Method for enrichment of n-3 polyunsaturated fatty acid glyceride from fish oil
A technology for unsaturated fatty acids and fatty acid glycerides, which is applied in the separation/purification of carboxylic acid compounds, organic chemistry, fermentation, etc., can solve problems such as esterification and enrichment, achieve good food safety, and is conducive to human digestion and absorption. The effect of good medical and health care
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Embodiment 1
[0022] Accurately weigh 10 g of the refined fish oil sample, add 150 mL of 2mol / L NaOH aqueous ethanol solution, the ethanol / water ratio (v / v) is 6:1, protect with nitrogen, saponify at 50 °C for 60 min, add 100 mL of n-hexane to extract the unsaponified The hydrated layer was acidified with 100 mL of 3mol / L HCl, and then the free n-3PUFA hydrolyzed was extracted with 100 mL of n-hexane × 3, washed with water until neutral, and passed through anhydrous Na 2 SO 4 , N 2 The solvent is blown dry to obtain n-3PUFA, the hydrolysis rate of fish oil is 95.5% by chemical hydrolysis, the yield of EPA is 92%, and the yield of DHA is 90%.
[0023] 2 g of the n-3PUFA mixed solution containing EPA and DHA obtained after the hydrolysis of the fish oil was subjected to chromatographic separation on a C18 column, the mobile phase was methanol / water, 70-100% methanol gradient elution was performed, and the eluent was collected by sections, using Mass spectrometry quickly analyzes the chromat...
Embodiment 2
[0026] Accurately weigh 10g of the refined fish oil sample, add 150mL of 2mol / L NaOH ethanol aqueous solution, the ethanol / water ratio (v / v) is 9:1, nitrogen protection, saponify at 60°C for 90min, add 100mL of n-hexane to extract unsaponified The hydrated layer was acidified with 100 mL of 3 mol / L HCl, and then the free n-3PUFA hydrolyzed by n-hexane was extracted with 100 mL × 3 of n-hexane, washed with water until neutral, and passed through anhydrous Na 2 SO 4 , N 2 The n-3PUFA is obtained by drying the solvent, the hydrolysis rate of fish oil is 92% by chemical hydrolysis, the yield of EPA is 90%, and the yield of DHA is 88%.
[0027] 2 g of the n-3PUFA mixed solution containing EPA and DHA obtained after the hydrolysis of the fish oil was subjected to chromatographic separation on a C18 column, the mobile phase was methanol / water, 70-100% methanol gradient elution was performed, and the eluent was collected by sections, using The chromatographic samples were quickly an...
Embodiment 3
[0030] Accurately weigh 10 g of the refined fish oil sample, add 150 mL of 2mol / L NaOH aqueous ethanol solution, the ethanol / water ratio (v / v) is 9:1, fill with nitrogen for protection, saponify at 50 ° C for 90 min, add 100 mL of n-hexane to extract the unsaponified The hydrated layer was acidified with 100 mL of 3mol / L HCl, and then the free n-3PUFA hydrolyzed was extracted with 100 mL of n-hexane × 3, washed with water until neutral, and passed through anhydrous Na 2 SO 4 , N 2 The solvent is dried to obtain n-3PUFA, the hydrolysis rate of fish oil is 94% by chemical hydrolysis, the yield of EPA is 91%, and the yield of DHA is 89%.
[0031] 2 g of the n-3PUFA mixed solution containing EPA and DHA obtained after the hydrolysis of the fish oil was subjected to chromatographic separation on a C18 column, the mobile phase was methanol / water, 70-100% methanol gradient elution was performed, and the eluent was collected by sections, using The chromatographic samples were quickl...
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