A method of removing a plasticiser from vitamin E
A vitamin and plasticizer technology, applied in organic chemistry, pharmaceutical formulations, medical preparations containing active ingredients, etc., can solve problems such as unsatisfactory effects, limited effect of removing plasticizers, and high safety risks in use. Small loss, high recovery, and the effect of improving purity
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Embodiment 1
[0068] Take 201×7300 g of gel-type strongly basic anion exchange resin, fully swell with 500 mL of 95% methanol aqueous solution, put it into a chromatographic column, and elute with 1000 mL of 95% methanol to equilibrate the chromatographic column.
[0069] Take 30g of 50% mixed tocopherol sample (purchased from Jiangsu Spring Valley Biological Products Co., Ltd.), add 4 times the mass of 95% methanol aqueous solution to dissolve and load the sample. 2 -95% methanol aqueous solution was eluted, and the eluate was collected continuously and detected by thin layer chromatography (TLC). The developer was n-hexane-ether-acetic acid 8:2:0.2, and the eluate fraction containing tocopherol was collected. After combining, they were concentrated under reduced pressure at 50°C to constant weight to obtain 15.606g of vitamin E product 1.
[0070] After testing, the vitamin E content in the sample before the deplasticizer was 48.21%, and the DEHP content was 196.0ppm; in the vitamin E pro...
Embodiment 2
[0072] Take 201×7300 g of gel-type strongly basic anion exchange resin, fully swell with 500 mL of 90% methanol aqueous solution, load it into a chromatographic column, and elute with 1000 mL of 90% methanol aqueous solution to equilibrate the chromatographic column.
[0073] Take 40% mixed tocopherol (purchased from Jiangsu Spring Valley Biological Products Co., Ltd.) sample 30g, add 3 times the mass of 90% methanol to dissolve and load the sample, the chromatographic column is first eluted with 1000mL90% methanol aqueous solution, and then 1500mL saturated CO 2 -90% methanol aqueous solution was eluted, and the eluate was collected continuously and detected by thin layer chromatography (TLC). The developer was n-hexane-ether-acetic acid 8:2:0.2, and the eluate fraction containing tocopherol was collected. After combining, they were concentrated under reduced pressure at 50°C until the organic solvent was completely removed to obtain 14.599g of vitamin E product 2.
[0074] A...
Embodiment 3
[0076] Take 201×7300g gel-type strongly basic anion exchange resin, fully swell with 500mL methanol, put it into the chromatographic column, and elute the equilibrated chromatographic column with 1000mL methanol.
[0077] Take 50% mixed tocopherol (purchased from Jiangsu Spring Valley Biological Products Co., Ltd.) sample 30g, add 4 times the mass of methanol to dissolve and load the sample, the chromatographic column is first eluted with 1000mL methanol, and then 1500mL saturated CO 2 - Methanol solution elution, the eluate is collected continuously and detected by thin layer chromatography (TLC), the developer is n-hexane-ether-acetic acid 8:2:0.2, the eluate fractions containing tocopherol are collected, and after merging Concentrate under reduced pressure at 50°C until the organic solvent is completely removed to obtain 15.969g of vitamin E product 3.
[0078] After testing, the vitamin E content in the sample before deplasticizer was 49.86%, and the DEHP content was 298.2...
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