区带逆流色谱法分离纯化丹参中的丹酚酸B和迷迭香酸

采用pH区带精制逆流色谱技术(pH-ZRCCC)快速分离纯化丹参中的丹酚酸B和迷迭香酸?以乙酸乙酯-水(1∶1,V/V)为溶剂体系,上相加入三氟乙酸,使浓度达到10 mmol/L,作为固定相;下相加入氨水使浓度达到20 mmol/L,作为流动相;设置主机转速为850 r/min,流速为2.0 mL/min,检测波长为280 nm,对样品进行分离制备?从500 mg丹参粗提物中一次分离得到386 mg丹酚酸B以及25 mg迷迭香酸,经HPLC分析纯度分别为96.3%和98.1%,各化合物通过电喷雾电离(ESI)谱和¹H-NMR进行了化学结构鉴定?研究结果表明,pH-ZRCCC是一种快速?高效分离纯化丹酚酸B和迷迭香酸的方法

Separation and purification of salvianolic acid B and rosmarinic acid from Salvia miltiorrhiza Bge. by pH-zone-refining counter-current#br# chromatography

We rapidly separated and purified salvianolic acid B and rosmarinic acid from Salvia miltiorrhiza Bge. By pH zone refining counter current chromatography ( pH-ZRCCC) . The extraction conditions included solvent system of ethyl acetate water ( 1∶1, V/ V) , upper stationary phase of 10 mmol/ L trifluoroacetic acid, lower mobile phase of 20 mmol/ L NH ₃ H ₂ O, rotation speed of 850 r/ min, flow speed of 2. 0 mL/ min, and detection wavelength of 280 nm. Salvianolic acid B of 386 mg and rosmarinic acid of 25 mg were extractedfrom crude extract of 500 mg, whose purities were 96. 3% and 98.1% through HPLC analysis. Their compound structures were identified by ESI MS and 1 H NMR. Experimental results show that pH ZRCCC is a rapid and efficient method to separate and purify salvianolic acid B and rosmarinic acid.