Method for simultaneously extracting three kinds of iridoid glycoside chemical reference substances from fructus ligustri lucidi

A technology of iridoid glycosides and Ligustrum lucidum, which is applied in the field of simultaneous extraction of three iridoid glycosides chemical reference substances from Ligustrum lucidum, which can solve the problems of cumbersome steps, long time consumption, and low utilization rate of medicinal materials. problems, to achieve the effect of simple and easy-to-obtain raw materials and high safety

Inactive Publication Date: 2016-02-17
DALIAN MEDICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] These existing methods have the following disadvantages: 1) only a single iridoid glycoside can be prepared, and the utilization rate of medicinal materials is too low; 2) a large amount of toxic organic solvents are used for extraction, normal phase silica gel column purification or recrystallization etc. are not conducive to large-scale production, and the preparation flux is small; 3) when preparing multi-component extracts, the steps are cumbersome, time-consuming, and the purity cannot be guaranteed

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  • Method for simultaneously extracting three kinds of iridoid glycoside chemical reference substances from fructus ligustri lucidi
  • Method for simultaneously extracting three kinds of iridoid glycoside chemical reference substances from fructus ligustri lucidi
  • Method for simultaneously extracting three kinds of iridoid glycoside chemical reference substances from fructus ligustri lucidi

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Embodiment 1

[0041] A method for simultaneously extracting three iridoid glycosides chemical reference substances from Ligustrum lucidum, comprising the following steps:

[0042] 1) Ligustrum lucidum total extract extract

[0043] Take 50g of Ligustrum lucidum medicinal material, pass through a 30-mesh sieve after being pulverized, heat and reflux extract with 150mL of 40% ethanol aqueous solution for 3 times, each time for 3 hours, combine three extracts, recover under reduced pressure, and obtain Ligustrum lucidum total extract Paste, about 22g.

[0044] 2) Extract the total glucosides of Ligustrum lucidum

[0045] Add about 20mL of water to disperse the total extract of Ligustrum lucidum, use HPD-100 macroporous resin column (45cm*4cm) for chromatographic separation, first elute with 2 times the column volume of water, and then use 3 times the column volume The ethanol solution with a concentration of 50% was used for elution, the eluate was collected, and the solvent was recovered un...

Embodiment 2

[0056] A method for simultaneously extracting three iridoid glycosides chemical reference substances from Ligustrum lucidum, comprising the following steps:

[0057] 1) Extraction of Ligustrum lucidum total extract

[0058] Take 500g of Ligustrum lucidum medicinal material, crush it and pass through a 50-mesh sieve, heat and reflux extraction with 1500mL of 50% ethanol aqueous solution for 2 times, each time for 3 hours, combine the two extracts, recover under reduced pressure, and obtain Ligustrum lucidum Total extract, about 195g.

[0059] 2) Extract the total glucosides of Ligustrum lucidum

[0060] Add about 200mL of water to disperse the total extract of Ligustrum lucidum, and carry out chromatographic separation with a Diaion macroporous resin column (90cm*8cm), first use 2 times of column volume for water elution, and then use 3 times of column volume for volume concentration of 40% ethanol aqueous solution was used for elution, the eluent was collected, and the solve...

Embodiment 3

[0067] A method for simultaneously extracting three iridoid glycosides chemical reference substances from Ligustrum lucidum, comprising the following steps:

[0068] 1) Extraction of Ligustrum lucidum total extract

[0069] Take 500g of Ligustrum lucidum medicinal material, crush it and pass through a 50-mesh sieve, heat and reflux extract once with 1500mL of 60% ethanol aqueous solution by volume concentration, extract for 3 hours, recover under reduced pressure, and obtain the total extract of Ligustrum lucidum, about 130g.

[0070] 2) Extract the total glucosides of Ligustrum lucidum

[0071] Add about 150mL of water to disperse the total extract of Ligustrum lucidum, use D101 macroporous resin column (90cm*8cm) to chromatographically separate, first use 2 times the column volume of water to elute, and then use 3 times the column volume to have a volume concentration of 60 % ethanol aqueous solution was eluted, the eluate was collected, and the solvent was recovered under ...

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Abstract

The invention discloses a method for simultaneously extracting three kinds of iridoid glycoside chemical reference substances from fructus ligustri lucidi. According to the method, extracting is performed with an ethyl alcohol aqueous solution to obtain a total fructus ligustri lucidi extract, chromatographic separation is performed with macroporous resin columns to obtain total fructus ligustri lucidi glycosides, the total fructus ligustri lucidi glycosides are purified and separated through inverse-phase efficient preparative liquid chromatography, and then the three kinds of the iridoid glycoside chemical reference substances including the specnuezhenide, the nuezhenoside G13 and the oil nuezhenoside of which the purity is larger than 98% are obtained. According to the method, the three kinds of the iridoid glycoside chemical reference substances of which the purity is up to 98% can be simultaneously obtained through simple treatment, and the problems that in the prior art, only one compound can be obtained, the steps are tedious, and the purity is low are solved.

Description

technical field [0001] The invention relates to a chemical reference substance for simultaneously extracting three iridoid glycosides from Ligustrum lucidum [0002] Methods. Background technique [0003] Ligustrum lucidum is the dried and mature fruit of Oleaceae plant Ligustrum lucidum Ait., which is a commonly used traditional Chinese medicine for strengthening the body and strengthening the body. , blindness, etc. Studies have shown that Ligustrum lucidum can promote osteoblast differentiation and resist osteoporosis caused by estrogen deficiency, regulate the balance of calcium ions in the body, and have anti-osteoporosis effects. [0004] The chemical components in Ligustrum lucidum mainly contain triterpenoids, iridoid glycosides, phenylethyl alcohol, phenylpropanoids, flavonoids, etc. Among them, the water-soluble active ingredient iridoid glycosides is one of the main medicinal ingredients in Ligustrum lucidum, rich in pharmacological activities, and has a wide r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08
CPCC07H1/08C07H17/04
Inventor 刘艳秋洪志来张晓哲
Owner DALIAN MEDICAL UNIVERSITY
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