Process for preparing and separating methyl docosapentaenoate and methyl docosahexenoate
A kind of technology of methyl docosahexaenoate and methyl docosahexaenoate, applied in the field of preparation and separation of methyl docosahexaenoate and methyl docosahexaenoate , which can solve the problems of complicated brine shrimp meal process and lower yield, and achieve the effect of short heating time, avoided loss and high yield.
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[0025] [Example 1]
[0026] The preparation of high-purity docosapentaenoic acid (DPA) methyl ester and docosahexaenoic acid (DHA) methyl ester by the silver nitrate column method includes the following steps:
[0027] 1) Preparation of crude fatty acid: Take 500g of microalgae oil, 50g of KOH, and 1000ml of methanol, add it to a three-necked flask, use nitrogen as protective gas, keep stirring, and reflux in a water bath at 60-120°C for 1 to 4 hours. After removing most of the solvent by rotary evaporation, 6mol / L hydrochloric acid was added for acidification, and the fatty acid was extracted three times with 300ml petroleum ether, and then 5% NaCl aqueous solution was added to wash the ether phase until the washing liquid was neutral. Add anhydrous Na 2 SO 4 Absorb the residual moisture in the ether phase, and spin-evaporate at 60°C to remove the solvent to obtain crude fatty acid.
[0028] 2) Preparation of DPA and DHA mixed fatty acid: Take 100g crude fatty acid, 30g~300g urea...
Example Embodiment
[0031] [Example 2]
[0032] The basic process is the same as in Example 1, and the specific operating parameters are as follows:
[0033] 1) Preparation of crude fatty acid: Take 250g of seaweed oil, 50g of KOH, and 500ml of methanol, add it to a three-necked flask, use nitrogen as protective gas, keep stirring, and reflux in a water bath at 60-120°C for 2 hours. After removing most of the solvent by rotary evaporation, 6mol / L hydrochloric acid was added for acidification, the fatty acid was extracted three times with 300ml petroleum ether, and the ether phase was washed with 5% NaCl aqueous solution until the washing liquid was neutral. Add anhydrous Na 2 SO 4 Absorb the residual moisture in the ether phase, and spin-evaporate at 60°C to remove the solvent to obtain crude fatty acid.
[0034] 2) Preparation of DPA and DHA mixed fatty acid: Take 75g crude fatty acid, 150g urea, 600ml methanol and mix, reflux in a water bath at 50-80°C for 15 minutes, cool and crystallize at -10°C ...
Example Embodiment
[0037] [Example 3]
[0038] The basic process is the same as in Example 1, and the specific operating parameters are as follows:
[0039] 1) The preparation of crude fatty acid, the preparation of DPA and DHA mixed fatty acid and the methyl esterification of DPA and DHA mixture are the same as in Example 2.
[0040] 2) Silver nitrate column method to obtain DPA methyl ester and DHA methyl ester: Prepare Ag according to the method in Example 1. + Silica gel, weighing out 100g Ag + Silica gel, wet packed column with n-hexane as eluent. Take 0.5 g of the mixture of DPA methyl ester and DHA methyl ester and load the sample. Elute with 2000ml of 0.5% acetone in n-hexane solution, 500ml of 10% acetone in n-hexane solution, and 1000ml of 15% acetone in n-hexane solution, each 60ml as a sample, evaporate and remove the solvent, detect by gas chromatography, combine the same group Separately, high-purity DPA methyl ester and DHA methyl ester can be obtained.
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