[1]王西宁,朱靖博,丁燕,等.桂枝化学成分系统化色谱分离方法研究[J].北方园艺,2013,37(14):107-111.
　WANG Xi-ning,ZHU Jing-bo,DING Yan,et al.Study on Systemic Chromatography Separation Methods of Chemical Compounds from Cinnamomi ramulus[J].Northern Horticulture,2013,37(14):107-111.

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桂枝化学成分系统化色谱分离方法研究

《北方园艺》[ISSN:1001-0009/CN:23-1247/S] 卷: 第37卷期数: 2013年14期页码: 107-111 栏目: 出版日期: 2013-07-15

Title:: Study on Systemic Chromatography Separation Methods of Chemical Compounds from Cinnamomi ramulus

文章编号:: 1001-0009(2013)14-0107-05

作者:: 王西宁¹; 朱靖博¹; 2; 丁燕¹; 2; 寇自农²; 王振中³; 萧伟³; 1.大连工业大学食品学院，辽宁大连 116034；
2.大连工业大学植物资源化学与应用研究所，辽宁大连 116034；
3.江苏康缘药业有限公司，江苏连云港 222001

Author(s):: WANG Xi-ning1; ZHU Jing-bo1; 2; DING Yan1; 2; KOU Zi-nong2; WANG Zhen-zhong3; XIAO Wei3; 1.School of Food Science and Technology,Dalian Polytechnic University,Dalian,Liaoning 116034；2.Institute of Chemistry and Application of Plant Resources,Dalian Polytechnic University,Dalian,Liaoning 116034；
3.Jiangsu Kanion Pharmaceutical Company Limited,Lianyungang,Jiangsu 222001

关键词:: 桂枝; 色谱分离; 薄层层析色谱; 制备色谱

Keywords:: Cinnamomi ramulus; chromatography separation; thin layer chromatography; preparative chromatography

分类号:: S 503.53

文献标志码:: A

摘要:: 以中药桂枝为试材，采用TLC和HPLC分析法对桂枝化学成分系统性色谱分离的样品前处理、色谱分离条件和制备色谱参数进行了系统研究。在台阶梯度洗脱时，根据TLC数据中的Rf值，利用化合物的移动速率u=u₀/(1+k)，对各化合物色谱分离洗脱剂的保留体积可以进行较准确的计算与预测，避免色谱分离时的盲目性。结果表明：甲醇提取和正己烷萃取是富集桂枝主要化学成分的有效方法；研究建立的系统性TLC分析方法可以快速有效地选择桂枝主要成分色谱分离的填料、溶剂体系、比例及程序。桂枝主要成分的最佳色谱分离填料为硅胶，最佳洗脱体系为正己烷乙酸乙酯。采用建立的条件经一次制备色谱分离，得到了8个纯化合物，5个化合物的HPLC纯度均在95%以上。该研究建立了桂枝化学成分有效的系统化色谱分离方法。

Abstract:: Taking Cinnamomi ramulus as material,the systemic chromatography separation methods including pre treatment of samples,selection of chromatography separation conditions and the estimate of parameters about preparative chromatography were systemically studied.Elution volumes of reagents and retention volume of each compounds could be calculated and estimated accurately based on the Rf value of TLC data and moving velocity of compounds u=u₀/(1+k) in silica gel chromatography which avoided the blindness of separation process.The results showed that extracted by methanol and nhexane extraction were effective methods for the enrichment of main compounds of Cinnamomi ramulus；the systemic TLC methods studied and built would select chromatography packing,reagents systems and reagents proportion quickly and effectively.For main compounds of Cinnamomi ramulus the best chromatography separation packing was silica gel and the best elution system was nhexane/ethyl acetate.8 compounds were separated by once preparative chromatography separation which conditions were selected by this method and purity of 5 fractions were greater than 95% detected by HPLC.Systemic chromatography separation methods for chemical compounds of Cinnamomi ramulus were built.

参考文献/References:

[1]刘江云.常用中药桂枝化学成分的研究[D].北京:中国协和医科大学,2002.

[2]Liu C,Zhong S M,Chen R Y,et al.Two new compounds frm the dried tender stems of Cinnamomum cassia[J].J Asian Nat Prod Res,2009,11(9):845-849.

[3]Tran M N,Do T H,Ik S L,et al.Two new diterpenes from the twigs of Cinnamomum cassia[J].Helv Chim Acta,2009,92:2058-2062.

[4]Tran M N,Ik S L,Do T H,et al.Tyrosinase inhibitory constituents from the twigs of Cinnamomum cassia[J].J Nat Prod,2009,72:1205-1208.

[5]Sun Y K,Yean K K,Ja Y K,et al.Platelet anti aggregation activities of compounds from Cinnamomum cassia[J].J Med Food,2010,13(5):1069-1074.

[6]Lu D Y,Kang Q S.Theory and practice from TLC to industrial preparative chromatography(IPC)in the separation of natural product[J].Natural product research and development,2004,16:153-156.

[7]Justin D F,Chad M K.Flash column chromatograms estimated from thin ayer chromatography data[J].J Chromatography A,2008,1211:49-54.

[8]Tero W,Irena V,Pia V,et al.Use of drylab for simulation of TLC separation and method transfer from TLC to HPLC[J].J Planar Chromatography,2009,19:118-122.

[9]许琴永.药食两用中药抑制α葡萄糖苷酶活性及作用机制研究[D].大连:大连工业大学,2010.

[10]卢佩章.高效液相色谱法及其专家系统[M].大连:辽宁科学技术出版社,1991:322-359.

[11]Ding Y,Wu E Q,Liang C,et al.Discrimination of cinnamon bark and cinnamon twig sample sourced from various countries using HPLC based fingerprint analysis[J].Food Chemistry,2011,127:755-760.

[12]张艺轩.基于液质联用技术的温络方药效物质基础研究[D].北京:北京协和医学院,2010.

[13]Szabolcs N,Karin D T,Georg C,et al.Strategies of mobile phase transfer from thin layer to medium pressure liquid chromatography with silica as the stationary phase[J].J Chromatography A,1990,499:453-462.

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备注/Memo

第一作者简介：王西宁（1989-），女，硕士研究生，研究方向为天然产物的研究及开发利用。E-mail:wangxining2010@126.com.

责任作者：朱靖博（1963-），男，博士，教授，硕士生导师，研究方向为中药现代化研究开发与应用。E-mail:zhujingb@sina.com.

基金项目：中药制药过程新技术国家重点实验室资助项目（SKL2010M0205；SKL2010Z0201）。

收稿日期：2013-03-04

更新日期/Last Update: 2014-08-10