核壳型色谱柱-高效液相色谱法快速分离检测水飞蓟素中7种非对映异构体  

Rapid Separation and Determination of Seven Diastereoisomers in Silymarin by Core-Shell Column-High Performance Liquid Chromatography

作　　者：徐静涵[1] 薛芸[1] 王彦[1] 闫超[1] 

机构地区：[1]上海交通大学,上海200240

出　　处：《化学与生物工程》2017年第6期65-70,共6页Chemistry & Bioengineering

基　　金：上海市科委科研计划项目(15142200200;16142200300);上海市博士后基金项目(14R21422700);上海市引进技术的吸收与创新专项(XC-ZXSJ-02-2016-11)

摘　　要：采用核壳型色谱柱-高效液相色谱法快速分离检测水飞蓟素中7种非对映异构体,优化了液相色谱条件,实现了7种非对映异构体的快速完全分离,并应用于市售水飞蓟制剂的分离检测。优化色谱条件如下:核壳型Halo C_(18)色谱柱(150mm×4.6mm,2.7μm)、甲醇-水-甲酸(30∶70∶0.1)-甲醇为流动相、梯度洗脱、流速0.35mL·min^(-1)、进样量2μL。该方法在0.01~0.1mg·mL^(-1)浓度范围内线性关系良好(R2>0.997),色谱峰峰面积和保留时间的相对标准偏差(RSD)分别为1.74%和0.67%(n=6)。该方法操作简单、省时、分离度好,可用于水飞蓟制剂的分析检测,也为水飞蓟素中非对映异构体的分离检测提供新的思路。In this study,seven diastereoisomers in silymarin were separated and determined rapidly by coreshell column-high performance liquid chromatography（HPLC）. The chromatographic conditions were opti- mized,rapid separation of seven diastereoisomers were achieved, and the separation and determination of the common commercial Silybum marianum preparations were also carried out with this method. The optimum chromatographic conditions were as follows： Halo C18 column（150 min×4.6 mm,2.7 μm） ,gradient elution with methanol-water-formic acid（30 ：70 ： 0.1）-methanol as a mobile phase,flow rate of 0.35 mL · min-1 ,injection volume of 2 μL. The linear relationship was good in the range of 0.01-0.1 mg · mL -1（R2〉0. 997）. The relative standard deviation（RSD） of the chromatographic peak area and the retention time were 1.74% and 0.67% （n=6） ,respectively. The advantages of this method are simple operation,short time and high separation degree. It can be used to analyze Silybum marianum preparations,and also provides a new idea for the separation and determination of diastereoisomers in silymarin.

关 键 词：高效液相色谱法 核壳型色谱柱 水飞蓟素 非对映异构体 

分 类 号：O658[理学—分析化学] O657.72[理学—化学]