Method for preparing high-purity chlorogenic acid by taking lonicera plants as raw materials

A technology of chlorogenic acid and honeysuckle, applied in the field of medicine and chemical industry, can solve the problems of large amount of organic solvent, high purification cost, time-consuming and laborious, etc., and achieve the effect of simple operation, wide sources and simple equipment requirements

Inactive Publication Date: 2018-08-24
NANKAI UNIV
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Problems solved by technology

[0013] The purpose of the present invention is to solve the problem of time-consuming and labor-intensive column separation methods such as macroporous resin method, cyclodextrin-bonded gel medium method, high-speed countercurrent chromatography and polyamide column chromatography in the separation and purification process of chlorogenic acid, and the purification cost is high. Problems such as large amount of organic solvents

Method used

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  • Method for preparing high-purity chlorogenic acid by taking lonicera plants as raw materials
  • Method for preparing high-purity chlorogenic acid by taking lonicera plants as raw materials
  • Method for preparing high-purity chlorogenic acid by taking lonicera plants as raw materials

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Embodiment 1

[0036] Embodiment 1. Investigation and implementation of supercritical carbon dioxide extraction process

[0037] Due to the instability of chlorogenic acid, high temperature, strong light and long-term heating cannot be used during extraction, so supercritical fluid extraction is an ideal method. The present invention takes the extraction rate of chlorogenic acid as an index, utilizes the orthogonal test method and the response surface design method to optimize the process conditions of supercritical fluid extraction, and takes the Lonicera japonica Thunb. planted in Julu County, Hebei Province The branches and leaves of the plant were used as raw materials, dried at 50°C for 12 hours, pulverized with a high-speed pulverizer, and passed through a 20-mesh sieve. The content of chlorogenic acid was measured by HPLC method, instrument: Shimadzu high performance liquid chromatography LC-15C, equipped with binary pump, SPD-15C ultraviolet detector, CTO-15C column thermostat, LC-So...

Embodiment 2

[0051] Example 2. Extraction of Chlorogenic Acid in Flos Lonicerae by Ultrasonic Method

[0052] Take the stem and leaf of Lonicera hypoglauca Miq. produced in Xincheng County, Guangxi as the raw material of Lonicera hypoglauca Miq. As raw material, get its powder 10g, add 70% ethanol solution of 1:30 (W / V) volume ratio, Ultrasonic power is 300W, ultrasonic frequency is 60KHz, ultrasonic extraction is 30 minutes, after filtration, depressurization is concentrated to obtain chlorogenic acid extract 1.95g, and adopt the HPLC method in the above-mentioned embodiment 1 to detect wherein the chlorogenic acid content can reach 5.9% .

Embodiment 3

[0053] Embodiment 3. The investigation of alkali removal and purification process

[0054] Take 0.76 g of the chlorogenic acid extraction extract obtained by the ultrasonic method in the above-mentioned Example 2, add 30 mL of deionized water, and ultrasonically dissolve it fully for 30 minutes. Repeated extraction was carried out with one volume of ethyl acetate respectively until the ethyl acetate layer was colorless and clear (5 times in total). Take the water layer, divide it into 6 parts on average, adjust the pH to 6~11 with NaOH respectively, let it settle for 3 hours, then centrifuge at 3000rpm for 10 minutes, and dry and weigh the obtained insoluble precipitate to investigate the efficiency of alkali removal. The result is as Figure 5 As shown, it is confirmed that the optimum pH of the alkali removal process is 10.

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Abstract

The invention discloses a method for preparing high-purity chlorogenic acid by taking lonicera plants as raw materials. The method is technically characterized by using overground parts, including buds, flowers, leaves and stems, of the lonicera plants, i.e., honeysuckle flower and flos lonicerae confuse as the raw materials, and extracting chlorogenic acid in the lonicera plants by adopting a supercritical extraction or ultrasonic wave extraction technology. Cleaning is performed by means of ethyl acetate extraction and alkalization precipitation, and then the chlorogenic acid in an extractive is enriched by acidified extraction, so that the purity of the chlorogenic acid can reach 50 percent or above. High-purity chlorogenic acid crystals can be further directly separated out by concentration and crystallization. The method has the advantages of wide source of the raw materials, simple operation, and capability of obtaining a high-purity chlorogenic acid product without operation processes, such as resin adsorption and column chromatography preparation, in traditional chlorogenic acid extraction and refining processes, and has wide industrialized application value.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and relates to a method for purifying and preparing high-purity chlorogenic acid using Lonicera plants as raw materials. Background technique [0002] Honeysuckle (Lonicera japonica Thunb.) is the dry flower bud of Lonicera japonica Lonicera. The theory of traditional Chinese medicine believes that honeysuckle is cold in nature and sweet in taste, and enters the lungs, heart, stomach and other meridians. and tumors. Mountain silver flower is Lonicera macranthoides Hand.-Mazz., Lonicera fulvotomentosa Hsu etS.C.Cheng, Lonicera hypoglauca Miq., Lonicera confuse DC .) of dried flower buds. The two kinds of Yinhua belong to the same genus and different species of easily mixed Chinese medicinal materials. Since the 2005 edition of the Pharmacopoeia, honeysuckle and mountain silver flower have been treated separately, but the descriptions of the properties, flavors, meridians,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/48C07C69/732
CPCC07C67/48C07C2601/14C07C69/732Y02P20/54
Inventor 白钢侯媛媛王彦帅
Owner NANKAI UNIV
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