目的 开发丹参Salviae Miltiorrhizae Radix et Rhizoma标准提取物的制备工艺，并建立其质量控制方法。方法 采用层次分析法（analytic hierarchy process，AHP）结合L₉(3⁴)正交试验，以总丹酚酸、总丹参酮、总多糖提取率和出膏率为参考指标，开发丹参标准提取物的制备工艺；利用HPLC法、紫外-可见分光光度法（UV-Vis）对15批丹参提取物进行定性和定量分析，建立丹参标准提取物质量控制方法。结果 丹参标准提取物最佳制备工艺为丹参饮片加10倍量80%乙醇水回流提取3次，每次1 h，药渣再加9倍量超纯水回流提取3次，每次1.5 h，合并滤液，冷冻干燥后即得。15批丹参标准提取物HPLC指纹图谱中有16个共有峰，对其中12个共有峰进行了指认，相似度评价均大于0.830；其中丹参素、原儿茶醛、咖啡酸、丹酚酸E、迷迭香酸、紫草酸、丹酚酸A、丹酚酸B 8种成分的总质量分数为2.87%～16.06%，二氢丹参酮I、隐丹参酮、丹参酮I、丹参酮II_A 4种成分的总质量分数为0.17%～1.09%，总多糖质量分数为2.04%～3.17%；多糖相对分子质量分布明显分为高、中、低3个部分，分别为3.94×10⁵～4.50×10⁵、6.69×10³～2.00×10⁴和1.20×10³～1.28×10³。结论 开发的先乙醇提取再用水提取的制备工艺可有效提取丹参中的丹酚酸类、丹参酮类和多糖类成分；建立的丹参标准提取物质量控制方法稳定、可靠，可用于丹参提取物的质量控制。

Objective To develop a preparation process of standard extract from Danshen (Salviae Miltiorrhizae Radix et Rhizoma, SMRR) (SMRR-SE) and establish its quality control method. Methods The extraction rates of total salvianolic acids, tanshinones and polysaccharides and extraction rate of solid substances were used as evaluation indicators, and the analytic hierarchy process (AHP) combined with L₉(3⁴) orthogonal experiment was used to develop the preparation process of SMRR-SE. Fifteen batches of SMRR extracts were analyzed qualitatively and quantitatively by HPLC and ultraviolet-visible spectrophotometry (UV-Vis) to establish the quality control method for SMRR-SE. Results The optimal preparation process of SMRR-SE was as follow: the SMRR decoction pieces were extracted with 10 volumes of 80% aqueous ethanol under reflux for 1 h for three times; then, the residue was further extracted with nine volumes of purified water for 1.5 h for three times. The combined filtrates were lyophilized to obtain the SMRR-SE. The HPLC fingerprints of fifteen batches of SMRR-SE were established with 16 common peaks including 12 identified ones, and the inter-batch similarities were all greater than 0.830. The content of eight compounds, including danshensu, protocatechuic aldehyde, caffeic acid, salvianolic acid E, rosmarinic acid, lithospermic acid, salvianolic acid A and salvianolic acid B ranged from 2.87% to 16.06%, that of four compounds, including dihydrotanshinone I, cryptotanshinone, tanshinone I, and tanshinone II_A, ranged from 0.17% to 1.09%, and that of the total polysaccharides ranged from 2.04% to 3.17%. The molecular weight distribution of polysaccharides in most of SMRR-SEwas clearly divided into high, medium and low parts, with distributions ranging from 3.94×10⁵—4.50×10⁵, 6.69×10³—2.00×10⁴, and 1.20×10³—1.28×10³, respectively. Conclusion The developed preparation process with successive extraction using aqueous ethanol and ultrapure water can efficiently extract salvianolic acids, tanshinones and polysaccharides from SMRR. The established quality control method for SMRR-SE is stable and reliable, which can be used for the quality control of SMRR extract.

R283.6

国家重点基础研究发展计划项目（2022YFC3501704）