Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for purifying and separating olefin bond containing active compound

A technology for active substances and olefinic bonds, applied in the field of purification of active substances containing olefinic bonds, can solve the problems of affecting separation efficiency, low separation efficiency, long separation consumption time, etc., and achieves a high degree of automation, high separation efficiency, and purification ability. strong effect

Inactive Publication Date: 2008-08-06
CHINESE ACAD OF INSPECTION & QUARANTINE
View PDF0 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this technology has many disadvantages: the impregnation of silver nitrate on the silica gel column is not uniform, which affects the separation efficiency; the column separation efficiency is not high under medium and normal pressure; the silver silica gel column is sensitive to light and can only be prepared immediately. The manual preparation process is complicated and tedious, and the reproducibility is poor; the separation takes a long time; the separation consumes a large amount of organic solvent
No patent literature reports related to silvery reversed-phase high-pressure liquid chromatography have been found after searching

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for purifying and separating olefin bond containing active compound
  • Method for purifying and separating olefin bond containing active compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1 Preparation of (2E, 4Z, 8Z, 10Z)-N-isobutyl dodecatetraenamide from Du Heng

[0018] (2E, 4Z, 8Z, 10Z)-N-isobutyl dodecatetraenamide exists in the medicinal plant Duheng, and has pharmacological activities such as antipyretic and analgesic. And (2E, 4E, 8Z, 10E)-N-isobutyl dodecatetraenamide are cis-trans isomers, which exist in Du Heng at the same time.

[0019] Dry the whole plant of Du Heng at 60°C for 20 minutes, crush it to 50 mesh, weigh 1 kg accurately, and extract it twice with n-hexane (2×2L) for 24 hours. Ethyl water (1:1) was used as the eluent to obtain the crude amide containing ethylenic bond. 1 / 10 of the sample was dissolved in 5 mL of methanol, and separated by silverized reversed-phase high-pressure liquid chromatography. It was completed on a Waters Delta Prep 4000 preparative high-pressure liquid chromatograph (996 photodiode array detector, Millennium 32 chromatography workstation). The chromatographic column adopts Japanese Shiseido C18...

Embodiment 2

[0022] Embodiment 2 prepares linoleic acid from soybean oil

[0023]Dissolve 100g of soybean oil in 200mL of n-hexane, and then use a silica gel chromatography column for rough separation, using n-hexane-ethyl acetate (1:1) as the eluent, and use gas chromatography to trace the crude component of linoleic acid. After extracting 50 mL of methanol, it was separated by silverization reversed-phase high-pressure liquid chromatography. It was completed on a WatersDelta Prep 4000 preparative high-pressure liquid chromatograph (996 photodiode array detector, Millennium 32 chromatography workstation). The chromatographic column adopts Japanese Shiseido C18 high-pressure preparation chromatographic column (250×25mm, 5μm); binary eluent, one phase is methanol, the other phase is 0.5% acetic acid solution and 0.3M silver ions are added, gradient elution Conditions: 30 minutes ramp from 40% methanol to 100% methanol, 20 minutes hold. The flow rate is 20mL / min, the detection wavelength i...

Embodiment 3

[0025] Embodiment 3 prepares pellitorine from asarum

[0026] Pheledine exists in the traditional Chinese medicine Asarum, and has pharmacological activities such as antipyretic and analgesic. The structure is (2E,4E)-N-isobutyl-2,4-decadienamide. Dry the root of asarum at a constant temperature of 60°C for 20min, crush it to 50 mesh, weigh 1kg accurately, and extract (2×2L) twice with n-hexane for 24h. Ethyl acetate (1:1) was used as the eluent, and the target components were tracked by gas chromatography to obtain crude components. Take 1 / 3 of the sample and dissolve it in 5 mL of methanol, and carry out silverization reversed-phase high-pressure liquid chromatography separation. It was completed on Waters DeltaPrep 4000 preparative high-pressure liquid chromatography (996 photodiode array detector, Millennium 32 chromatography workstation). The chromatographic column adopts Japanese Shiseido C18 high-pressure preparation chromatographic column (250 × 25mm, 5 μm); binary ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a method for separating high-purity ethylenic-linkage containing active compounds from oil and fat or natural drugs. The method comprises adding silver ions into an eluting agent; using a reverse-phase high-pressure liquid chromatography system to perform high-selectivity separation of ethylenic-linkage containing active compounds which are difficult to isolate; collecting target distillates to get high-purity target compounds. Employing an argentation eluting agent, which can adjust silver ion concentration on line according to the purifying difficulty of target compounds so as to regulate the separation and purification ability of the system, the method has the advantages of good controllability and high automation degree; using a common reverse-phase preparative chromatography column, the method is cost-effective and convenient; adopting the high-pressure liquid chromatography system, the method also has the advantages of strong purification ability, high separation efficiency, fast separation rate, low organic solvent consumption, excellent reproducibility, etc., and is applicable to preparation and purification of ethylenic-linkage containing active compounds in oil and fat or natural drugs.

Description

technical field [0001] The present invention relates to the purification of ethylenic bond-containing active substances, in particular to a high-purity ethylenic bond-containing active substance, especially unsaturated fatty acid, which is separated from oil or natural medicine by using silverized reversed-phase high-pressure liquid chromatography technology and its derivatives. Background technique [0002] Active substances containing ethylenic bonds widely exist in oils or natural medicines, and have health care and pharmacological activities on the human body. Unsaturated fatty acids such as oleic acid, linoleic acid, linolenic acid, and arachidonic acid in oils can significantly reduce high-density lipoprotein and serum cholesterol, thereby reducing the incidence of hypertension, heart disease, and stroke. It plays an important role in maintaining the structure and function of biofilm, and this type of product can be widely used in medicine, nutritional supplements, he...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07B63/00B01D15/36B01D15/32C07C51/47C07C231/24
Inventor 张峰储晓刚凌云雍炜李秀琴
Owner CHINESE ACAD OF INSPECTION & QUARANTINE
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com