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 promoting the development of marine economy
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Embodiment 1
[0022] Accurately weigh 10g of refined fish oil sample, add 150mL of 2mol / L NaOH ethanol aqueous solution, the ratio of ethanol / water (v / v) is 6:1, protect with nitrogen, saponify at 50°C for 60min, add 100mL of n-hexane to extract unsaponified The hydrated layer was acidified with 100mL 3mol / L HCl, and then the free n-3PUFA was extracted with n-hexane 100mL×3, washed with water until neutral, and washed with anhydrous Na 2 SO 4 , N 2 Dry the solvent to obtain n-3PUFA, the hydrolysis rate of fish oil by chemical method is 95.5%, the yield of EPA is 92%, and the yield of DHA is 90%.
[0023] Put 2 g of the n-3PUFA mixed solution containing EPA and DHA obtained after hydrolysis of the fish oil on a C18 column for chromatographic separation, the mobile phase is methanol / water, 70-100% methanol gradient elution, and the eluent is collected in parts, using Rapidly analyze the chromatographic samples by mass spectrometry, and use HPLC to detect the purity of EPA and DHA collected ...
Embodiment 2
[0026] Accurately weigh 10g of refined fish oil sample, add 150mL of 2mol / L NaOH ethanol aqueous solution, the ratio of ethanol / water (v / v) is 9:1, protect with nitrogen, saponify at 60°C for 90min, add 100mL of n-hexane to extract unsaponified The hydrated layer was acidified with 100mL 3mol / L HCl, and then the free n-3PUFA was extracted with n-hexane 100mL×3, washed with water until neutral, and washed with anhydrous Na 2 SO 4 , N 2 The solvent is blown dry to obtain n-3PUFA, and the hydrolysis rate of fish oil by chemical method is 92%, the yield of EPA is 90%, and the yield of DHA is 88%.
[0027] Put 2 g of the n-3PUFA mixed solution containing EPA and DHA obtained after hydrolysis of the fish oil on a C18 column for chromatographic separation, the mobile phase is methanol / water, 70-100% methanol gradient elution, and the eluent is collected in parts, using Rapidly analyze the chromatographic samples by mass spectrometry, and use HPLC to detect the purity of EPA and DHA...
Embodiment 3
[0030] Accurately weigh 10g of refined fish oil sample, add 150mL of 2mol / L NaOH ethanol aqueous solution, the ratio of ethanol / water (v / v) is 9:1, protect with nitrogen, saponify at 50°C for 90min, add 100mL of n-hexane to extract unsaponified The hydrated layer was acidified with 100mL 3mol / L HCl, and then the free n-3PUFA was extracted with n-hexane 100mL×3, washed with water until neutral, and washed with anhydrous Na 2 SO 4 , N 2 Drying the solvent to obtain n-3PUFA, the hydrolysis rate of fish oil by chemical method is 94%, the yield of EPA is 91%, and the yield of DHA is 89%.
[0031] Put 2 g of the n-3PUFA mixed solution containing EPA and DHA obtained after hydrolysis of the fish oil on a C18 column for chromatographic separation, the mobile phase is methanol / water, 70-100% methanol gradient elution, and the eluent is collected in parts, using Rapidly analyze the chromatographic samples by mass spectrometry, and use HPLC to detect the purity of EPA and DHA collected...
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