离子液体作为流动相添加剂高效液相色谱法同时测定黄连中5种生物碱

Determination of five alkaloids in Huanglian by high performance liquid chromatography using 1-hexyl-3-methylimidazolium tetrafluoroborate as the mobile phase additives

建立了高效液相色谱法(HPLC)同时测定黄连中5种生物碱含量的方法。黄连药材经甲醇超声提取后,用Spherigel C_(18)色谱柱(250×4.6 mm,5μm)进行HPLC测定,流动相为含有1-己基-3-甲基咪唑四氟硼酸盐添加剂的甲醇-水(25:75,V/V),流动相流速为1.0 m L/min,检测波长为345 nm,同时测定了黄连药材中药根碱、表小檗碱、黄连碱、巴马汀和小檗碱含量。在1~200μg/m L浓度范围内,5种生物碱的线性相关系数均大于0.9990,药根碱、表小檗碱、黄连碱、巴马汀和小檗碱的检测限(LOD)分别为0.19,0.13,0.11,0.18,0.15 mg/L。测定了3种不同产地的黄连生物碱的含量并进行加标回收,回收率在98%~102%之间。

A sensitive, selective method was developed for determination of alkaloids of Huanglian by high performance liquid chromatography （HPLC）. Huanglian samples were extracted with methanol under sonication and analyzed by HPLC using a Spherigel C18 column. The mobile phases were methanol-water （25：75, V/V） with 1-hexyl-3-methylimidazolium tetrafluoroborate as the mobile phase additives. The flow-rate of the mobile phase was 1.0 mL/min and the effluent was monitored at 345 nm. Five alkaloids including jatrorrhizine, epiberberine, coptisine, palmatine and berberine were determined simultaneously. The correlation coefficients were all better than 0. 9990 over the concentration range of 1-200 p.g/mL. For jatrorrhizine, epiberberine, coptisine, palmatine and berberine, the limits of detection （LODs） were 0. 19, 0. 13, 0. 11, 0. 18 and 0. 15 mg/L, respectively. The proposed method had been successfully applied to the determination of the content of alkaloids of Huanglian from three different producing areas. The recovery of this method was in the range of 98% - 102%.