lower and the content of effectual component was higher and so on. Furthermore, compared with modern extracting methods such as microwave extracting method, this method obtained same extraction effect, but it reduced the equipments of extraction. Moreover, this method was easier to undertake in factory, so it had a good future in industrial application.In order to understand Two-step thoroughly, extraction temperature was changed to observe the effect of extraction. This paper studied the mechanism of Two-step extraction method. When temperature was around boiling point of
releasable solvent, the extraction ratio had a break, and then the mechanism of internal evaporation of liquid was put forward. This method was that, when boiling hot solvent was poured into plant materials that was desorbed by releasable solvent, the releasable solvent inner the plant boiled before the diffusion of releasable solvent, the boiling caused inner convection and made effectual component to be extracted quickly out of the plant. As a result, the extraction speed quickened. By observing the phenomena in the process of the experiment, the bubble was produced inside the inner grain and then it lightened the density of the grain and slowed down sedimentation velocity.
本文提出了解吸-内部沸腾两步提取法,该法是先将植物干物料粉碎,再加入一定量的解吸剂,等充分浸润后再加入沸腾的溶剂提取,过滤分离,提取两次。用该提取法对金银花、银杏叶、肉桂皮和黄连的有效成分进行了提取,同时做了传统法实验与之比较,结果表明该方法与传统回流提取法相比不仅可以大量缩短提取时间,减少有机溶剂的消耗,还提高了提取液和浸膏中有效成分的含量。效果显著,具有良好的应用前景。此外还与文献中的微波预处理提取方法进行了比较,获得了与它相似的提取效果,但却节省了提取设备,更易于实现产业化。
为了对两步法深入了解,本文对提取机理进行了研究,通过改变提取温度来观察提取效果,发现提取温度在解吸剂沸点附近时提取速率有一个突变,因而提出了孔内沸腾传质机理,即通过加入沸腾的热溶剂使预先进入植物细胞内部的解吸剂沸腾汽化,汽化产生的内部汽液对流,夹带有效成分快速离开植物组织的过程,从而加速了提取速
In the phylogeny of Chinese traditional medicine, application of its extraction had a long history in our country, but many problems weren't solved such as old-dated extraction process, low extraction rate and so on. In order to increase ratio of effectual component in extraction succus and decrease production cost, it was necessary to apply modern techniques to research and analyze its extraction process.This paper put forward the extraction method of the two-step of release and internal evaporation of liquid. In Two-step, first, the plant was put into little releasable solvent. And then, after the effectual component in these materials was desorbed by releasable solvent adequately, boiling extraction solvent was added. The boiling extraction solvent was filtrated and separated and then the same process was undertaken to the sedimentation. The result showed that compared with extraction of traditional one, effectual component of Flos Lonicerae, Ginkgo biloba, Chinese cinnamon and Rhizoma Coptidis were extracted by this method, it had many advantages: the extraction time was shorter, the consumption of organic solvent was lower and the content of effectual component was higher and so on. Furthermore, compared with modern extracting methods such as microwave extracting method, this method obtained same extraction effect, but it reduced the equipments of extraction. Moreover, this method was easier to undertake in factory, so it had a good future in industrial application.In order to understand Two-step thoroughly, extraction temperature was changed to observe the effect of extraction. This paper studied the mechanism of Two-step extraction method. When temperature was around boiling point of
releasable solvent, the extraction ratio had a break, and then the mechanism of internal evaporation of liquid was put forward. This method was that, when boiling hot solvent was poured into plant materials that was desorbed by releasable solvent, the releasable solvent inner the plant boiled before the diffusion of releasable solvent, the boiling caused inner convection and made effectual component to be extracted quickly out of the plant. As a result, the extraction speed quickened. By observing the phenomena in the process of the experiment, the bubble was produced inside the inner grain and then it lightened the density of the grain and slowed down sedimentation velocity.
引文
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[5] 李鹰,丁青龙,赵静安.用正交试验探讨金银花煎煮条件对绿原酸含量的影响[J].江苏药学与临床研究,2000,8(1):33-35.
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[7] 黄祖良,何有成,韦国锋,等.从植物十大功劳中制取四氢小檗碱的工艺研究[J],广西化工,2002,32(2):16-17,49.
[8] 张春红,张崇禧,郑友兰,等.浸渍法提取人参皂苷最佳工艺的研究[J].吉林农业大学学报,2003,25(1):73～74,78.
[9] 刘进月,赵典刚,韩月香.渗漉法提取芦丁的实验研究[J].中国中医药科技,1999,6(5):320-321.
[10] 邵方晓,刘吉晨.苦参总碱浸膏提取工艺的研究[J].中国新医药,2003,2(6):8.
[11] 刘祥兰,刘重芳,张英,等.金银花中绿原酸提取工艺的比较和优化研究[J].中成药,2000,22(6):402-404.
[12] 方阵,吴健,王康才.正交实验筛选黄连水提工艺[J].时珍国医国药,2001,12(11):982-983.
[13] Qingyong Lang, Chien M. Wai. Supercritical fluid extraction in herbal and natural product studies—a practical review [J]. Talanta, 2001(53):771-782.
[14] 韩玉谦,隋晓.银杏叶活性成分萃取工艺的研究[J].精细化工,2000,17(9):505-506,514.
[15] 曾虹燕,周朴华,唐艳林.石香薷挥发油提取的比较研究[J].天然产物研究与开发,2003,15(2):135-137.
[16] 陈从贵,潘见,张宏康.超临界CO2提取分离银杏叶药用成分的工艺研究[J].农业工程学报,2002,18(4):142-145.
[17] 冯青然,陈燕军.中药提取工艺研究进展[J].中国实验方剂学杂志,9(s):61-64.
[18] Mircea Vinatoru. An overview of the ultrasonically assisted extraction of bioactive principles form herbs [J]. Ultrasonic Sonochemistry, 2001(8):303-313.
[19] J.L. Luque-Garcya, M.D. Luque de Castro. Ultrasound-assisted Soxhlet extraction: an expeditive approach for solid sample treatment Application to the extraction of total fat from oleaginous seeds[J]. Chromatography A, 2004 (1034): 237-242.
[20] Zdena Hromadkova, Ju lia Kovacikova, Anna Ebringerova. Study of the classical and ultrasound-assisted extraction of the corn cob xylan[J]. Industrial Crops and Products, 1999(9): 101-109.
[21] 王万能、全学军、陆天健.超声波提取大豆异黄酮动力学研究[In].第一届全国化学工程与 生物化工年会论文摘要集(下),南京,2004:994-995.
[22] 冯青然,陈燕军.中药提取工艺研究进展[J].中国实验方剂学杂志,2003(9s):61-64.
[23] Inci Cinar. Effects of Cellulase and Pectinase Concentrations on the Ccolour Yield of Enzyme Extracted Plant Carotenoids[J]. Process Biochemistry, 2005(40): 945-949.
[24] Francisco Delgado-Vargas, Octavio Paredes-Lopez. Effects of enzymatic treatments on carotenoid extraction form marigold flowers [J]. Food Chemistry, 1997(58):255-258.
[25] 许明淑,罗明芳,邢新会.银杏叶黄酮的酶法提取强化工艺条件研究[In].第一届全国化学工程与生物化工年会论文摘要集(下),南京,2004:1004-1005.
[26] Cecilia Sparr Eskilsson, Erland Bjorklund. Analytical-scale Microwave-assisted Extraction [J]. Journal of Chromatography A, 902 (2000):227-250.
[27] Pare J R J,Belanger J M R,Stafford S S. Microwave Assisted Process(MAPTM)a: a new tool for the analytical laboratory[J].Trends in Analytical Chemistry, 1994, 13(4): 176.
[28] 郝金玉,韩伟,邓修.新鲜银杏叶经微波辅助提取后微观结构的变化[J].中草药,2002,33(8):739-741.
[29] Rong Tsao, Zeyuan Deng. Separation Procedures for Naturally Occurring Antioxidant Phytochemicals[J]. Journal of Chromatography B, 2004 (812): 85-99.
[30] 沈岚,冯年平,韩朝阳,等.微波萃取对不同形态结构中药及含不同极性成分中药的选择性研究[J].中草药,2002,32(7):604.
[31] Maria Then, Klara Szentmihalyi, Agnes Sarkozi, etc. Effect of sample handling on alkaloid and mineral content of aqueous extracts of greater celandine (Chelidonium majus L.)[J]. Journal of Chromatography A, 2000 (889): 69-74.
[32] Devanand P, Fulzele, Ramesh K, Satdive. Comparison of techniques for the extraction of the anticancer drug camptothecin from Nothapodytes foetida[J].Chromatography A, 2005(1063):9-13.
[33] 杨张渭,张善政,邓丽仪,等.人参精采用超滤工艺的中式研究[J].中成药,1994,16(1):4.
[34] 王成章,郁青,潭卫红,等.超滤在纯化银杏叶黄酮甙中的应用[J].林业科技通讯,1997,(2):21.
[35] 彭国平,郭立玮,徐丽华,等.超滤技术应用对中药成分的影响[J].南京中医药大学学报,2002,18,6.
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