应用化学

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黄连黄柏提取液中3种生物碱的原位生成离子液体微萃取及HPLC测定

曹玺珉*,吴昊,张晋,刘霞,杜黎明   

  1. (山西师范大学分析测试中心 临汾 041004)
  • 收稿日期:2013-06-17 修回日期:2013-08-16 出版日期:2013-12-10 发布日期:2013-12-10
  • 通讯作者: 曹玺珉,副教授; Tel:0357-2051157; Fax:0357-2051158; E-mail:lwzcxm@sina.com; 研究方向:色谱和光谱分析
  • 基金资助:
    国家自然科学基金(31171167)山西省自然科学基金(2009011044-1)资助项目

HPLC Determination of Three Alkaloids in Rhizoma coptidis and Cortex phellodend Microextracted with in situ Formed Ionic Liquids

CAO Ximin*, WU Hao, ZHANG Jin, LIU Xia, DU Liming   

  1. (Analytical and Testing Center,Shanxi Normal University,Linfen 041004,China)
  • Received:2013-06-17 Revised:2013-08-16 Online:2013-12-10 Published:2013-12-10

摘要: 通过加入水溶性离子液体[C6MIM][Br]和离子对试剂NaPF6在黄连和黄柏的提取液中,原位生成非水溶性离子液体[C6MIM][PF6]萃取其生物碱,离心分相后,用HPLC测离子液体相中的生物碱小檗碱、巴马汀和黄连碱,其线性相关系数分别为0.9998、0.9996和0.9997,线性范围为1~2000 μg/L,检出限皆为0.5 μg/L,加标回收率96.52%~104.34%。 这种方法可用于黄连和黄柏中的小檗碱、巴马汀和黄连碱的检测。

关键词: 生物碱, 离子液体, 原位溶剂生成微萃取, 高效液相色谱

Abstract: NaPF6 (as an ion-pairing agent) was added to the extraction solution of Rhizoma coptidis and Cortex phellodend containing [C6MIM][Br](as hydrophilic ionic liquid(IL)). A cloudy solution formed as a result of the formation of fine droplets of [C6MIM][PF6]. After centrifugation, the sedimented phase enriched with alkaloids was analyzed by HPLC with UV detection. In this method, several important parameters, such as the type and volume of ILs, the amount of NaPF6, solution pH, extraction time and centrifugation time, influencing the extraction efficiency of IL-ISFME(in situ solvent formation microextraction) were optimized. Under optimal conditions, berberine, palmatine and coptisine exhibit good linearity, with correlation coefficients of 0.9998, 0.9996 and 0.9997, respectively, a linear range of 1~2000 μg/L and the detection limit of 0.5 μg/L. The spiked recovery for each analyte is in the range of 96.52%~104.34%. The experimental results indicate that the proposed method is successfully applied to the analysis of three alkaloids in Rhizoma coptidis and Cortex phellodend.

Key words: alkaloids, ionic liquid, in situ solvent formation microextraction, high performance liquid chromatography

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