School of Pharmaceutical Sciences, Sun Yat-sen University, Guangzhou, China.
Nansha Research Institute, Sun Yat-sen University, Guangzhou, China.
J Sep Sci. 2018 May;41(9):2092-2101. doi: 10.1002/jssc.201701423. Epub 2018 Feb 27.
The objective of this study was to develop a consecutive preparation method for the isolation and purification of hainanmurpanin, meranzin, and phebalosin from leaves of Murraya exotica L. The process involved supercritical fluid extraction with CO , solvent extraction, and two-step high-speed countercurrent chromatography. Pressure, temperature, and the volume of entrainer were optimized as 27 MPa, 52°C, and 60 mL by response surface methodology in supercritical fluid extraction with CO , and the yield of the crude extracts was 7.91 g from 100 g of leaves. Subsequently, 80% methanol/water was used to extract and condense the three compounds from the crude extracts, and 4.23 g of methanol/water extracts was obtained. Then, a two-step high-speed countercurrent chromatography procedure was developed for the isolation of the three target compounds from methanol/water extracts, including conventional high-speed countercurrent chromatography for further enrichment and consecutive high-speed countercurrent chromatography for purification. The yield of concentrates from high-speed countercurrent chromatography was 2.50 g from 4.23 g of methanol/water extracts. Finally, the consecutive high-speed countercurrent chromatography produced 103.2 mg of hainanmurpanin, 244.7 mg of meranzin, and 255.4 mg of phebalosin with purities up to 97.66, 99.36, and 98.64%, respectively, from 900 mg of high-speed countercurrent chromatography concentrates in one run of three consecutive sample loadings without exchanging a solvent system.
本研究的目的是从九里香（Murraya exotica L.）叶中连续制备分离和纯化海南蒲桃新宁素、密苏里花椒素和仙鹤草酚醇。该过程包括超临界 CO2 萃取、溶剂萃取和两步高速逆流色谱。通过响应面法优化超临界 CO2 萃取的压力、温度和夹带剂体积分别为 27 MPa、52°C 和 60 mL，从 100 g 叶中获得粗提物的产率为 7.91 g。然后，用 80%甲醇/水从粗提物中提取和浓缩这三种化合物，得到 4.23 g 甲醇/水提取物。然后，开发了两步高速逆流色谱法从甲醇/水提取物中分离这三种目标化合物，包括常规高速逆流色谱进一步富集和连续高速逆流色谱纯化。从高速逆流色谱中浓缩物的产率为 2.50 g，从 4.23 g 甲醇/水提取物中得到。最后，连续高速逆流色谱从 900 mg 高速逆流色谱浓缩物中一次连续三个样品负荷运行，无需更换溶剂系统，分别得到 103.2 mg 海南蒲桃新宁素、244.7 mg 密苏里花椒素和 255.4 mg 仙鹤草酚醇，纯度均达到 97.66%、99.36%和 98.64%。
