摘要
所研制的圆盘嵌入式螺旋管高速逆流色谱仪采用双分离柱串联设计,公转半径为70mm,β值范围为0.3～0.7,柱总容积为30mL。将所研制的新型分离柱与传统多层缠绕色谱柱对不同溶剂体系的保留能力进行对比,根据溶剂极性不同,分别选择正庚烷-甲醇、正己烷-乙酸乙酯-甲醇-水、正丁醇-醋酸-水及聚乙二醇1000-磷酸钾盐-水双水相体系用于固定相保留能力的研究。结果表明:在L-I-T洗脱模式下,当流速为1mL/min时,传统多层缠绕色谱柱和圆盘嵌入式螺旋管高速逆流色谱仪在正庚烷-甲醇体系中的固定相保留率(Sf)分别为50%和60%,在正己烷-乙酸乙酯-甲醇-水体系中的Sf值分别为60%和68%。在U-O-H洗脱模式下,流速为0.5mL/min时,传统多层缠绕色谱柱和圆盘嵌入式螺旋管高速逆流色谱仪在正丁醇-醋酸-水体系中的Sf值分别为22%和60%;在L-I-T洗脱模式下,流速为0.5mL/min时两种色谱柱在聚乙二醇1000-磷酸钾盐-水双水相体系中的Sf值分别为15%和46%。各个体系下Sf与(1/g-levels)1/2线性相关。将所研制的新型逆流色谱仪初步应用于黑果枸杞花青素样品的分离,对其实际分离纯化能力进行考察研究。采用极性较强的甲基叔丁基醚-正丁醇-乙腈-水-三氟乙酸(体积比2.5:1.5:1:5:0.001),在1mL/min的流速下,分离得到纯度89%黑果枸杞花青素。
A type-J coil planet centrifuge with a 7.0 cm revolution radius was designed through the tandem connection of two spiral tubes. The β value was in the range of 0.3-0.7. The total column capacity was 30 mL. Different polarity solvent systems such as n-heptane：methanol, n-hexane：ethyl acetate：methanol：water, n-butanol：acetic acid：water and PEG 1000：K2HPO4：water were used to comparatively study the retention capacities of the new HSCCC and the traditional multilayer coil HSCCC. The stationary phase retention factor （Sf） of the traditional multilayer coil HSCCC was 50% in n-heptane：methanol system and 60% in n-hexane：ethyl acetate：methanol：water system at a flow rate of 1 mL/min under the L-I-T elution mode, while for the spiral tube HSCCC, the Sf values were 60% and 68%, respectively. The Sfvalues of the traditional multilayer coil HSCCC and the spiral tube HSCCC were 22% and 60% in n-butanol：acetic acid：water system at a flow rate of 0.5 mL/min under the U-O-H elution mode and 15% and 46% in PEG 1000：K2HPO4：water system at the same flow rate under the L-I-T elution mode, respectively. An excellent linear relationship between Sf and （l/g-levels）^1/2 was achieved using each investigated solvent system. The new HSCCC was applied to separate anthocyanins from Lycium ruthenicum Murr. using a highly polar system composed of methyl tert-butyl ether, n-butanol, acetonitrile, water and trifluoroacetic acid （2.5：1.5：1：5：0.001）, and the results showed that anthocyanins with a purity of 89% were obtained at a flow rate of 1 mL/min.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2012年第11期1-7,共7页
Food Science
基金
国家自然科学基金项目(20877005)
关键词
高速逆流色谱
圆盘嵌入式螺旋管柱
双水相全系
花青素
high-speed counter-current chromatography
spiral tube column
aqueous two-phase system
anthocyanins
作者简介
裴海闰（1984-），男，硕士，研究方向为生物分离技术。E—mail：peihairun@th．btbu．edu．cn
通信作者：曹学丽（1967-），女，教授，博士，研究方向为生物分离技术。E—mail：caoxl@th．btbu．edu．cn
