Method for separating single tocopherol from mixed tocopherol
A technology for separating tocopherols, which is applied in the field of separating single tocopherols, and achieves the effects of high degree of production automation, simple process and high production efficiency
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Embodiment 1
[0033] Simulated moving bed system CSEP _ 916 (Norr, Germany), equipped with 8 chromatographic columns (ID2×10cm), 2 in each zone, the chromatographic columns are filled with silica gel, and the columns are packed by high-pressure wet method. The mobile phase was n-hexane / ethanol solution (99.5 / 0.5, v / v), and the temperature was 30°C. The purity of the mixed tocopherols used for feeding is 97.5%, which contains 22.8% of α-tocopherol, 2.8% of β-tocopherol, 34.7% of γ-tocopherol and 37.2% of δ-tocopherol. mg / ml feed solution.
[0034] a. Operating conditions
[0035] Injection liquid flow rate: U F =1ml / min
[0036] Eluent flow rate: U D =2.8ml / min
[0037] Raffinate flow rate: U R =2.0ml / min
[0038] Extraction flow rate: U E =1.8ml / min
[0039] Zone 1 velocity: U E =6.4ml / min
[0040] Switching time: t s =757s
[0041] b. Finished product analysis
[0042] The composition of raffinate and extract was analyzed by silica gel column. The purity and yield of δ-toco...
Embodiment 2
[0044] Simulated moving bed system CSEP_ 916 (Norr, Germany), equipped with 8 chromatographic columns (ID2×10cm), 2 in each zone, the chromatographic columns are filled with powdered activated carbon, and packed by high-pressure wet method. The mobile phase was n-hexane / methanol solution (99.5 / 0.5, v / v), and the temperature was 30°C. The purity of the mixed tocopherols used for feeding is 97.5%, which contains 22.8% of α-tocopherol, 2.8% of β-tocopherol, 34.7% of γ-tocopherol and 37.2% of δ-tocopherol. mg / ml feed solution.
[0045] a. Operating conditions
[0046] Injection liquid flow rate: U F =1ml / min
[0047] Eluent flow rate: U D =2.6ml / min
[0048] Raffinate flow rate: U R =1.8ml / min
[0049] Extraction flow rate: U E =2.0ml / min
[0050] Zone 1 velocity: U E =6.7ml / min
[0051] Switching time: t s =720s
[0052] b. Finished product analysis
[0053] The composition of raffinate and extract was analyzed by silica gel column. The purity and yield of δ-tocoph...
Embodiment 3
[0055] Simulated moving bed system CSEP _ 916 (Noel, Germany), equipped with 8 chromatographic columns (ID2×10cm), 2 in each zone, the chromatographic columns are filled with activated alumina, and the columns are packed by high-pressure wet method. The mobile phase was n-hexane / acetone solution (99 / 1, v / v), and the temperature was 30°C. The purity of the mixed tocopherols used for feeding is 97.5%, which contains 22.8% of α-tocopherol, 2.8% of β-tocopherol, 34.7% of γ-tocopherol and 37.2% of δ-tocopherol. mg / ml feed solution.
[0056] a. Operating conditions
[0057] Injection liquid flow rate: U F =1ml / min
[0058] Eluent flow rate: U D =3.1ml / min
[0059] Raffinate flow rate: U R =2.2ml / min
[0060] Extraction flow rate: U E =1.9ml / min
[0061] Zone 1 velocity: U E =6.9ml / min
[0062] Switching time: t s =708s
[0063] b. Finished product analysis
[0064] The composition of raffinate and extract was analyzed by silica gel column. The purity and yield of δ-t...
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