CN106591382B - Method for extracting ferulic acid from bran - Google Patents
Method for extracting ferulic acid from bran Download PDFInfo
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- CN106591382B CN106591382B CN201611051124.8A CN201611051124A CN106591382B CN 106591382 B CN106591382 B CN 106591382B CN 201611051124 A CN201611051124 A CN 201611051124A CN 106591382 B CN106591382 B CN 106591382B
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Abstract
A method for efficiently extracting ferulic acid by taking bran as a raw material comprises the following steps: 1) drying testa Tritici or testa oryzae; 2) pulverizing the dried bran to below 0.5 mm; 3) adding a sodium hydroxide solution with the concentration of 0.1-1N into the bran particles, wherein the addition amount of the sodium hydroxide is 1-10% of the dry weight of the bran, and soaking for 6-24 hours at the temperature of 30-80 ℃; 4) adjusting the pH value of the soaked bran to be less than or equal to 7.0, and then shearing for 10-30min at 10000-20000r/min by using a high-speed shearing machine; 5) carrying out high-pressure puffing treatment on the cut sample; 6) adding enzyme into the sample after puffing treatment, wherein the addition amount of the enzyme is 0.1-2% of the dry weight of the bran; adjusting pH to 5.0-6.0, treating for 6-48 hr at 20-70 deg.C; centrifuging the treated sample, and taking supernatant; 7) extracting the supernatant with ethyl acetate, and evaporating the extractive solution to dryness to obtain crude ferulic acid.
Description
Technical Field
The invention relates to a method for extracting ferulic acid, in particular to a method for extracting ferulic acid from bran by using a high-pressure puffing pretreatment technology.
Background
Ferulic acid belongs to the field of folic acid compounds, and has effects of resisting oxidation, scavenging free radicals, resisting thrombi, resisting mutation, preventing cancer, etc. Furthermore, ferulic acid also inhibits the growth of a variety of microorganisms. The product has wide application in the fields of food, medicine, cosmetics and the like, and has great market development potential. Bran (including wheat bran, rice bran, corn bran, brewer's grains and the like) is used as a byproduct in the processes of grain processing and brewing, contains a certain amount of ferulic acid, and the ferulic acid is extracted from the byproduct, so that the economic value of the ferulic acid is remarkably increased, and the ferulic acid is fully developed and utilized. At present, the ferulic acid extracted from the bran is mainly treated by alkali and enzyme, so that the ferulic acid in a combined state in the bran is not easy to be fully released into a free state, and the extraction rate is low.
Disclosure of Invention
The invention aims to provide a method for efficiently extracting ferulic acid by using wheat bran and rice bran as raw materials.
In order to achieve the purpose, the invention comprises the following technical scheme:
a method for extracting ferulic acid from bran comprises the following steps:
(1) drying testa Tritici or testa oryzae;
(2) pulverizing the dried bran to below 0.5 mm;
(3) sterilizing the bran particles;
(4) adding a sodium hydroxide solution with the concentration of 0.1-1N into the bran particles, wherein the addition amount of the sodium hydroxide is 1-10% of the dry weight of the bran, and soaking for 6-24 hours at the temperature of 30-80 ℃;
(5) adjusting the pH value of the soaked bran to be less than or equal to 7.0, and then shearing for 10-30min at 10000-20000r/min by using a high-speed shearing machine;
(6) carrying out high-pressure puffing treatment on the cut sample;
(7) adding enzyme into the sample after puffing treatment, wherein the addition amount of the enzyme is 0.1-2% of the dry weight of the bran; adjusting pH to 5.0-6.0, treating for 6-48 hr at 20-70 deg.C; centrifuging the treated sample, and taking supernatant;
(8) extracting the supernatant with ethyl acetate, and evaporating the extractive solution to dryness to obtain crude ferulic acid.
In the method, the wheat bran is preferably wheat bran, barley bran or brewer's grain.
In the method, the pressure of the high-pressure puffing treatment is preferably 300 to 1800 atm.
The method as described above, preferably, the enzyme is one or more of xylanase, glucanase, cellulase and hemicellulase.
The method as described above, preferably, the method comprises the steps of:
(1) drying wheat bran or rice bran in a drying oven at 70 deg.C, wherein the wheat bran is wheat bran, barley bran or brewer's grain;
(2) pulverizing the dried bran into powder with a grinder to a particle size below 0.5 mm;
(3) sterilizing bran particles for 30 min;
(4) adding 0.1N sodium hydroxide solution (4% of dry weight of bran), and soaking at 30-80 deg.C for 6-24 hr;
(5) adjusting the pH value of the soaked bran to be less than or equal to 7.0 by using acetic acid, and shearing for 10-30min at 10000-20000r/min by using a high-speed shearing machine;
(6) carrying out high-pressure puffing treatment on the cut sample for 3-5 times; the pressure of the high-pressure puffing treatment is 300-1800 atmospheric pressure;
(7) adding enzyme into the sample after puffing treatment, wherein the addition amount of the enzyme is 0.1-2% of the dry weight of the bran; the enzyme is one or more of xylanase, glucanase, cellulase and hemicellulase; adjusting pH to 5.2 with sodium acetate buffer solution at 20-70 deg.C for 6-48 hr; centrifuging the treated sample, and taking supernatant;
(8) extracting the supernatant with ethyl acetate, and evaporating the extractive solution to dryness to obtain crude ferulic acid.
The invention has the beneficial effects that: the invention optimizes the process for extracting ferulic acid from bran, and mainly adopts the processes of alkali liquor soaking, high-efficiency shearing, high-pressure puffing treatment and enzyme digestion (as shown in figure 1). Wherein the alkali liquor soaking step is used for catalyzing and hydrolyzing ferulic acid ester, improving the water retention of bran cells and contributing to strengthening the subsequent wall breaking effect; the high-efficiency shearing step has the function of breaking the cell walls of the bran; the high-pressure puffing step has the effects of further promoting the wall breaking of bran cells, and allowing water to enter a system, so that ferulic acid ester undergoes a hydrolysis reaction to obtain free ferulic acid; the enzyme treatment step serves to further hydrolyze the ferulic acid ester to ferulic acid. The extraction rate of ferulic acid of the bran treated by the steps reaches more than 50mg/g, and compared with an extraction method without the steps of efficient shearing and high-pressure puffing, the extraction rate is improved by more than 10 times.
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FIG. 1 is a process flow diagram of a preferred embodiment of the present invention.
Detailed Description
The present invention is further illustrated by the following specific examples, but the following examples are only illustrative of the present invention, and the scope of the present invention shall include the contents of the claims, and not limited to the examples.
Example 1
Drying the brewery spent grains bran collected from a brewery in a drying oven at 70 ℃; pulverizing the dried bran into about 0.3mm particle size with a grinder; weighing 2g of the sieved bran, sterilizing the weighed bran for 30min by using a sterilizing pot, and inactivating the endogenous enzyme activity of the bran. Adding 40mL of 0.1N sodium hydroxide, and soaking at 60 ℃ for 12 hours; adjusting pH of the soaked bran to 7.0 with acetic acid, and shearing at 18000r/min for 30min with high speed shearing machine. Carrying out high-pressure puffing on the cut sample (low pressure 400 atm for 1 time, medium pressure 950 atm for 1 time and high pressure 1700 atm for 1 time); adding glucanase into the sample after the puffing treatment, wherein the adding amount of the glucanase is 0.3 percent of the dry weight of the bran. The pH was adjusted to 5.2 with sodium acetate buffer solution for 24 hours at 42 ℃. Centrifuging the treated sample at 8000r/min for 15min, and collecting supernatant; adding equal volume of ethyl acetate into the supernatant, extracting twice, and combining the extracts; and rotatably evaporating the extract to dryness to obtain a crude product of ferulic acid. Dissolving with 5mL of anhydrous ethanol, measuring light absorption value with a spectrophotometer, and contrasting with a standard curve to obtain the extraction rate of the ferulic acid of 46.8 mg/g.
Example 2
Drying the brewery spent grains bran collected from a brewery in a drying oven at 70 ℃; pulverizing the dried bran into about 0.3mm particle size with a grinder; weighing 2g of the sieved bran, sterilizing the weighed bran for 30min by using a sterilizing pot, and inactivating the endogenous enzyme activity of the bran. Adding 40mL of 0.1N sodium hydroxide solution, and soaking at 60 ℃ for 12 hours; adjusting pH of the soaked bran to 7.0 with acetic acid, and shearing at 18000r/min for 30min with high speed shearing machine. Puffing the sheared sample under high pressure (1 time under 500 atm and 2 times under 1700 atm); xylanase was added to the treated sample in an amount of 0.3% of the dry weight of the bran. The pH was adjusted to 5.2 with sodium acetate buffer for 48 hours at 50 ℃. Centrifuging the treated sample at 4000r/min for 15min, and taking supernatant; adding equal volume of ethyl acetate into the supernatant, extracting twice, and combining the extracts; and rotatably evaporating the extract to dryness to obtain a crude product of ferulic acid. Dissolving the mixture by using 5mL of absolute ethyl alcohol, and measuring a light absorption value of the mixture by using a spectrophotometer; by comparing with the standard curve, the extraction rate of ferulic acid is 48.5 mg/g.
Example 3
Drying the brewery spent grains bran collected from a brewery in a drying oven at 70 ℃; pulverizing the dried bran into about 0.3mm particle size with a grinder; weighing 2g of the sieved bran, sterilizing the weighed bran for 30min by using a sterilizing pot, and inactivating the endogenous enzyme activity of the bran. Adding 20mL of 0.1N sodium hydroxide and 30mL of distilled water, and soaking at 70 ℃ for 6 hours; adjusting pH of the soaked bran to 7.0 with acetic acid, and shearing at 18000r/min for 30min with a high-speed shearing machine; the sheared sample was puffed at high pressure (500 atm low pressure 2 times, 1700 atm high pressure 2 times). Adding glucanase into the treated sample, wherein the addition amount is 1% of the dry weight of the bran; cellulose and hemicellulase, the addition amount of each of which is 0.3% of the dry weight of the bran. The pH was adjusted to 5.2 with sodium acetate buffer solution for 48 hours at 42 ℃. Centrifuging the treated sample at 8000r/min for 15min, and collecting supernatant; adding equal volume of ethyl acetate into the supernatant, extracting twice, and combining the extracts; the extract was rotary evaporated to dryness. The average extraction rate of ferulic acid was 56.4 mg/g.
Example 4
Drying wheat bran collected from a flour processing plant in a drying box at 70 ℃; pulverizing the dried bran into about 0.5mm particle size with a pulverizer; weighing 5g of the sieved bran, sterilizing the weighed bran for 30min by using a sterilizing pot, and inactivating the endogenous enzyme activity of the bran. Adding 50mL of 0.1N sodium hydroxide solution, and soaking at 60 ℃ for 6 hours; adjusting pH of the soaked bran to 7.0 with sulfuric acid, and shearing at 18000r/min for 30min with a high-speed shearing machine. The sheared sample was puffed at high pressure (800 atm for 1 time and 1600 atm for 2 times). Adding glucanase and xylanase into the treated sample, wherein the addition amount of the glucanase and the xylanase is 0.5% of the dry weight of the bran respectively; cellulose and hemicellulase, the addition amount of each of which is 0.3% of the dry weight of the bran. The pH was adjusted to 5.2 with sodium acetate buffer for 48 hours at 45 ℃. Centrifuging the treated sample at 8000r/min for 15min, and collecting supernatant; adding equal volume of ethyl acetate into the supernatant, extracting twice, and combining the extracts; the extract was rotary evaporated to dryness. The average extraction rate of ferulic acid was 52.6 mg/g.
Comparative example 1
Drying the brewery spent grains bran collected from a brewery in a drying oven at 70 ℃; pulverizing the dried bran into about 0.3mm particle size with a grinder; weighing 2g of the sieved bran, sterilizing the weighed bran for 30min by using a sterilizing pot, and inactivating the endogenous enzyme activity of the bran. Adding 20mL of 0.1N sodium hydroxide solution, and soaking at 60 ℃ for 6 hours; adjusting pH of the soaked bran to 7.0 with acetic acid, and shearing at 18000r/min for 20min with high speed shearing machine. Dextranase was added to the treated samples at an amount of 0.3% dry weight of bran. The pH was adjusted to 5.2 with sodium acetate buffer solution for 24 hours at 42 ℃. Centrifuging the treated sample at 4000r/min for 20min, and taking supernatant; adding equal volume of ethyl acetate into the supernatant, extracting twice, and combining the extracts; and rotatably evaporating the extract to dryness to obtain a crude product of ferulic acid. Dissolving the mixture by using 5mL of absolute ethyl alcohol, and measuring a light absorption value of the mixture by using a spectrophotometer; by contrast with the standard curve, the extraction rate of ferulic acid was 24.95 mg/g.
The experimental results show that under the condition of not using high-pressure puffing treatment, only high-efficiency shearing is used, and the extraction rate is only about half of that of using high-pressure puffing.
Claims (2)
1. A method for extracting ferulic acid from bran is characterized by comprising the following steps:
(1) drying testa Tritici or testa oryzae; the testa Tritici is testa Tritici, fructus Hordei vulgaris bran or brewer's grain;
(2) pulverizing the dried bran to below 0.5 mm;
(3) sterilizing the bran particles;
(4) adding a sodium hydroxide solution with the concentration of 0.1-1N into the bran particles, wherein the addition amount of the sodium hydroxide is 1-10% of the dry weight of the bran, and soaking for 6-24 hours at the temperature of 30-80 ℃;
(5) adjusting the pH value of the soaked bran to be less than or equal to 7.0, and then shearing for 10-30min at 10000-20000r/min by using a high-speed shearing machine;
(6) carrying out high-pressure puffing treatment on the cut sample; the pressure is 300-1800 atmospheric pressure;
(7) adding enzyme into the sample after puffing treatment, wherein the enzyme is one or more of xylanase, glucanase, cellulase and hemicellulase, and the addition amount of the enzyme is 0.1-2% of the dry weight of the bran; adjusting pH to 5.0-6.0, treating for 6-48 hr at 20-70 deg.C; centrifuging the treated sample, and taking supernatant;
(8) extracting the supernatant with ethyl acetate, and evaporating the extractive solution to dryness to obtain crude ferulic acid.
2. Method according to claim 1, characterized in that it comprises the following steps:
(1) drying wheat bran or rice bran in a drying oven at 70 deg.C, wherein the wheat bran is wheat bran, barley bran or brewer's grain;
(2) pulverizing the dried bran into powder with a grinder to a particle size below 0.5 mm;
(3) sterilizing bran particles for 30 min;
(4) adding 0.1N sodium hydroxide solution (4% of dry weight of bran), and soaking at 30-80 deg.C for 6-24 hr;
(5) adjusting the pH value of the soaked bran to be less than or equal to 7.0 by using acetic acid, and shearing for 10-30min at 10000-20000r/min by using a high-speed shearing machine;
(6) carrying out high-pressure puffing treatment on the cut sample for 3-9 times; the pressure of the high-pressure puffing treatment is 300-1800 atmospheric pressure;
(7) adding enzyme into the sample after puffing treatment, wherein the addition amount of the enzyme is 0.1-2% of the dry weight of the bran; the enzyme is one or more of xylanase, glucanase, cellulase and hemicellulase; adjusting pH to 5.2 with sodium acetate buffer solution at 20-70 deg.C for 6-48 hr; centrifuging the treated sample, and taking supernatant;
(8) extracting the supernatant with ethyl acetate, and evaporating the extractive solution to dryness to obtain crude ferulic acid.
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| CN102633628A (en) * | 2012-03-28 | 2012-08-15 | 常熟市滨江农业科技有限公司 | Method for extracting ferulic acid from wheat by-products |
| CN103045658A (en) * | 2012-12-24 | 2013-04-17 | 保龄宝生物股份有限公司 | Method of taking bran as raw materials to prepare high-purity low-poly araboxylan and ferulic acid |
| CN103642851A (en) * | 2013-12-10 | 2014-03-19 | 江南大学 | Method for preparing ferulic acid from wheat bran by using two-enzyme method |
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