豆豉姜中生物碱的pH区带逆流色谱分离研究

建立pH区带逆流色谱分离制备豆豉姜中生物碱的方法。运用pH区带逆流色谱对豆豉姜中的生物碱进行分离,以氯仿-甲醇-水(4:3:2,V/V)作为溶剂系统,在上相溶液中加入70 mmol/L盐酸作为固定相,在下相溶液中加入10 mmol/L三乙胺作为流动相,仪器转速为800 r/min,流速为2 m L/min,检测波长为254 nm,固定相保留率为65%。经一次pH区带逆流色谱分离,从1.5 g豆豉姜粗提物中得到波尔定246 mg,六驳碱524 mg和异波尔定317 mg。经HPLC分析,其纯度分别为97.35%,95.48%,97.54%。研究结果表明,pH区带逆流色谱能对豆豉姜中的主要活性成分(阿朴啡型生物碱)进行有效的分离制备。

Separation and purification of alkaloids from Litsea cubeba (Lour.)Pers.by pH-zone-refining counter-current chromatography

We construct a method for separating and purifying alkaloids from Litsea cubeba(Lour．) Pers.by pH zone refining counter current chromatography (CCC).Our experimental conditions are solvent of chloroform methanol water(4:3:2,V/V),upper stationary phase of 70 mmol/L HCl, lower mobile phase of 10 mmol/L TEA, revolution speed of 800 r/min, flow rate of 2 mL/min, detection wavelength of 254 nm, and stationary phase retention rate of 65%.We acquire 246 mg of boldine, 524 mg of laurotetanine and 317 mg of isoboldine from 1.5 g crude extract of Litsea cubeba(Lour．) Pers.through one time pH zone refining CCC.Their purities are 97.35%, 95.48% and 97.54% by HPLC analysis.Results show that pH zone refining CCC can effectively separate and prepare major active components of Litsea cubeba(Lour．) Pers.,aporphine alkaloids.