Extraction method of alkyl resorcinol in wheat bran

A technology of alkyl resorcinol and wheat bran, which is applied in the field of separation and purification of natural functional substances, can solve the problems of high price, high risk, and difficult control, and achieve toxicity, environmental protection, low price, and high utilization rate Effect

Active Publication Date: 2019-07-12
NANJING UNIV OF FINANCE & ECONOMICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The research on ARs has the following problems: First, there is a lack of reasonable and standardized alkyl resorcinol separation technology. -CH 2 , its polarity is similar and it is difficult to separate; second, the standard product of alkyl resorcinol is expensive and has a long delivery period, which can easily affect the research progress of alkyl resorcinol; third, there are chemical synthesis in previous studies Alkyl resorcinol is a precedent, but the synthesis process is complicated, difficult to control, and dangerous, and further purification is required in the later stage, which has the risk of secondary pollution to the environment

Method used

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  • Extraction method of alkyl resorcinol in wheat bran
  • Extraction method of alkyl resorcinol in wheat bran
  • Extraction method of alkyl resorcinol in wheat bran

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) Raw material pretreatment: remove gravel, silt, and diseased insect grains from the wheat harvested in the same year, wash and dry, and use a mill to grind the wheat bran to 80 mesh after obtaining the bran;

[0039] (2) Extraction: Ultrasonic extraction of wheat bran was performed with ethyl acetate as the extraction solvent, the extraction time was 30 min, and the extraction power was 300 W;

[0040] (3) Centrifugation: Centrifuge at 3500 r / min for 10 minutes to obtain the sample supernatant;

[0041] (4) Concentration: Collect the supernatant obtained by centrifugation and concentrate it using a rotary evaporator at a temperature of 45 °C to obtain a concentrated solution of the alkyl resorcinol ethyl acetate extract;

[0042](5) Separation and purification: using silica gel column chromatography, first place 100-200 mesh silica gel powder in a 120 °C oven for high temperature activation for 30 min, and then place it in a desiccator to cool to room temperature. ...

Embodiment 2

[0056] (1) Raw material pretreatment: remove gravel, silt, and diseased insect grains from the wheat harvested in the same year, wash and dry, and use a mill to grind the wheat bran to 80 mesh after obtaining the bran;

[0057] (2) Extraction: Ultrasonic extraction of wheat bran was performed with ethyl acetate as the extraction solvent, the extraction time was 30 min, and the extraction power was 300 W;

[0058] (3) Centrifugation: Centrifuge at 3500 r / min for 10 minutes to obtain the sample supernatant;

[0059] (4) Concentration: Collect the supernatant obtained by centrifugation and concentrate it using a rotary evaporator at a temperature of 45 °C to obtain a concentrated solution of the alkyl resorcinol ethyl acetate extract;

[0060] (5) Separation and purification: select a solid phase extraction column, first use n-pentane to flush the column to remove impurities and reduce the polarity of the solid phase extraction column, and then load the concentrated solution of t...

Embodiment 3

[0074] Comparing the separation and purification effects of various alkyl resorcinols, the mixture obtained in Example 1 has good separation and few impurities. The alkylresorcinol homologue mixture obtained in Example 1 was used to further prepare the alkylresorcinol monomer through the semi-preparative liquid phase.

[0075] The semi-preparative liquid chromatography conditions are:

[0076] (1) Mobile phase: A phase 0.1% formic acid aqueous solution; B phase 0.1% formic acid methanol solution, flow rate: 2 mL / min, column temperature: 30 ℃, injection volume: 200 µL;

[0077] (2) The mobile phase elution program is: 0min, A phase 15~25%, B phase 75~85%; 5min, A phase 15~10%, B phase 75~90%; 10min, A phase 5~10% , B phase 90~95%; 15min, A phase 0~5%, B phase 95~100%; 35min, A phase 15~25%, B phase 75~85%;

[0078] (3) Detector: DAD detector is used, and the detection wavelength is 280 nm.

[0079] Obtained 5 monomers of alkylresorcinol under the above-mentioned conditions, ...

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Abstract

The invention belongs to the field of separation and preparation of natural functional substances, and relates to an extraction method of alkyl resorcinol in wheat bran. The method comprises the following steps: selecting dried wheat bran as a raw material, selecting, arranging and grinding the raw material, then adding ethyl acetate to carry out ultrasonic extraction, carrying out centrifuging toobtain a supernate, and carrying out rotary evaporation to obtain a concentrated solution; and then carrying out silica gel column chromatography by using a solid-phase extraction or a silica gel mixing sample for separation and purification, and further concentrating the eluent to obtain a mixed solution of different homolog of alkyl resorcinol. Through high performance liquid chromatography analysis, different homolog in the alkyl resorcinol product has the advantages of good separation degree, high purity and the like. Compared with the existing alkyl resorcinol preparation technology, themethod disclosed by the invention has the advantages that silica gel column chromatography is used for separating and purifying naturally existed alkyl resorcinol in the wheat bran, so that complexity and risks of chemical synthesis are greatly reduced, and operability is high.

Description

technical field [0001] The invention relates to an extraction method of alkylresorcinol in wheat bran, belonging to the field of separation and purification of natural functional substances. Background technique [0002] Alkyl resorcinol ( Alkylresorcinols, ARs ) is the general term for a class of derivatives of 1,3-resorcinol, whose 5-position of the benzene ring is substituted with an alkyl group containing an odd number of carbon atoms. It belongs to phenolic lipids and has amphiphilic properties. ARs are distributed in the cortex of wheat grains and are the main phenolic components in wheat, with a total content ranging from 320 to 1010 μg / g. ARs are composed of a variety of homologues, whose alkyl side chains contain an odd number of carbon atoms (13 to 27), named C13:0 to C27:0, and the main components are C19:0 and C21:0. ARs is an important biomarker for judging whole wheat flour according to the current grain industry standard (LS / T 3244-2015), and it is also one ...

Claims

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Application Information

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IPC IPC(8): C07C37/70C07C37/82C07C39/08C07C39/19
CPCC07C37/004C07C39/08C07C39/19Y02P60/87
Inventor 方勇邹燕羽黄沁沁严曲李彭谢旻皓刘琴
Owner NANJING UNIV OF FINANCE & ECONOMICS
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