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Quality control method for embelin

A quality control method, the technology of anthracene, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of low extraction purity, high production cost and low yield of anthracene, so as to improve market competitiveness and production The effect of short cycle time and fast separation speed

Active Publication Date: 2017-08-18
GUANGXI INST OF CHINESE MEDICINE & PHARMA SCI
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Problems solved by technology

[0006] The purpose of the present invention is to overcome the disadvantages of low extraction purity, low yield or high production cost of anthracene, as well as the non-systematic extraction, purification and quality control methods of anthracene, and to provide a preparation method and method for high-purity anthracene Its quality control method, the anthrabesine prepared by this method has high purity and good quality, and can be used as a chemical reference substance or standard substance, and the quality control method is effective, stable and uniform

Method used

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  • Quality control method for embelin
  • Quality control method for embelin
  • Quality control method for embelin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Embodiment 1: the preparation of high-purity anthrabeline

[0048] Take the ripe and dried fruit of Saccharomyces vine, add ether to extract 3 times, each time the amount of ether added is 8 times the weight of the medicinal material, and the extraction time is 2 hours each time, the extracts are combined, filtered, and the filtrate is concentrated to obtain an extract, which is adsorbed by a silica gel column and used Petroleum ether-ethyl acetate (0: 100-90:10) gradient elution, the eluted fraction containing anthrabezine was collected and concentrated to obtain crude crystals of anthrabezine.

[0049] The crude crystals were prepared by preparative RP-HPLC (chromatographic column: C-18 column; mobile phase: methanol:water volume ratio of 87:13; detection wavelength was 290nm; flow rate was 5ml / min), and the collected purity was 90 %-98% and the eluate with a purity greater than 98% was concentrated under reduced pressure to obtain anthrabeline with a purity between 9...

Embodiment 2

[0051] Embodiment 2: the preparation of high-purity anthrabeline

[0052] Take the mature fruit of Saccharomyces vines, add ether to extract twice, each time the amount of ether added is 10 times the weight of the medicinal material, each time the extraction time is 3 hours, filter, combine the filtrates, concentrate to obtain the extract, the extract is adsorbed by a silica gel column, Use petroleum ether-ethyl acetate (0: 100 to 85:15) gradient elution, collect the eluted fraction containing anthracenbeline, and concentrate to obtain crude crystals of anthracenebeline.

[0053] The crude crystals were prepared by preparative RP-HPLC (chromatographic column: C-18 column; the mobile phase methanol:water volume ratio was 80:20; the detection wavelength was 290nm; the flow rate was 5ml / min), and the collected purity was 90% The eluate between -98% and purity greater than 98% was concentrated under reduced pressure to obtain anthrabeline with a purity between 90%-98% and greater ...

Embodiment 3

[0055] Embodiment 3: the preparation of high-purity anthrabeline

[0056] Take the ripe and dried fruit of Saccharomyces vines, add ether to extract 8 times, add ether twice the weight of the medicinal material each time, and extract for 1 hour each time, filter, combine the filtrates, concentrate to obtain extract, the extract is adsorbed by silica gel column, Gradient elution with petroleum ether-ethyl acetate (0: 100 to 80:20) was used to collect the eluted fractions containing anthracenebecin and concentrate to obtain crude crystals of anthraceneberine.

[0057] Detected by HPLC, collected the fractions containing anthracene, combined and concentrated to obtain crude crystals of anthracene. The crude crystals were prepared by preparative RP-HPLC (chromatographic column: C-18 column; the mobile phase methanol:water volume ratio was 90:10; the detection wavelength was 290nm; the flow rate was 5ml / min), and the collected purity was 90% The eluate between -98% and purity grea...

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Abstract

The invention discloses a quality control method for embelin, and particularly discloses a method for extracting high-purity embelin from mature dried fruits of embelia laeta (Linn.) Mez (Embelia laeta (Linn.)Mez) as raw materials and detecting the embelin. The method comprises the processes of extracting taken embelia laeta plant, extracting dried fruits of the embelia laeta as the raw materials by using diethyl ether, separating through a column chromatography on silica gel, detecting a product by using TLC, combining, collecting a fraction containing the embelin and separating by adopting a reversed-phase preparative high performance liquid chromatography; and detecting each part of collected eluent by using an analytical high performance liquid chromatography, combining and reserving high-purity embelin components, and carrying out quality control by adopting a thin-layer chromatography and a liquid chromatography. According to the method, the purity of the embelin can be improved and the production cost can be reduced.

Description

technical field [0001] The invention relates to the field of a method for quality control of medicinal material chemical reference substances, in particular to a method for extracting and quality control of anthrabesin. Background technique [0002] Anthracene is a diterpene glycoside chemical component, one of the active components of plants, and an index component for standard quality control of many plants and pharmaceuticals. At present, there is no corresponding national drug standard substance, and there is no report on the systematic research on anthrabexine reference substances at home and abroad. Referring to the technical requirements of traditional Chinese medicine chemical reference substances (for content determination), the anthrabeline chemical reference substances are studied and established. The batch extraction process, purity and content, and the analysis and determination method of impurity inspection of anthrabexine chemical reference substances, so as t...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/94
CPCG01N30/02G01N30/94
Inventor 刘布鸣韦宝伟黄艳曾宪彪柴玲冯军谭小青
Owner GUANGXI INST OF CHINESE MEDICINE & PHARMA SCI
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