Method for separating and purifying lecithin through fixed-bed adsorption method

A fixed-bed adsorption, separation and purification technology, applied in the direction of selective adsorption, edible phospholipid composition, ion exchange, etc., can solve the problems of difficult regeneration of adsorbents, large equipment investment, and low concentration, and achieve low energy consumption and simplified solvent recovery. The effect of simple process and operation process

Active Publication Date: 2013-08-21
ZHEJIANG UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0005] Chinese patent ZL200510026994.5 discloses a process for preparing phosphatidylcholine by high-shear leaching with ethanol as a solvent. The content of phosphatidylcholine is only 55%. Low
Chinese patent ZL201110054014.8 discloses a method for preparing soybean lecithin by adsorption method, using soybean lecithin as raw material, C1-C4 alcohol as solvent, adding adsorbent, stirring and adsorbing, then filtering, and the filtrate is desolvated under reduced pressure and vacuum-dried After that, soybean lecithin products containing more than 80% of phosphatidylcholine can be obtained, and the yield can reach more than 85%. The intermittent stirring tank adsorption operation needs to put in fresh adsorbent many times to achieve the target purity, and the consumption of adsorbent is large. , and the adsorbent needs to be removed by plate and frame filtration or centrifugal filtration, the recovered adsorbent is difficult to regenerate, and the production cost is high
[0008] There is not much room for solvent extraction to improve the purity of phosphatidylcholine. It is generally used for the crude extraction of phospholipids, that is, the extraction of total phospholipids; with supercritical carbon dioxide as the extraction solvent, its purity can reach 90%, but the polarity of supercritical carbon dioxide is relatively high. Weak, its dissolving ability to the stronger phosphatidylcholine of polarity is poor, is unfavorable for the separation of each phospholipid, and supercritical fluid extraction operation condition is harsh, and equipment investment is big; Components still have considerable difficulty, and it is necessary to develop a membrane with specific selective functions to obtain high-purity phosphatidylcholine; column chromatography (also known as column chromatography) is indeed the current method to obtain high-purity phosphatidylcholine Choline is a more effective method, but due to the low utilization rate of chromatographic stationary phase in batch operation of chromatography, its inherent defects lead to large solvent consumption, dilute product concentration collected by peak cutting, high energy consumption for solvent recovery, and high requirements for self-control in the operation process
[0009] In the prior art, silica gel or alumina is used as the chromatographic stationary phase, and the amount of ocean is limited each time, the processing capacity is small, and the concentration of the fraction collected after sample injection is very low, and the energy consumption of evaporating the solvent to recover the product is high; Stirred tank type adsorption consumes a lot of adsorbent, and the regeneration of the adsorbent is difficult, and the operation process is also intermittent operation, non-continuous operation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Put the macroporous weakly basic adsorption resin D303 with an average particle size of about 0.4mm into an adsorption column with a size of Φ2cm×25cm, and the column bed volume (abbreviated as BV) is about 76ml. The raw material solution for loading samples was prepared by dissolving soybean powder phospholipids (40% phosphatidylcholine content) in 95% ethanol to prepare a 25 mg / mL raw material solution. Continuously feed 15BV of powdered phospholipid raw material solution at a flow rate of 2BV / hr. When the adsorption column reaches the maximum adsorption performance, the sample loading is stopped, and the effluent is collected. After HPLC analysis, the content of phosphatidylcholine can reach 89.4%, and the yield is 85.3%. Then concentrated by vacuum distillation to obtain phosphatidylcholine product.

[0047] Rinse the adsorption column with 1BV of 95% ethanol to collect the eluate. The collected eluate contains phosphatidylcholine, which can be recycled as the colu...

Embodiment 2

[0049] Put the macroporous weakly basic adsorption resin D303 with an average particle size of about 0.4mm into an adsorption column with a size of Φ2cm×25cm, and the column bed volume (abbreviated as BV) is about 76ml. The raw material solution for loading samples was prepared by dissolving soybean powder phospholipids (60% phosphatidylcholine content) in 95% ethanol to prepare a 50 mg / mL raw material solution. Continuously feed 12BV of powdered phospholipid raw material solution at a flow rate of 3BV / hr. When the adsorption column reaches the maximum adsorption performance, the sample loading is stopped, the effluent is collected, and analyzed by HPLC, the content of phosphatidylcholine in it can reach 87.6%, and the yield is 82.1%. Then concentrated by vacuum distillation to obtain phosphatidylcholine product.

[0050] Rinse the adsorption column with 1BV of 95% ethanol to collect the eluate. The collected eluate contains phosphatidylcholine, which can be recycled as the c...

Embodiment 3

[0052] Put the macroporous weakly basic adsorption resin D303 with an average particle size of about 0.4mm into an adsorption column with a size of Φ2cm×25cm, and the column bed volume (abbreviated as BV) is about 76ml. The raw material solution for loading samples was prepared by dissolving soybean powder phospholipids (60% phosphatidylcholine content) in 95% ethanol to prepare a 100 mg / mL raw material solution. Continuously feed 6BV of powdered phospholipid raw material solution at a flow rate of 0.5BV / hr. When the adsorption column reaches the maximum adsorption performance, stop loading the sample, collect the effluent, and analyze by HPLC, the content of phosphatidylcholine in it can reach 86.5%, and the yield is 80.1%. Then concentrated by vacuum distillation to obtain phosphatidylcholine product.

[0053] Rinse the adsorption column with 1BV of 95% ethanol to collect the eluate. The collected eluate contains phosphatidylcholine, which can be recycled as the column mate...

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Abstract

The invention discloses a method for separating and purifying lecithin through a fixed-bed adsorption method. The method comprises the following steps of: dissolving a phosphatidylcholine raw material in a solvent to prepare a raw material liquid, enabling the raw material liquid to continuously pass through an adsorption column filled with an adsorbent to ensure that impurities in the raw material liquid are preferentially adsorbed, collecting an effluent liquid at an outlet of the adsorption column, enabling the effluent liquid to be subjected to reduced pressure distillation and concentration and obtaining a phosphatidylcholine product, wherein the impurities are cephalin, phosphatidylserine and sphingomyelin. The method disclosed by the invention has the advantages that by adopting a continuous feeding mode, the main impurities such as the cephalin, the phosphatidylserine, the sphingomyelin and the like in the phosphatidylcholine raw material liquid can be removed through a single adsorption operation, so that the process flow of purifying the phosphatidylcholine is greatly simplified and the phosphatidylcholine yield is increased.

Description

technical field [0001] The invention relates to the technical field of adsorption separation, in particular to a method for separating and purifying lecithin by a fixed-bed adsorption method. Background technique [0002] Lecithin is an important basic substance of life, and its chemical name is Phosphatidylcholine (Phosphatidyl Choline referred to as PC). Phosphatidylcholine is an important component of the cell membrane, which can repair the membrane damage caused by free radicals attacking biological macromolecules; it has a choline component, and choline has an affinity for fat, allowing fat to pass through the blood from the liver in the form of phospholipids It is transported out to prevent the formation of fatty liver; it is the precursor substance that provides the neurotransmitter acetylcholine, has brain-building functions, and is also used in the research of liposomes and as anticancer drugs. [0003] It is treated as a high-level nutrient in Europe, America and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/10B01D15/08
Inventor 任其龙苏宝根闻光东陈丽芬鲍宗必杨启炜邢华斌张治国杨亦文苏云
Owner ZHEJIANG UNIV
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