Method for removing diglyceride in medium-and-long-chain-structure ester

A technology of diglyceride and medium-long chain, which is applied in the field of removal of medium-long chain structural ester diglyceride, can solve the problems of complex process, impracticality, and poor separation effect, and achieve simple process, low cost, Strong adsorption effect

Inactive Publication Date: 2018-04-24
GUANGZHOU HANFANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, separation and purification of diglycerides commonly include molecular distillation, silica gel column chromatography, and florisil adsorption fractionation. Separation and removal of diglycerides from esters to obtain the target product of medium and long-chain structure triglycerides with high purity, the process is complicated and the separation effect is not good, so it is not practical

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] According to the ratio of medium and long-chain structure ester raw materials to alumina as 1:5, weigh about 250kg of alumina to dry-pack the chromatography column; take 50kg of medium- and long-chain structure ester raw materials for elution on the column, and first use n-hexane-ether ( 9:1), the elution rate is 0.3L / min, and the elution is 3 column volumes, and then 2 column volumes are eluted with n-hexane-ether (19:1), the elution rate is 0.3L / min. The two eluted fractions were collected and combined with the column eluted fraction of the sample, concentrated under reduced pressure at 60°C to evaporate the solvent, dried in vacuum at 80°C to constant weight, weighed, sealed with a parafilm, and stored in the dark. The removal rate of diglycerides detected by high performance liquid chromatography was 99.3%, and the recovery rate of medium and long-chain structural esters was 91.2%.

Embodiment 2

[0022] According to the ratio of medium and long-chain structure ester raw materials to alumina as 1:3, weigh about 150kg of alumina to dry-pack the chromatography column; take 50kg of medium- and long-chain structure ester raw materials for elution on the column, and first use n-hexane-ether ( 19:1), the elution rate is 0.2L / min, 5 column volumes are eluted, and then 1 column volume is eluted with n-hexane-ether (29:1), the elution rate is 0.2L / min. The two eluted fractions were collected and combined with the column eluted fraction of the sample, concentrated under reduced pressure at 60°C to evaporate the solvent, dried in vacuum at 80°C to constant weight, weighed, sealed with a parafilm, and stored in the dark. The removal rate of diglycerides detected by high performance liquid chromatography was 97.0%, and the recovery rate of medium and long-chain structural esters was 89.9%.

Embodiment 3

[0024] According to the ratio of medium and long-chain structure ester raw materials to alumina as 1:5, weigh about 250kg of alumina to dry-pack the chromatography column; take 50kg of medium- and long-chain structure ester raw materials for elution on the column, and first use n-hexane-ether ( 9:1), the elution rate is 0.3L / min, and the elution is 3 column volumes, and then 2 column volumes are eluted with n-hexane-ether (19:1), the elution rate is 0.3L / min. The two eluted fractions were collected and combined with the column eluted fraction of the sample, concentrated under reduced pressure at 60°C to evaporate the solvent, dried in vacuum at 80°C to constant weight, weighed, sealed with a parafilm, and stored in the dark. The removal rate of diglycerides detected by high performance liquid chromatography was 99.1%, and the recovery rate of medium and long-chain structural esters was 91.4%.

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Abstract

The invention discloses a method for removing diglyceride in medium-and-long-chain-structure ester. The method includes following steps: taking alumina to fill a chromatographic column through a dry process, and taking medium-and-long-chain-structure ester raw material to load the chromatographic column, wherein a mass ratio of the medium-and-long-chain-structure ester raw material to alumina is 1:3-10; using normal hexane-ethyl ether for elution, and collecting elution fraction, wherein a volume ratio of normal hexane to ethyl ether is 19-4:1; using normal hexane-ethyl ether for elution, andcollecting elution fraction, wherein a volume ratio of normal hexane to ethyl ether is 29-14:1; combining the elution fraction with sample column-loading elution fraction, depressurizing for concentration to dryness, vacuum drying, weighing, using a sealing film for sealing, and storing at a dark place. The method realizes effect of removing diglyceride through one-step adsorption and is simple inprocess, low in cost and high in purity of obtained products; alumina has higher adsorption ability and better adsorption effect on two isomesides of diglyceride, and the problem that diglyceride adsorbed by silica gel can be desorbed by fraction with higher polarity in the medium-and-long-chain-structure ester is solved effectively.

Description

technical field [0001] The invention belongs to the field of separation and purification of fats and oils, and in particular relates to a method for removing diglycerides of medium- and long-chain structural esters. Background technique [0002] Middle-chain triglycerides (MCT) refers to a class of triglycerides composed of fatty acids with a fatty acid carbon chain length between 8 and 10. It does not exist in nature. MCT was first used by Babayan to treat intestinal Synthesized for the purpose of disturbed absorption of nutrients. [0003] Long-chain triglycerides (LCT) refer to a type of oil with a fatty acid carbon chain length between 12 and 24 on the glycerol skeleton in triglycerides. It is generally found in terrestrial animal fats, vegetable oils and marine animal fats. Clinically and in the pharmaceutical industry, soybean oil and safflower oil are generally used as base oils for long carbon chain fats. At present, long carbon chain triglyceride fat emulsion is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C11B3/10C11B7/00B01D15/42
CPCB01D15/426C11B3/10C11B7/0058
Inventor 蔡鸿飞许文东江程唐顺之关伟键牟肖男李康强刘菊妍吴伟锋杨阳王小妹潘裕清李海波龙海林
Owner GUANGZHOU HANFANG PHARMA
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