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Method for separating chemical components of pine needles

A separation method and technology for chemical components, which can be used in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., and can solve the problems of long cycle, difficult industrial production, and poor repeatability.

Active Publication Date: 2017-08-11
CHENGDU KANGHONG PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the separation method of monomer chemical components in pine needles is mainly extraction and separation from plant raw materials. The separation means involved are based on silica gel and gel column chromatography. The purity of monomer compounds prepared by these traditional methods is low, and the steps cumbersome, long cycle, poor repeatability, difficult to apply to industrial production

Method used

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  • Method for separating chemical components of pine needles
  • Method for separating chemical components of pine needles
  • Method for separating chemical components of pine needles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] The preparation of embodiment one pine leaf extract

[0040] Fresh pine leaves, add ZNTD-50 extraction and concentration unit, add water to decoct twice, add 8 times the amount of water for the first time, decoct for 1.5 hours, add 6 times the amount of water for the second time, decoct for 1.5 hours; the filtrate is concentrated under reduced pressure Form the extract whose relative density is 1.2 at 70°C; spray dry to obtain.

Embodiment 2

[0041] Example 2 Traditional phytochemical separation method to prepare pine needle compound

[0042] (1) Preparation of test solution

[0043] Take 1200g of pine leaf extract, extract with ethyl acetate and water-saturated n-butanol successively to obtain ethyl acetate extraction extract, water-saturated n-butanol extraction extract and the remaining extract from the water layer, and the numbers are Pr.1~ 3. Time-consuming 5d.

[0044] (3) Rough classification

[0045] Take Pr.2 (water-saturated n-butanol extract), absorb it with macroporous resin D101, elute with 3 times the column volume of water, then separate through SBC MCI gel, and elute with 3 times the column volume of 30% ethanol to obtain Pr. .2A1, separated by eluting with 3 times column volume of 40% ethanol to obtain Pr.2A2. Time consuming 3d.

[0046] Take Pr.2A2 (40% ethanol eluent) and pass through Sephadex G25 column, eluted with 3 times column volume of water to obtain 3 parts Pr.2A2A, Pr.2A2B, and Pr.2...

Embodiment 3

[0059] The preparation of embodiment three pine needle compounds

[0060] (1) Preparation of test solution

[0061] Weigh 35g of pine leaf extract, add 500mL methanol in two times, sonicate for 1 hour each time, let it stand for precipitation, take the supernatant, evaporate in vacuum at 60°C, freeze-dry after concentration, and dissolve the dried product in 40mL supernatant Pure water, through 0.45μm filter membrane, that is. It takes 9 hours.

[0062] (2) One-dimensional preparative liquid phase separation

[0063] Instrument: Waters purification factory, chromatographic column: XAqua C18 (250mm×20mm×10μm), each injection volume is 8mL. Use water (aqueous phase) containing 0.1% formic acid and methanol (organic phase) containing 0.1% formic acid as the mobile phase for gradient elution, the elution conditions are 0-35min, 25%-60% organic phase, 35-36min , 60%-95% organic phase, 36-55min, 95%-95% organic phase, the flow rate is 20mL / min, and the detection wavelength is 28...

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Abstract

The invention relates to a method for separating chemical components of pine needles. The chemical components comprise birch glucoside and massonianoside C; the method is characterized by comprising steps as follows: preparation of a test solution, separation, purification, secondary separation and the like. With the adoption of the separation method, the use amount of an organic solvent is reduced, the solvent is easy to recycle, and the method is simple and easy to popularize.

Description

technical field [0001] The invention relates to the field of medicinal chemistry, in particular to a method for separating chemical components of pine leaves. Background technique [0002] Pine leaves (pine needles) are the most important by-products of Pinaceae (Pinaceae) plants, and are the representative part of Pinus medicinal. Pinaceae plants in my country mainly include Pinus massoniana, Pinus tabulaeformis, Pinus chinensis, Pinus sylvestris, Pinus slashes, etc. Among them, Pinus massoniana is the most important pine plant in southern my country. Nearly a hundred years of research has found that pine needle extract has a series of pharmacological activities such as analgesia, anti-inflammation, sedation, antitussive, expectorant, asthma, blood lipid lowering, anti-oxidation, anti-aging, anti-mutation, anti-tumor, etc. Due to its resources Rich and diverse effects have caused scholars to conduct in-depth research on the chemical components of pine needles. In recent y...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/18C07H15/26C07H1/08
CPCC07H1/08C07H15/18C07H15/26
Inventor 柯潇叶亮张秀莉梁鑫淼赵曼茜
Owner CHENGDU KANGHONG PHARM CO LTD
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