菊苣酸在高效液相色谱测定过程中与流动相中银离子配位的探讨  

Study of Coordination of Cichoric Acid with Silver Nitrate in Mobile Phase in its Determining Process by High Performance Liquid Chromatography

作　　者：周蓓蓓[1] 潘见[1] 开桂青[1] 金日生[1] 

机构地区：[1]合肥工业大学,农产品生物化工工程技术研究中心,合肥230009

出　　处：《分析化学》2008年第9期1245-1248,共4页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金重点项目(NO.20136020)资助

摘　　要：菊苣酸是紫锥菊属植物中的一种水溶性酚酸类化合物。本研究对紫锥菊提取物中菊苣酸检测的条件是:流动相为V(乙腈):V(去离子水)=38:62(含0.8%冰醋酸和8mmol/LAgNO3);色谱柱为RestekPinna-cle11C18柱(250mm×4.6mm,5μm);流速为0.5mL/min;进样量为10μL;检测波长为326nm。实验发现,在流动相中添加AgNO3后可以明显改善菊苣酸测定效果,提高分离度,并有效除去其它杂质成分的干扰,r大于0.99;检出限为8～40mg/L,此方法的相对标准偏差小于3.0%;平均回收率为98.5%,方法符合测试要求。AgNO3改善分离效果的原因可能为菊苣酸和Ag+之间存在一定的配位作用,改变了菊苣酸的性质,扩大了与杂质成分的结构差异,从而使测定更准确,同时用红外和紫外光谱辅助解释了可能的配位机理和配位点。A chromatographic method was developed for the determination of cichoric acid in echinacea purpurea plant. The interference of other impurity can be removed and the degree of separation can be improved by adding 8 mmol/L silver nitrate into the mobile phase （ acetonitrile： water = 38：62 with a total of 0. 8% acetic acid）. The analytical column was a Restek Pinnacle 11 C18 （250 mm× 4.6 mm, 5 μm）. The flow rate was 0.5 mL/min. The detection wavelength was 326 nm. The injection volume was 10 L. The linear range of the method was 8 to 40 mg/L with r 〉0.99 for cichoric acid. The RSD was less than 3.0% and the average recovery was 98, 5%. The existence of coordination between cichoric acid and Ag ＋ could change the natures and existence station of cichoric acid and enlarge the difference between cichoric acid and other impu- rities, The mechanism of coordination and possible coordination site was investigated by IR,UV. The method would serve as a basis of the determination of cichoric acid and provide a simple basis for more in-depth research and separation of cichoric acid.

关 键 词：配位 菊苣酸 银离子 高效液相色谱 红外光谱 紫外光谱 

分 类 号：TQ911[化学工程]