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Method for preparing high-purity conjugated linoleate by using simulated moving bed

A technology of conjugated linoleate and conjugated ethyl linoleate, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, and can solve problems such as the inability to prepare pure products

Active Publication Date: 2019-09-20
THE FIRST INST OF OCEANOGRAPHY SOA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional separation and preparation methods, such as urea inclusion method and lipase catalysis, cannot prepare products with a purity of more than 95%.

Method used

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  • Method for preparing high-purity conjugated linoleate by using simulated moving bed
  • Method for preparing high-purity conjugated linoleate by using simulated moving bed
  • Method for preparing high-purity conjugated linoleate by using simulated moving bed

Examples

Experimental program
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Effect test

preparation example Construction

[0020] (1) Preparation of the raw material solution, dissolving the low-purity conjugated ethyl linoleate raw material in methanol (or ethanol) to prepare a raw material solution.

[0021] (2) The eluent can be ethanol / water, methanol / water, acetonitrile / water, etc., preferably methanol / water (80:20W / W).

[0022] (3) The raw material liquid and eluent are continuously flowed into the simulated moving bed chromatography system, which is a four-zone simulated moving bed, with two chromatographic columns arranged in each zone, and the two chromatographic columns are both C18 silica gel columns, or C8 silica gel The chromatographic column and C18 silica gel are connected in series, the product is taken out from the extraction port, and the impurities are flowed out from the raffinate port. Set an appropriate switching time for separation and purification, see the specific process flow figure 2 .

[0023] The purified conjugated ethyl linoleate was determined by gas chromatograp...

Embodiment 1

[0025] The preparation method of high-purity conjugated ethyl linoleate comprises the following steps:

[0026] For the preparation of the raw material injection solution, ethyl conjugated linoleate with a purity of 80.15% was dissolved in methanol to prepare a 25 mg / mL solution.

[0027] The eluent was methanol / water (80:20W / W).

[0028] The raw material liquid and eluent flow into the simulated moving bed chromatographic system continuously. The system is a four-zone simulated moving bed. Two chromatographic columns are arranged in each zone, and the two chromatographic columns are C18 silica gel chromatographic columns. The product is taken out from the extraction port, and Impurities flow out from the raffinate port. Set the switching time for 5 minutes, and the flow rate in the I-IV area is 3.8mL / min, 3.2mL / min, 3.5mL / min and 2.8mL / min in sequence for separation and purification.

[0029] Utilize gas chromatography to measure the content of conjugated ethyl linoleate af...

Embodiment 2

[0031] The preparation method of high-purity conjugated ethyl linoleate comprises the following steps:

[0032] For the preparation of the raw material injection solution, ethyl conjugated linoleate with a purity of 80.15% was dissolved in methanol to prepare a 25 mg / mL solution.

[0033] The eluent was methanol / water (80:20W / W).

[0034] The raw material liquid and the eluent are continuously flowed into the simulated moving bed chromatography system. The system is a four-zone simulated moving bed, and two chromatographic columns are arranged in each zone. The two chromatographic columns are a C8 silica gel column and a C18 silica gel in series. The product is taken out from the extraction port (Extract), while the impurities flow out from the raffinate port (Raffinate). Set the switching time to 5.2min, and the flow rate in the I-IV area is 3.6mL / min, 3.1mL / min, 3.3mL / min and 2.5mL / min in sequence, for separation and purification.

[0035] Utilize gas chromatography to mea...

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Abstract

The invention discloses a method for preparing high-purity conjugated linoleate by using a simulated moving bed. A conjugated ethyl linoleate is selected as a raw material; the stationary phase is selected from C8 and C18 silica gel; and the mobile phase is ethanol / water, methanol / water and acetonitrile / water. The method comprises the following steps: preparation of a raw material liquid sample injection liquid: dissolving low-purity conjugated ethyl linoleate in methanol to prepare a raw material solution, the eluent being methanol / water; continuously feeding raw material liquid and eluent into a simulated moving bed chromatographic system, herein, the system is a four-zone simulated moving bed, each zone is formed by connecting two or more chromatographic columns in series, and the chromatographic columns are filled with C18 silica gel, and withdrawing a product from an extraction opening, and meanwhile impurities flow out from a raffinate opening. The method has the beneficial effect that the raw material with the conjugated ethyl linoleate content of 80% is purified into a high-purity product with the content of 97% or above.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and relates to a method for large-scale preparation of high-purity conjugated linoleic acid ester by using a simulated moving bed. Background technique [0002] Conjugated linoleic acid (CLA for short) is an isomer of linoleic acid, generally refers to conjugated linoleic acid with unsaturated double bonds at carbon 9 and 11 or carbon 10 and 12, and theoretically has four isomers isomers, but generally c9, t11-CLA and t10, c12-CLA are the two most abundant isomers. CLA is a natural regulator of lipid and carbohydrate metabolism. It participates in the lipid and carbohydrate metabolism of organisms, improves the imbalanced lipid-sugar balance, and plays an important role in balancing fat cells and blood sugar. Studies have shown that CLA has a good preventive effect on obesity, hyperlipidemia and other diseases due to its unique weight loss and lipid-lowering effect. At present, CLA ha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/56C07C69/587
CPCC07C67/56C07C69/587
Inventor 郑洲缪锦来曲长凤
Owner THE FIRST INST OF OCEANOGRAPHY SOA
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