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Method for removing mineral oil in natural vitamin E

A technology of natural vitamins and mineral oil, applied in the field of biomedicine, can solve problems such as mineral oil residues, and achieve the effect of short cycle, low energy consumption and guaranteed income.

Active Publication Date: 2018-04-13
NINGBO DAHONGYING BIO ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The present invention solves the problem of trace residue of mineral oil in natural vitamin E by utilizing the polarity difference between mineral oil and natural vitamin E

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Take 80g of 100-200 mesh coarse-pore silica gel, add a small amount of n-hexane, fill it into a chromatographic column, elute and compact the chromatographic column with 3 times the volume of n-hexane, and mix 6g of natural vitamin E containing 30% mixed tocopherols with Dissolve the sample in n-hexane at a ratio of 2:1 (m / v). After loading the sample, use 6 times the volume of n-hexane to elute, and then use 3 times the volume of n-hexane: ethyl acetate = 15:1 (v / v) The mixed solvent is eluted, the eluate is collected in sections, and the natural vitamin E product is obtained through concentration (the yield of natural vitamin E is 96.3%). The residual amount of mineral oil in natural vitamin E is 9ppm (MOAH 1ppm, MOSH 8ppm) , the silica gel column was regenerated by washing with 2 volumes of ethyl acetate.

Embodiment 2

[0039]Take 80g of granular activated carbon, add a small amount of cyclohexane, fill it into the chromatographic column, elute and compact the chromatographic column with 4 times the volume of cyclohexane, and mix 7g of raw material natural vitamin E containing 50% mixed tocopherols with cyclohexane Alkanes were dissolved and loaded at 2:1 (m / v), first eluted with 5 volumes of cyclohexane, and then 6 volumes of cyclohexane: ethyl acetate = 10:1 (v / v) mixed solvent Carry out elution, collect the eluate in sections, and concentrate to obtain natural vitamin E product (natural vitamin E yield is 97.0%), the residual amount of mineral oil is 9ppm (wherein MOAH 1ppm, MOSH8ppm), activated carbon with 2 times the volume of ethyl acetate Esters flush to regenerate.

Embodiment 3

[0041] Take 90g of HZ-202 gel-type strong base anion exchange resin, add a small amount of petroleum ether with a boiling range of 60-90°C, fill it into a chromatography column, and elute with 3 times the volume of petroleum ether with a boiling range of 60-90°C The chromatographic column was compacted, and 9 g of raw material natural vitamin E containing 40% mixed tocopherols and petroleum ether with a boiling range of 60 to 90 ° C were dissolved and loaded at a ratio of 2:1 (m / v). Elute with petroleum ether with a boiling range of 60 to 90°C in double volume, and then with a mixed solvent of petroleum ether:ethyl acetate=12:1 (v / v) with a boiling range of 3 times in volume from 60 to 90°C , collect the eluate in sections, and concentrate to obtain natural vitamin E product (natural vitamin E yield is 95.6%), the residual amount of mineral oil is 8ppm (wherein MOAH 0ppm, MOSH 8ppm), resin column uses 2 times volume of ethyl acetate Rinse to regenerate.

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PUM

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Abstract

The invention discloses a method for removing mineral oil in natural vitamin E. The method comprise the following steps: (1) sample loading: taking a separating agent, adding an eluent a, charging into a chromatographic column, performing elution and compaction on the chromatographic column with the eluent a, and dissolving a loaded sample according to the following formula: a raw material:the eluent a(m / v)=2:1; (2) elution: after finish of sample loading, performing elution with the eluent at first, and then performing elution with an eluent b; (3) collection: performing fractional collectionon an elution liquid, and concentrating the collected elution liquid to obtain a natural vitamin E product; and (4) reproduction: flushing the chromatographic column with an eluent c for reproduction. The raw material is natural vitamin E, the eluent a is a low-pole solvent, the eluent b is a mixed low-pole solvent consisting of the eluent a and the eluent c, and the eluent c is a high-pole solvent. By use of polarity difference between mineral oil and natural vitamin E, the problem of trace residue of mineral oil in natural vitamin E is well solved.

Description

technical field [0001] The invention relates to the technical field of biomedicine, in particular to a method for removing mineral oil from natural vitamin E. Background technique [0002] Mineral oil is a hydrocarbon mixture formed by physical separation (distillation, extraction) and chemical conversion (hydrogenation, cracking, alkylation, and isomerization) of crude oil, including saturated oils composed of straight chain, branched chain, and ring. Mineral oil saturated hydrocarbons (MOSH, mineral oil saturated hydrocarbons) and mineral oil aromatic hydrocarbons (MOAH, mineral oil aromatic hydrocarbons) composed of polyaromatic compounds are colorless, odorless, less dense than water, slightly soluble in ethanol, and easily soluble in hydrocarbons , Transparent liquid of chlorinated solvent, which is a mixture of hydrocarbons other than animal and vegetable oils. In 1995, the Joint Food and Agriculture Organization / WHO Joint Expert Committee on Food Additives (JECFA) cl...

Claims

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Application Information

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IPC IPC(8): C07D311/72
CPCC07D311/72
Inventor 王嘉磊肖翔章生
Owner NINGBO DAHONGYING BIO ENG
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