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Preparative isolation and purification of hainanmurpanin, meranzin, and phebalosin from leaves of Murraya exotica L. using supercritical fluid extraction combined with consecutive high‐speed countercurrent chromatography
Journal of Separation Science ( IF 2.8 ) Pub Date : 2018-02-27 , DOI: 10.1002/jssc.201701423 Rongwei Yan 1 , Jie Shen 1 , Xiaojing Liu 2 , Yong Zou 1, 3 , Xinjun Xu 1, 3
Journal of Separation Science ( IF 2.8 ) Pub Date : 2018-02-27 , DOI: 10.1002/jssc.201701423 Rongwei Yan 1 , Jie Shen 1 , Xiaojing Liu 2 , Yong Zou 1, 3 , Xinjun Xu 1, 3
Affiliation
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 CO2, 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 CO2, 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.
中文翻译:
超临界流体萃取-连续高速逆流色谱法从穆拉亚叶中制备海南紫花pan素,黑色素和酞菁蛋白的分离纯化
本研究的目的是开发一种用于从叶分离和hainanmurpanin,meranzin的纯化和phebalosin连续制备方法九里香L.该过程涉及超临界流体萃取的CO 2,溶剂萃取,和两步高快速逆流色谱。在CO 2超临界流体萃取中,通过响应表面方法将压力,温度和夹带剂的体积优化为27 MPa,52°C和60 mL,从100克树叶中提取的粗提物的产量为7.91克。随后,使用80%的甲醇/水从粗提取物中提取和浓缩三种化合物,得到4.23g的甲醇/水提取物。然后,开发了一种两步高速逆流色谱方法,用于从甲醇/水提取物中分离出三种目标化合物,包括常规的高速逆流色谱以进一步富集,以及连续的高速逆流色谱以进行纯化。高速逆流色谱法从4.23 g甲醇/水提取物中得到的浓缩物产量为2.50 g。最后,连续的高速逆流色谱法产生的纯净度高达97.66,产生了103.2 mg hainanmurpanin,244.7 mg melanzin和255.4 mg phebalosin,
更新日期:2018-02-27
中文翻译:
超临界流体萃取-连续高速逆流色谱法从穆拉亚叶中制备海南紫花pan素,黑色素和酞菁蛋白的分离纯化
本研究的目的是开发一种用于从叶分离和hainanmurpanin,meranzin的纯化和phebalosin连续制备方法九里香L.该过程涉及超临界流体萃取的CO 2,溶剂萃取,和两步高快速逆流色谱。在CO 2超临界流体萃取中,通过响应表面方法将压力,温度和夹带剂的体积优化为27 MPa,52°C和60 mL,从100克树叶中提取的粗提物的产量为7.91克。随后,使用80%的甲醇/水从粗提取物中提取和浓缩三种化合物,得到4.23g的甲醇/水提取物。然后,开发了一种两步高速逆流色谱方法,用于从甲醇/水提取物中分离出三种目标化合物,包括常规的高速逆流色谱以进一步富集,以及连续的高速逆流色谱以进行纯化。高速逆流色谱法从4.23 g甲醇/水提取物中得到的浓缩物产量为2.50 g。最后,连续的高速逆流色谱法产生的纯净度高达97.66,产生了103.2 mg hainanmurpanin,244.7 mg melanzin和255.4 mg phebalosin,