栀子苷在乙腈水体系中诱导相分离分配行为

doi:10.3724/SP.J.1095.2013.30125

摘要/Abstract

摘要： 研究了栀子乙腈水提取液中的栀子苷在诱导相分离后在两相中的分配行为，建立了乙腈/水分相体系分离纯化栀子苷的新方法。重点考察了能使乙腈/水体系分相的诱导剂的种类，分析了诱导剂的组成比例以及用量、乙腈的体积分数、样品加入量和温度对栀子苷分配行为的影响。当温度为25 ℃时，栀子的乙腈/水（体积比1∶1）提取液中加入KCl与MgSO4组成的混盐（质量比2∶1）分相诱导剂后，栀子苷的萃取率达到81.63%，含量由分相前的3.05%提高至13.54%。

关键词: 栀子苷, 栀子果, 乙腈水提取液, 诱导相分离, 分离纯化

Abstract: After geniposide in the acetonitrile aqueous extract solution of Gardenia was separated into two phases by inductors, the partition characteristics of it in two phases were studied. A new method was established for the separation and purification of geniposide. The types of inductors inducing phase separation of acetonitrile aqueous solution were researched in detail. The effects on partition characteristics of geniposide were analyzed via investigation of the composition proportion of inductors, the additive amount of inductors, the volume fraction of acetonitrile, the additive amount of sample and temperature. The results show that when inductors were added into the acetonitrile/aqueous(volume ratio 1∶1) extract at 25 ℃, the preliminary purification of geniposide could be finished by one step. The extraction yield of geniposide reaches 81.63% and the purity is increased from 3.05% primitively to 13.54%. The best inductors are composed of KCl and MgSO4(mass ratio 2∶1).

Key words: geniposide, gardenia, acetonitrile aqueous extract solution, inducing phase separation, separation and purification

中图分类号:

O658.2

盛碧, 陈智, 李红舟, 陈波. 栀子苷在乙腈水体系中诱导相分离分配行为[J]. 应用化学, DOI: 10.3724/SP.J.1095.2013.30125.

SHENG Bi, CHEN Zhi, LI Hongzhou, CHEN Bo*. Partition Characteristics of Geniposide in Inducing Phase Separation of Acetonitrile Aqueous Solution System[J]. Chinese Journal of Applied Chemistry, DOI: 10.3724/SP.J.1095.2013.30125.

参考文献

[1] CHENG Hong,XIAO Yongqing,LI Li,et al. Studies on Chemical Constituents in Fruit of Gardenia Jasminoides[J]. China J Chinese Mater Med,2007,32(11):1041-1043(in Chinese).

陈红,肖永庆,李丽,等. 栀子化学成分研究[J]. 中国中药杂志,2007,32(11):1041-1043.

[2] MENG Xiangle,LI Hongwei,LI Yan,et al. Advances in Studies on Chemical Constituents and Pharmacological Activities of Gardenia Jasminoides[J]. China J New Drugs,2011,20(11):959-967(in Chinese).

孟祥乐,李红伟,李颜,等. 栀子化学成分及其药理作用研究进展[J]. 中国新药杂志，2011,20(11):959-967.

[3] FU Honglei,LIANG Huazheng,LIAO Fusheng. Present Condition and Perspective of Utilization of the Geniposide in Gardenia Jasminoides[J]. Lishizhen Med Mater Med Res,2005,16(1):54-56(in Chinese).

付红蕾,梁华正,廖夫生. 栀子中京尼平苷的研究现状和应用前景[J]. 时珍国医国药,2005,16(1):54-56.

[4] TANG Ronghua,DUAN Wei,CHEN Bo,et al. Preparation of Genipin Cross-linked Magnetic Chitosan Microsphere and Its Immobilization on Lipase[J]. Chinese J Appl Chem,2013,30(8):922-926(in Chinese).

唐荣华,段玮,陈波,等. 京尼平交联磁性壳聚糖微球的制备及其脂肪酶的固定化[J]. 应用化学,2013,30(8):922-926.

[5] YIN Yuji,YAO Kangde,LIU Wenguang,et al. Chitosan-Gelatin Network Based Biomaterials in Tissue Engineering[J]. Chinese J Appl Chem,2004,21(3):217-222(in Chinese).

尹玉姬,姚康德,刘文广,等. 组织工程相关壳聚糖-明胶基生物材料[J]. 应用化学,2004,21(3):217-222.

[6] Jin J,Song M,Hourston D J. Novel Chitosan-Based Films Cross-Linked by Genipin with Improved Physical Properties[J]. Biomacromolecules,2004,5(1):162-168.

[7] MA Chunhong,ZHU Hong,WANG Lang,et al. Application and Progress of Aqueous Two-Phase Extraction Technology[J]. China J Spectrosc Lab,2010,27(5):1906-1914(in Chinese).

马春宏,朱红,王良,等. 双水相萃取技术的应用研究进展[J]. 光谱实验室，2010,27(5):1906-1914.

[8] LIN Jinqing,JIN Chunying,TANG Pinghua,et al. Phase Separation and Mechanism of Hydrophilic Organic Phase-Salt Aqueous Solution System[J]. Chinese J Appl Chem,2005,22(11):1203-1207(in Chinese).

林金清,金春英,谭平华,等. 亲水有机相-含盐水两相体系的形成机理与分相能力[J]. 应用化学,2005,22(11):1203-1207.

[9] LIU Yang,YU Yonglei,SU Hongcai,et al. Effect of Salt on the Aqueous Two- Phase System Equilibrium Comprising PEG[J]. Chem Res Appl,2011,23(9):1205-1208(in Chinese).

刘杨,虞永蕾,苏红彩,等. 成相无机盐种类对PEG双水相相平衡影响[J]. 化学研究与应用,2011,23(9):1205-1208.

[10] Liu G Z,Yang H,Chen Bo,et al. Novel Isolation of Phytochemical Compositions by Phase Transition Extraction with Acetonitrile[J]. J Sep Sci,2011,34(3):347-353.

[11] ZHANG Mingshan,LIU Guozhu,CHEN Bo,et al. Solvent Induced Phase Transition Extraction Method for High Performance Liquid Chromatography Mass-Spectrometry Analysis of Plasma Samples of Pretreatment[J]. Chem J Chinese Univ,2010,31(8):1517-1521(in Chinese).

张鸣珊,刘国柱,陈波,等. 溶剂诱导相变萃取法用于高效液相色谱-质谱分析的血浆样品前处理[J]. 高等学校化学学报,2010,31(8):1517-1521.

[12] Liu G Z,Zhou N,Chen B,et al. Hydrophobic Solvent Induced Phase Transition Extraction to Extract Drugs from Plasma for High Performance Liquid Chromatography Mass Spectrometric Analysis[J]. J Chromatogr A,2010,1217(3):243-249.

[13] PENG Sheng,PENG Mijun,HUANG Meie,et al. Extraction and Separation of Flavonoids from Leave of Eucommiaulmoides in Aqueous Two phase System[J]. J Chinese Med Mater,2009,32(11):1754-1757(in Chinese).

彭胜,彭密军,黄美娥,等. 双水相体系萃取分离杜仲黄酮[J]. 中药材,2009,32(11):1754-1757.