CN106591382A - Method for efficiently extracting ferulic acid from wheat bran - Google Patents
Method for efficiently extracting ferulic acid from wheat bran Download PDFInfo
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- CN106591382A CN106591382A CN201611051124.8A CN201611051124A CN106591382A CN 106591382 A CN106591382 A CN 106591382A CN 201611051124 A CN201611051124 A CN 201611051124A CN 106591382 A CN106591382 A CN 106591382A
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P7/00—Preparation of oxygen-containing organic compounds
- C12P7/40—Preparation of oxygen-containing organic compounds containing a carboxyl group including Peroxycarboxylic acids
- C12P7/42—Hydroxy-carboxylic acids
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Abstract
The invention discloses a method for efficiently extracting ferulic acid from wheat bran as a raw material. The method comprises 1) drying wheat bran or rice bran, 2) crushing the dried wheat bran to obtain particles having sizes of 0.5mm or less, 3) adding a sodium hydroxide solution having a concentration of 0.1 to 1N into the bran particles, wherein the use amount of the sodium hydroxide is 1 to 10% of the dry weight of the bran, and immersing the mixture at 30 to 80 DEG C for 6 to 24 hours, 4) adjusting pH of the immersed bran to less than or equal to 7.0, and shearing the bran through a high speed shearing machine at a rate of 10000-20000r/min for 10-30min, (5) carrying out high pressure puffing treatment on the sheared sample, 6) adding an enzyme into the puffed product, wherein the use amount of the enzyme is 0.1-2% of the dry weight of the bran, adjusting pH to 5.0-6.0, carrying out treatment at a temperature of 20-70 DEG C for 6-48h, carrying out centrifugation on the treated sample and taking a supernatant and 7) extracting the supernatant with ethyl acetate and drying the extract through evaporation to obtain a crude ferulic acid product.
Description
Technical field
The present invention relates to a kind of extracting method of ferulic acid, and in particular to one kind is using high pressure swelling preconditioning technique from bran
The method that ferulic acid is extracted in skin.
Background technology
Ferulic acid belongs to fragrant acid compounds, with antioxidation and removing free radical, antithrombotic, mutation and protective effect on cancer risk
Deng.And, ferulic acid can also suppress multiple-microorganism to grow.It is widely used in fields such as food, medicine and cosmetics, is pole
The product of tool market development potential.And wheat bran (including Testa Tritici, Oryza glutinosa wheat bran, corn bran, distiller's grains of beer etc.) is used as grain
Processing and the by-product of wine-making technology process, containing certain ferulic acid, extract ferulic acid, not only significantly from these by-products
Increase its economic worth, and make it obtain sufficient exploitation.At present, ferulic acid is extracted from wheat bran and mainly adopts alkali
And ferment treatment, it is not easy to the ferulic acid in wheat bran in combined state is fully released to into free state, therefore extraction ratio is relatively low.
The content of the invention
It is an object of the present invention to provide one kind is with Testa Tritici and Oryza glutinosa wheat bran as raw material, the method for high efficiency extraction ferulic acid.
For achieving the above object, the present invention includes following technical scheme：
A kind of method that ferulic acid is extracted from wheat bran, the method comprises the steps：
(1) by Testa Tritici or Oryza glutinosa drying wheat bran；
(2) wheat bran of drying is crushed to into below 0.5mm；
(3) sterilization treatment is carried out to wheat bran granule；
(4) sodium hydroxide solution that concentration is 0.1～1N is added in wheat bran granule, the addition of sodium hydroxide is wheat bran
The 1～10% of dry weight, in 30-80 DEG C 6-24 hours are soaked；
(5) wheat bran after immersion is adjusted into pH to≤7.0, followed by high-speed shearing machine with 10000-20000r/min, is cut
Cut 10-30min；
(6) sample sheared is carried out into high pressure swelling process；
(7) enzyme is added in the sample after expanding treatment, the addition of enzyme is the 0.1-2% of wheat bran dry weight；Adjusting pH is
5.0-6.0, process time is 6-48 hours, and temperature is 20-70 DEG C；By the sample handled well centrifugation, supernatant is taken；
(8) supernatant is extracted with ethyl acetate, extract is evaporated, obtain crude product ferulic acid.
Method as above, it is preferable that described Testa Tritici is Testa Tritici, Fructus Hordei Vulgaris bran or distiller's grains of beer.
Method as above, it is preferable that the pressure that the high pressure swelling is processed is 300～1800 atmospheric pressure.
Method as above, it is preferable that the enzyme is xylanase, glucanase, cellulase and hemicellulase
In one or more.
Method as above, it is preferable that methods described comprises the steps：
(1) will from Testa Tritici or Oryza glutinosa wheat bran in drying baker 70 DEG C drying, the Testa Tritici be Testa Tritici, Fructus Hordei Vulgaris bran or
Distiller's grains of beer；
(2) wheat bran of drying is crushed to into below 0.5mm with grinder；
(3) to wheat bran granule sterilization treatment 30min；
(4) add concentration for the sodium hydroxide solution of 0.1N, the addition of sodium hydroxide is the 4% of wheat bran dry weight, in 30-
80 DEG C of immersion 6-24 hours；
(5) wheat bran after immersion is adjusted into pH to≤7.0 with acetic acid, using high-speed shearing machine with 10000-20000r/min,
Shearing 10-30min；
(6) sample sheared is carried out into high pressure swelling to process 3-5 time；The pressure of high pressure swelling process is 300～1800
Atmospheric pressure；
(7) enzyme is added in the sample after expanding treatment, the addition of enzyme is the 0.1-2% of wheat bran dry weight；Enzyme is poly- for wood
One or more in carbohydrase, glucanase, cellulase and hemicellulase；It is 5.2 to adjust pH with sodium acetate buffer,
Process time is 6-48 hours, and temperature is 20-70 DEG C；Sample after process is centrifuged, supernatant is taken；
(8) supernatant is extracted with ethyl acetate, extract is evaporated, obtain crude product ferulic acid.
The beneficial effects of the present invention is：Present invention optimizes wheat bran extract ferulic acid technique, mainly take dipping by lye,
Efficiently shearing, high pressure swelling are processed and enzymic digestion technique (as shown in Figure 1).Wherein, the effect of dipping by lye step is catalytic water
Solution ferulic acid ester, and cells of bran moisture-holding capacity is improved, contribute to strengthening subsequent shell-broken effect；Efficiently shearing the effect of step is
Make cells of bran breaking cellular wall；The effect of high pressure swelling step is further promotion cells of bran breaking cellular wall, and moisture enters system so that Ah
There are hydrolysis in Wei's acid esters, obtain free state ferulic acid；The effect of enzymatic treatment step is further to be hydrolyzed to ferulic acid ester
Ferulic acid.The extraction rate of ferulaic acid form of wheat bran reaches more than 50mg/g Jing after above-mentioned steps process, with unused efficiently shearing, high pressure
The extracting method of bulking step is compared, and extraction ratio improves nearly more than 10 times.
Description of the drawings
Fig. 1 is a kind of process chart of preferred implementation of the invention.
Specific embodiment
Below in conjunction with specific embodiment, the invention will be further described, but below example is only limitted to explain this
Bright, protection scope of the present invention should include the content of claim, be not limited only to the present embodiment.
Embodiment 1
70 DEG C of drying in drying baker by the distiller's grains of beer wheat bran collected from brewery；The wheat bran dried is crushed with grinder
To about 0.3mm grain diameters；The wheat bran for having sieved is weighed into 2g autoclaves sterilizing 30min, its endogenous enzymatic activity is inactivated.Plus
The sodium hydroxide for entering 40mL concentration 0.1N soaks 12 hours in 60 DEG C；Wheat bran after immersion is adjusted into pH to 7.0 with acetic acid, using height
Fast cutter shears 30min with 18000r/min.By the sample after shearing carry out high pressure swelling (400 atmospheric pressure of low pressure 1 time, in
Press 950 atmospheric pressure 1 time, 1700 atmospheric pressure of high pressure 1 time)；Glucanase, the addition of enzyme are added in the sample after expanding treatment
For the 0.3% of wheat bran dry weight.It is 5.2 to adjust pH with sodium acetate buffer, and process time is 24 hours, and temperature is 42 degree.Will
The sample 8000r/min centrifugation 15min for handling well, take supernatant；Equal-volume ethyl acetate is added to be extracted twice in supernatant,
Combining extraction liquid；Extract rotation is evaporated, crude product ferulic acid is obtained.With the anhydrous alcohol solution of 5mL, spectrophotometric determination
Its light absorption value, reference standard curve, the extraction ratio for obtaining ferulic acid is 46.8mg/g.
Embodiment 2
70 DEG C of drying in drying baker by the distiller's grains of beer wheat bran collected from brewery；The wheat bran dried is crushed with grinder
To about 0.3mm grain diameters；The wheat bran for having sieved is weighed into 2g autoclaves sterilizing 30min, its endogenous enzymatic activity is inactivated.Plus
The sodium hydroxide solution for entering 40mL concentration 0.1N soaks 12 hours in 60 DEG C；Wheat bran after immersion is adjusted into pH to 7.0, profit with acetic acid
With high-speed shearing machine with 18000r/min, 30min is sheared.Sample after shearing is carried out into high pressure swelling (500 atmospheric pressure 1 time, height
Press 1700 atmospheric pressure 2 times)；Xylanase is added in the sample after process, the addition of enzyme is the 0.3% of wheat bran dry weight.With
It is 5.2 that sodium acetate buffer adjusts pH, and process time is 48 hours, and temperature is 50 degree.By the sample 4000r/min after process
Centrifugation 15min, takes supernatant；Equal-volume ethyl acetate is added to be extracted twice in supernatant, combining extraction liquid；Extract is revolved
Turn to be evaporated, obtain crude product ferulic acid.With the anhydrous alcohol solution of 5mL, spectrophotometric determination its light absorption value；Reference standard is bent
Line, the extraction ratio for obtaining ferulic acid is 48.5mg/g.
Embodiment 3
70 DEG C of drying in drying baker by the distiller's grains of beer wheat bran collected from brewery；The wheat bran dried is crushed with grinder
To about 0.3mm grain diameters；Wheat bran after screening is weighed into 2g autoclaves sterilizing 30min, its endogenous enzymatic activity is inactivated.Plus
Enter the sodium hydroxide of 20mL concentration 0.1N, 30ml distilled water soaks 6 hours in 70 DEG C；Wheat bran after immersion is adjusted into pH with acetic acid
To 7.0, using high-speed shearing machine with 18000r/min, 30min is sheared；Sample after shearing is carried out into high pressure swelling (low pressure 500
Atmospheric pressure 2 times, 1700 atmospheric pressure of high pressure 2 times).Glucanase, addition is added to be wheat bran dry weight in the sample after process
1%；Cellulose and hemicellulase, addition is respectively the 0.3% of wheat bran dry weight.Adjusting pH with sodium acetate buffer is
5.2, process time is 48 hours, and temperature is 42 degree.By the sample 8000r/min centrifugation 15min after process, supernatant is taken；To
Equal-volume ethyl acetate is added to be extracted twice in supernatant, combining extraction liquid；Extract rotation is evaporated.Ferulic acid is averagely carried
Rate is taken for 56.4mg/g.
Embodiment 4
70 DEG C of drying in drying baker by the Testa Tritici collected from flour mill；The wheatfeed that will be dried with pulverizer
It is broken to about 0.5mm grain diameters；Wheat bran after screening is weighed into 5g autoclaves sterilizing 30min, its endogenous enzymatic activity is inactivated.
The sodium hydroxide for adding 50mL concentration 0.1N soaks 6 hours in 60 DEG C；Wheat bran after immersion is adjusted into pH to 7.0 with sulphuric acid, is utilized
High-speed shearing machine shears 30min with 18000r/min.Sample after shearing is carried out into high pressure swelling (800 atmospheric pressure 1 time, high pressure
1600 atmospheric pressure 2 times).Glucanase and xylanase, addition is added to be respectively wheat bran dry weight in the sample after process
0.5%；Cellulose and hemicellulase, addition is respectively the 0.3% of wheat bran dry weight.Adjusting pH with sodium acetate buffer is
5.2, process time is 48 hours, and temperature is 45 degree.By the sample 8000r/min centrifugation 15min after process, supernatant is taken；To
Equal-volume ethyl acetate is added to be extracted twice in supernatant, combining extraction liquid；Extract rotation is evaporated.Ferulic acid is averagely carried
Rate is taken for 52.6mg/g.
Comparative example 1
70 DEG C of drying in drying baker by the distiller's grains of beer wheat bran collected from brewery；The wheat bran dried is crushed with grinder
To about 0.3mm grain diameters；Wheat bran after screening is weighed into 2g autoclaves sterilizing 30min, its endogenous enzymatic activity is inactivated.Plus
The sodium hydroxide for entering 20mL concentration 0.1N soaks 6 hours in 60 DEG C；Wheat bran after immersion is adjusted into pH to 7.0 with acetic acid, using height
Fast cutter shears 20min with 18000r/min.Glucanase is added in the sample after process, the addition of enzyme is wheat bran
The 0.3% of dry weight.It is 5.2 to adjust pH with sodium acetate buffer, and process time is 24 hours, and temperature is 42 degree.After processing
Sample 4000r/min centrifugation 20min, take supernatant；Add equal-volume ethyl acetate to be extracted twice in supernatant, merge extraction
Take liquid；Extract rotation is evaporated, crude product ferulic acid is obtained.With the anhydrous alcohol solution of 5mL, spectrophotometric determination its extinction
Value；Reference standard curve, the extraction ratio for obtaining ferulic acid is 24.95mg/g.
Experimental result is illustrated, in the case of the process of unused high pressure swelling, only with efficiently shearing, extraction ratio is only to use
Half of high pressure swelling or so.
Claims (5)
1. it is a kind of from wheat bran extract ferulic acid method, it is characterised in that the method comprises the steps：
(1) by Testa Tritici or Oryza glutinosa drying wheat bran；
(2) wheat bran of drying is crushed to into below 0.5mm；
(3) sterilization treatment is carried out to wheat bran granule；
(4) sodium hydroxide solution that concentration is 0.1～1N is added in wheat bran granule, the addition of sodium hydroxide is wheat bran dry weight
1～10%, in 30-80 DEG C soak 6-24 hours；
(5) wheat bran after immersion is adjusted into pH to≤7.0, followed by high-speed shearing machine with 10000-20000r/min, shears 10-
30min；
(6) sample sheared is carried out into high pressure swelling process；
(7) enzyme is added in the sample after expanding treatment, the addition of enzyme is the 0.1-2% of wheat bran dry weight；Regulation pH is 5.0-
6.0, process time is 6-48 hours, and temperature is 20-70 DEG C；By the sample handled well centrifugation, supernatant is taken；
(8) supernatant is extracted with ethyl acetate, extract is evaporated, obtain crude product ferulic acid.
2. method according to claim 1, it is characterised in that described Testa Tritici is Testa Tritici, Fructus Hordei Vulgaris bran or medicated beer
Grain.
3. method according to claim 1 and 2, it is characterised in that the pressure that the high pressure swelling is processed is 300～1800
Atmospheric pressure.
4. method according to claim 3, it is characterised in that the enzyme be xylanase, glucanase, cellulase and
One or more in hemicellulase.
5. method according to claim 4, it is characterised in that methods described comprises the steps：
(1) will dry for 70 DEG C in drying baker from Testa Tritici or Oryza glutinosa wheat bran, the Testa Tritici is Testa Tritici, Fructus Hordei Vulgaris bran or medicated beer
Grain；
(2) wheat bran of drying is crushed to into below 0.5mm with grinder；
(3) to wheat bran granule sterilization treatment 30min；
(4) add concentration for the sodium hydroxide solution of 0.1N, the addition of sodium hydroxide is the 4% of wheat bran dry weight, in 30-80 DEG C
Immersion 6-24 hours；
(5) wheat bran after immersion is adjusted into pH to≤7.0 with acetic acid, using high-speed shearing machine with 10000-20000r/min, shearing
10-30min；
(6) sample sheared is carried out into high pressure swelling to process 3-9 time；The pressure of high pressure swelling process is 300～1800 air
Pressure；
(7) enzyme is added in the sample after expanding treatment, the addition of enzyme is the 0.1-2% of wheat bran dry weight；Enzyme be xylanase,
One or more in glucanase, cellulase and hemicellulase；It is 5.2 to adjust pH with sodium acetate buffer, is processed
Time is 6-48 hours, and temperature is 20-70 DEG C；Sample after process is centrifuged, supernatant is taken；
(8) supernatant is extracted with ethyl acetate, extract is evaporated, obtain crude product ferulic acid.
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| CN2016106329064 | 2016-08-04 | ||
| CN201610632906 | 2016-08-04 |
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| CN106591382A true CN106591382A (en) | 2017-04-26 |
| CN106591382B CN106591382B (en) | 2021-08-27 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109022501A (en) * | 2018-07-13 | 2018-12-18 | 江南大学 | A method of ferulic acid is obtained using waste |
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|---|---|---|---|---|
| CN101629191A (en) * | 2009-08-18 | 2010-01-20 | 河南工业大学 | Ultrasound-assisted enzymolysis wheat bran method for preparing ferulic acid |
| 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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2016
- 2016-11-24 CN CN201611051124.8A patent/CN106591382B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101629191A (en) * | 2009-08-18 | 2010-01-20 | 河南工业大学 | Ultrasound-assisted enzymolysis wheat bran method for preparing ferulic acid |
| 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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| 李次力: "酶-碱法协同水解麦麸提取阿魏酸及功能性研究", 《食品工业科技》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109022501A (en) * | 2018-07-13 | 2018-12-18 | 江南大学 | A method of ferulic acid is obtained using waste |
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