Method for extracting and separating lupulone from lupulus

Abstract

The invention relates to a method for extracting and separating lupulone from lupulus. The method comprises the following specific steps: filling the compressed lupulus into a subcritical ultrasonic extractor, introducing an R134a mixed solvent into the extractor, dissolving the active ingredients of the extracted material in the R134a mixed solvent in a liquid state or a subcritical state, and pumping the filtrate into a separator; regulating the temperature and pressure so that R134a in the R134a mixed solvent is converted from liquid state into gas state, separating the R134a from the extracting solution, concentrating the methanol-containing extracting solution by virtue of a concentration evaporator so as to obtain the lupulus extract, and entering a crystallization section; adding a certain amount of lupulus extract into a reaction kettle, adding water, stirring, standing at room temperature, performing suction filtration, and collecting the insoluble substance; adding water to the insoluble substance, stirring, standing at room temperature, and performing suction filtration; and stirring and performing suction filtration, collecting the insoluble substance, thereby obtaining the crude lupulone. According to the method disclosed by the invention, a subcritical ultrasonic extraction technology is utilized, the R134a mixed solvent is taken as an extraction solvent, and the solvent can return to a high-purity state without being subjected to special treatment in production.

Description

technical field [0001] The invention relates to the field of lupulone separation, in particular to a method for extracting and separating lupulone from hops. Background technique [0002] Hops (Humulus lupulus L.) is the female inflorescence of hops, a perennial herb of the genus Humulus in the family Cannabisaceae. It is cultivated in Northeast my country, East China, Shandong, Shaanxi, Gansu and other places. The main active ingredients of hops are lupulone and humulone. Lupulone in hops has strong estrogen, and its role is mainly used to treat amenorrhea and dysmenorrhea in women, and can also be used to inhibit male indulgence. [0003] The existing technology for extracting and separating lupulone from hops is to extract hop compressed matter with 95% methanol (or ethanol) at 50°C for 2h at reflux, coarsely filter, and extract the residue with 95% methanol (or ethanol) for 2h, coarsely filter, and remove the residue Then extract with 95% methanol (or ethanol) for 2 h...

AI Technical Summary

Problems solved by technology

[0004] But in the extraction method in the prior art, must use 95% and above methyl alcohol (or ethanol) during solvent method extraction, otherwise have a strong impact on the separation of lupulone because of the many water-soluble impurities of extracting solution, therefore must utilize refined lupulone in production. Distillation tower is used to purify the concentration of methanol, which increases the production cost due to the loss of methanol

In order to maintain a high extraction rate, the extraction temperature must be kept at 80-85°C, otherwise the extraction rate will be greatly reduced, and the product will be easily damaged due to the high temperature

Due to the limitation of the operation of the extraction tank, the raw materials are not easy to be crushed too finely, otherwise the extraction liquid will be difficult to flow out, and the extraction rate will decrease because the raw materials cannot be crushed too finely

Supercritical CO 2 Due to the high pressure required for extraction by the traditional method, the equipment manufacturing requirements are strict, and the extraction volume is small, which seriously affects the large-scale production.

The acid-base adjustment is not easy to control during separation and purification, often resulting in incomplete removal of impurities and low crystallization purity