Novel method for preparing salidroside from glossy privet fruit

A technology of salidroside and Ligustrum lucidum, applied in the field of medicine, to achieve the effects of cost saving, simple separation and purification method, and high product yield

Inactive Publication Date: 2012-01-18
石任兵
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there is no method involving the preparation of high-purity salidroside on the basis of greatly increasing the content of salidroside in Ligustrum lucidum through transformation

Method used

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  • Novel method for preparing salidroside from glossy privet fruit
  • Novel method for preparing salidroside from glossy privet fruit
  • Novel method for preparing salidroside from glossy privet fruit

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Ligustrum lucidum crude powder is extracted with 10 times the volume of 75% ethanol, reflux extraction 3 times, each time for 1 hour, the extract is concentrated until it has no alcohol smell, dispersed with water 10 times the amount of crude drug, and then 4000 rpm Centrifuge at high speed for 30 minutes, discard the precipitate after centrifugation to make up the volume, which is the supernatant.

[0049] The amount of alkali added to the supernatant is the amount of crude drug: NaOH (g:g) with a ratio of 10:1, heated to reflux for extraction for 2 hours, and the conversion solution is adjusted to neutrality by adding HCl. It is the sample solution.

[0050] After the gained sample solution is diluted to 0.05g / mL (equivalent to the crude drug), the HPD-100 type macroporous resin with a volume ratio of (equivalent to the gram of crude drug) and resin of 1:2 is loaded as a sample, and the resin diameter-to-height ratio is 1:11, for dynamic adsorption, the adsorption fl...

Embodiment 2

[0056] Ligustrum lucidum crude powder is extracted with 10 times the volume of 80% ethanol, reflux extraction twice, each time for 1 hour, the extract is concentrated until it has no alcohol smell, dispersed with water 10 times the amount of the crude drug, and then 4000 rpm Centrifuge at high speed for 30 minutes, discard the precipitate after centrifugation to make up the volume, which is the supernatant.

[0057] The amount of alkali added to the supernatant is the amount of crude drug: NaOH (g:g) of 12:1 NaOH, heated to reflux for extraction for 1.5 hours, and the conversion solution is adjusted to neutrality by adding HCl. It is the sample solution.

[0058] After the gained sample solution is diluted to 0.1g / mL (equivalent to the crude drug), the HPD-100 type macroporous resin with a resin volume ratio of 1: 1.5 (equivalent to the gram of crude drug) is loaded as a sample, and the resin diameter-to-height ratio is 1:14, for dynamic adsorption, the adsorption flow rate i...

Embodiment 3

[0064] Ligustrum lucidum crude powder is extracted with 15 times the volume of 50% ethanol, reflux extraction 3 times, each time for 1 hour, the extract is concentrated until it has no alcohol smell, dispersed with water 10 times the amount of the crude drug, and then 4000 rpm Centrifuge at high speed for 30 minutes, discard the precipitate after centrifugation to make up the volume, which is the supernatant.

[0065] The amount of alkali added to the supernatant is the amount of crude drug: NaOH (g:g) is 8:1 NaOH, heated to reflux for extraction for 2.5 hours, and the conversion solution is adjusted to neutrality by adding HCl. It is the sample solution.

[0066] After the gained sample solution is diluted to 0.067g / mL (equivalent to the crude drug), the HPD-100 type macroporous resin with a resin volume ratio of 1: 2.5 is loaded on (equivalent to the gram of crude drug), and the diameter-to-height ratio of the resin is 1:8, for dynamic adsorption, the adsorption flow rate i...

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Abstract

The invention discloses a novel method for separating and preparing salidroside from glossy privet fruit, which comprises the following steps: heating the medicinal material glossy privet fruit with ethanol under reflux to obtain an extracting solution; recycling the extracting solution under reduced pressure until no alcohol smell is emitted; centrifugalizing, carrying out alkaline hydrolysis on the supernatant, adding acid to regulate the solution to neutral state, carrying out primary separation with macroporous adsorbent resin, and separating by silica gel column chromatography to obtain a crude salidroside product; and purifying the crude product by a solvent method or column chromatography to obtain the white acicular crystals of salidroside. The determination on the salidroside by high efficiency liquid chromatography indicates that the purity is higher than 98%.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a method for separating high-purity salidroside from Chinese medicinal material Ligustrum lucidum on the basis of alkali transformation. Background technique [0002] Salidroside, English name salidroside, chemical name "p-hydroxyphenyl alcohol-β-D-glucopyranoside". The molecular formula is: C 14 h 20 o 7 , the molecular weight is 300.30. [0003] Structural formula: [0004] [0005] Salidroside has anti-fatigue, anti-aging, anti-oxidation, anti-inflammatory and analgesic effects; it has protective effects on cardiovascular, central nervous system, liver and kidney; it also has anti-tumor, anti-radiation, scavenging free radicals, immune regulation effects, etc. , is a drug with broad application prospects. At present, the main methods for preparing salidroside include extraction, separation and chemical synthesis from Rhodiola rosea. However, rhodiola belongs to platea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/18C07H1/08
Inventor 石任兵姜艳艳李娟
Owner 石任兵
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