Separating and purifying method of camptothecin

Abstract

The invention relates to a separating and purifying method of camptothecin. The method comprises the following steps of: (1) adding a camptothecin mixture into a sodium hydroxide solution for a ring opening treatment; (2) sequentially adding a separating reagent and a separating solvent to the reaction solution in the step (1) and reacting for 2-3 hours at 40-80 DEG C; naturally cooling; and standing at -10-40 DEG C till compound crystals of the camptothecin with opened rings and the separating reagent for separation; and filtering to obtain a compound crystal crude product of the camptothecin and the separating reagent, wherein the separating reagent is guanidine hydrochloride, guanidine carbonate, guanidine sulfate or guanidine nitrate, and the separating solvent is methanol-water, ethanol-water or acetone-water; and (3) recrystallizing the compound crystal crude product of the open-ring and the separating reagent and filtering, and adding filter cakes into concentrated hydrochloric acid to be uniformly mixed; and then, carrying out suction-filtering, washing and drying to obtain the camptothecin. The method provided by the invention can be used for reasonably and efficiently separating the camptothecin, and provides great convenience for experimental and production works, and meanwhile avoids material and energy source wastes.

Description

technical field [0001] The invention relates to a method for separating and purifying camptothecin, which belongs to the technical field of chemical separation. Background technique [0002] Camptothecin (Camptothecin, CPT) is an alkaloid isolated from Camptotheca acuminata Dence. Camptothecin has significant curative effect on various malignant tumors such as head and neck cancer, gastric cancer, colon cancer, bladder cancer and leukemia. It is the only inhibitor of topoisomerase I found so far. Camptothecins are the second natural medicines with anticancer activity that have been approved for marketing after paclitaxel. [0003] [0004] Camptothecin structure [0005] The currently widely used methods for separating camptotheca alkaloids include recrystallization, chromatography and chromatography, macroporous adsorption resin extraction, polyamide separation and purification, high-speed countercurrent chromatography, supercritical fluid CO2 extraction, etc. The com...

AI Technical Summary

Problems solved by technology

The commonly used recrystallization method is to obtain the final product after repeated recrystallization of the crude product extracted by solvent or alkali. Although the recrystallization method is easy to operate, the purity is not high; the solvent consumption of the chromatography method is large, and the operation time is long. The loss of finished products in the process is large, resulting in low final yield; although high-speed countercurrent chromatography overcomes the irreversible adsorption consumption, the complex structure of the equipment is not suitable for large-scale production, and it is difficult to choose a suitable solvent system, which directly affects the purity of the finished product; supercritical The fluid CO2 extraction method removes volatile oils, esters and other components in camptotheca, but only reduces the impurities in the crude extraction, and cannot subdivide the various components of camptotheca alkaloids

In general, the traditional extraction and separation method of camptotheca alkaloids has large solvent consumption, complex operation process, long duration, low extraction purity and high production cost

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