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目的:优选Zn2+沉淀法纯化丹酚酸B的工艺条件。方法:采用HPLC测定丹酚酸B含量,色谱条件为流动相乙腈-0.05%磷酸溶液梯度洗脱,柱温30℃,检测波长286 nm,进样量10μL。以丹酚酸B提取率为指标,通过单因素试验优选提取工艺;以丹酚酸B转移率为指标,通过单因素试验考察碱液种类、ZnCl2用量、盐酸摩尔浓度及pH对Zn2+沉淀法纯化工艺的影响。结果:优选的丹酚酸B提取、纯化工艺为加6倍量pH 2～3盐酸溶液温浸3次,每次1 h,加1%Na2CO3溶液调pH6.0～6.5,加30%药材质量的ZnCl2,用2 mol·L-1盐酸溶液溶解,调pH 2～3,加等倍量乙酸乙酯萃取2次,减压低温干燥,丹酚酸B得率3.47%,纯度达80%。结论:优选的纯化工艺稳定可行,可避免长时间高温和pH对丹酚酸B的破坏。
OBJECTIVE: To optimize the process conditions of salvianolic acid B by Zn2 + precipitation. Methods: The content of salvianolic acid B was determined by HPLC. The mobile phase consisted of gradient elution with acetonitrile - 0.05% phosphoric acid solution. The column temperature was 30 ℃, the detection wavelength was 286 nm and the injection volume was 10 μL. The extraction rate of salvianolic acid B was taken as an index, and the extraction process was optimized by single factor test. The salvianolic acid B transfer rate was used as an index to investigate the types of lye, the amount of ZnCl2, the molar concentration of hydrochloric acid and the pH of Zn2 + The impact of technology. Results: The optimal salvianolic acid B extraction and purification process was adding 6 times pH 2 ~ 3 hydrochloric acid solution to soak for 3 times, 1 hour each time, adding 1% Na2CO3 solution to adjust pH6.0 ~ 6.5, adding 30% medicinal material quality Of ZnCl2 was dissolved in 2 mol·L-1 hydrochloric acid, adjusted to pH 2-3, extracted twice with ethyl acetate and dried under reduced pressure at low temperature. The yield of salvianolic acid B was 3.47% and the purity was 80%. Conclusion: The preferred purification process is stable and feasible, which can avoid the destruction of salvianolic acid B under prolonged temperature and pH.