Method for preparing desoxy-podophyllotoxin

Abstract

The invention discloses a method for preparing desoxy-podophyllotoxin, which comprises the following steps of: 1) smashing radix podophylli raw material into middlings, quenching and percolating or extracting in a backflow way to obtain radix podophylli extract liquid; 2) concentrating the radix podophylli extract liquid obtained by the step 1) to obtain the concentration liquid of the radix podophylli extract liquid, evenly mixing with silica gel, drying, grinding, and filling into a chromatographic column, wherein the chromatographic column is filled with blank silica gel for column chromatography; and 3) eluting the chromatographic column with eluent, taking effluent liquid, the volume of which is equal to that of blank silica gel in the chromatographic column, as one fraction, collecting desoxy-podophyllotoxin-containing fraction, removing the eluent in the desoxy-podophyllotoxin-containing fraction, dissolving residue with dichloromethane or trichloromethane, and recrystallizing to obtain the desoxy-podophyllotoxin. The purity of the desoxy-podophyllotoxin obtained by the method is more than 70%, so that the method is suitable for not only laboratory preparation in small scale but also industrial preparation in large scale.

Description

technical field [0001] The invention belongs to the field of raw material medicine preparation and relates to a method for preparing deoxypodophyllotoxin. Background technique [0002] Deoxypodophyllotoxin is a highly toxic plant component that can be used to produce anticancer drugs or biopesticides. At present, no high-purity deoxypodophyllotoxin has been sold. The deoxypodophyllotoxin used by the authors of all literature reports is self-supplied by the researchers. The preparation methods are all self-explored, and the laboratory is prepared in a small amount. The preparation method is relatively complicated and reported. The content is brief and difficult to reproduce. In addition, the production cost is relatively high, which is not conducive to large-scale production. Liu Fa et al. (Liu Fa, Shang Tianmin, Fu Yongfeng, Research on the Chemical Constituents of Huaguijiu, Acta Pharmaceutica Sinica, 1979, 14(4): 241-145) used an alumina column (diameter-to-height ratio o...

AI Technical Summary

Problems solved by technology

At present, no high-purity deoxypodophyllotoxin has been sold. The deoxypodophyllotoxin used by the authors of all literature reports is self-supplied by the researchers. The preparation methods are all self-explored, and the laboratory is prepared in a small amount. The preparation method is relatively complicated and reported. The content is simple and difficult to reproduce. In addition, the production cost is high, which is not conducive to large-scale production

Liu Fa et al. (Liu Fa, Shang Tianmin, Fu Yongfeng, Research on the Chemical Constituents of Huaguijiu, Acta Pharmaceutica Sinica, 1979, 14(4): 241-145) used an alumina column (diameter-to-height ratio of 1:25) from Huagui Deoxypodophyllotoxin was prepared by separating and preparing deoxypodophyllotoxin in mortar, and the eluent was benzene-ethanol. This method not only has a large diameter-to-height ratio, and a long elution period, but also uses benzene, a highly toxic organic solvent; Jiang Zihua et al. Jiang Zihua, Chen Sixing. The chemical constituents of the Sichuan star anise lotus [J]. Yunnan Botanical Research, 1989, 11 (4): 479-481) using multiple silica gel column chromatography and recrystallization method to separate and prepare the deoxygenated Podophyllotoxin, the literature does not report the amount of silica gel, diameter-height ratio, column chromatography times and eluent composition. The main disadvantage of this method is that it needs to go through silica gel column chromatography for many times, the preparation period is long, and the production cost is high; Shang Mingying et al. (Shang Mingying, Li Jun, Cai Shaoqing, et al., Study on the Chemical Constituents of Tibetan Medicinal Lily chinensis, Chinese Herbal Medicine, 2000, 31(8): 569-571) used silica gel column chromatography with gradient elution of petroleum ether-ethyl acetate , through repeated refining (i.e. multiple times of silica gel column chromatography), deoxypodophyllotoxin was isolated and prepared from Lily chinensis, the amount of silica gel, diameter-height ratio, refining times and eluent ratio were not reported in the literature, the main points of this method The disadvantage is that it needs to go through silica gel column chromatography for many times, the preparation cycle is long and the production cost is high

[0003] The conventional method of separating and preparing compounds with a silica gel column is to use a silica gel column with a diameter-to-height ratio greater than 1:10. The amount of blank silica gel is large, reaching more than 30 times the amount of the extract (edited by Shanghai Institute of Materia Medica, Chinese Academy of Sciences. Extraction of active ingredients in Chinese herbal medicines) and Separation (Second Edition). Shanghai Science and Technology Press, 1983: 90-95), for the medicinal material of Auranthus chinensis (also known as Auranthus chinensis), the extraction rate of the medicinal material is 5% to 15%. , the amount converted into conventional silica gel should be 150% to 450% of the medicinal materials, and it needs to be refined on the column many times, which has the disadvantages of long production cycle, large amount of solvent, and high product cost.

Images