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Preparation method of ferulic acid from corn bran
Description
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Technical field
The present invention relates to a kind of preparation method of forulic acid, relate in particular to the preparation method of forulic acid in a kind of maize peel.
Background technology
Forulic acid (4-hydroxyl-3 methoxy cinnamic acid), is a kind of botanic fragrant acid that is prevalent in, and is one of effective constituent of the Chinese medicinal materialss such as Ligusticum wallichii, Radix Angelicae Sinensis, asafoetide, is extensively present in the agricultural and sideline products such as hominy chop, cavings.Forulic acid is to produce the basic raw material that is used for the treatment of the disease medicines such as cardiovascular and cerebrovascular diseases and oligoleukocythemia, also has the effect of protection skin.Therefore, in fields such as food, healthcare products, makeup, be widely used, in foodstuffs industry, mainly for the production of vanillin food grade,1000.000000ine mesh, antisepsis antistaling agent, food linking agent etc., its main Physiological Function has oxidation-resistance, antisepsis and anti-inflammation, reducing blood-fat, antithrombotic, anti-mutation, anti-coronary heart disease and anti-cancer etc.
At present, the preparation method of forulic acid mainly contains chemical synthesis and plant extraction method.The chemical synthesis long reaction time of forulic acid, the product of acquisition is trans and mixture cis forulic acid.China's plant resources is abundant, agricultural wastes particularly, as: cavings, Deng material, from plant, extract forulic acid and can make agricultural wastes be reused, increased added value, the method for therefore extracting forulic acid from plant has caused increasing concern, it mainly comprises alkaline process, enzyme process and additive method, but for extracting forulic acid research report seldom from maize peel.
Summary of the invention
Technical problem to be solved by this invention is to provide the preparation method of forulic acid in a kind of simple to operate, cost is low, forulic acid yield is high maize peel.
For addressing the above problem, the preparation method of forulic acid in a kind of maize peel of the present invention, comprises the following steps:
(1), after maize peel being cleaned and being dried, in temperature, be the enzyme 3 ~ 5h that goes out under the condition of 100 ~ 110 ℃, and pulverized 40 mesh sieves, the maize peel after being processed;
(2) in the maize peel after described processing, add the water of 2 ~ 10 times of its quality, after stirring, obtain slip;
(3) in described slip, by the maize peel after processing described in every 1000g, add the high temperature resistant α-amylase of 0.1 ~ 0.7mL, the Water Under that is 95 ℃ in temperature is bathed 20 ~ 60min, and every 5min vibration once, obtains removing the maize peel of starch;
(4) the maize peel that removes starch described in is cooled to after room temperature, adds the compound protease of 0.2 ~ 0.8g by the maize peel after processing described in every 1000g, and the Water Under that is 45 ℃ in temperature is bathed insulation 20 ~ 60min, and does not stop to stir, and obtains the maize peel of deproteination;
(5) the maize peel of described deproteination is heated to 100 ℃ of enzyme 10min that go out, then centrifugal, obtains residue, and this residue is washed till suspension with distilled water and under temperature is the condition of 50 ~ 60 ℃, dries to constant weight after without muddiness, obtains dry destarch deproteinated maize peel;
(6) in described dry destarch deproteinated maize peel, add the sodium hydroxide solution that 30 ~ 100 times of its quality, volumetric concentration are 0.2% ~ 2.5%, in temperature, be under the condition of 60 ℃ after water bath with thermostatic control 2 ~ 8h, through centrifugal supernatant A and the filter residue of obtaining respectively, twice of this filter residue washing, obtain supernatant liquor B, merge described supernatant A and described supernatant liquor B, obtain forulic acid extracting solution;
(7) after the standing 1h of described forulic acid extracting solution lucifuge, the centrifugal 8 ~ 12min of speed with 3500 ~ 4500r/min, is then settled to 100mL by this forulic acid extracting solution;
(8) by the forulic acid extracting solution of described constant volume, in temperature, be to concentrate under 45 ~ 55 ℃, the vacuum tightness condition that is 0.05 ~ 0.10MPa, until liquid, reduce at 3/4 o'clock, obtain forulic acid concentrated solution; Described forulic acid concentrated solution is to dry to constant weight under the condition of 40 ~ 50 ℃ in temperature, obtains forulic acid meal.
The present invention compared with prior art has the following advantages:
1, the present invention utilizes enzyme-alkaline process synergetic hydrolysis maize peel to extract forulic acid, and Technology is simple, easy handling; Meanwhile, the yield of forulic acid reaches 3 ~ 5 ‰ (w/w).
2, the present invention effectively utilizes agricultural wastes maize peel, increases added value.
3, reaction process of the present invention is stable, is convenient to implement, and is conducive to suitability for industrialized production.
Embodiment
embodiment 1a preparation method for forulic acid in maize peel, comprises the following steps:
(1), after maize peel being cleaned and being dried, in temperature, be the enzyme 5h that goes out under the condition of 100 ℃, and pulverized 40 mesh sieves, the maize peel after being processed;
(2) in the maize peel after processing, add the water of 2 times of its quality, after stirring, obtain slip;
(3) the maize peel after processing by every 1000g in slip adds the high temperature resistant α-amylase of 0.1mL, and the Water Under that is 95 ℃ in temperature is bathed 20min, and every 5min vibration once, obtains removing the maize peel of starch;
(4) the maize peel that removes starch is cooled to after room temperature, and the maize peel after processing by every 1000g adds the compound protease of 0.2g, and the Water Under that is 45 ℃ in temperature is bathed insulation 20min, and does not stop to stir, and obtains the maize peel of deproteination;
(5) the maize peel of deproteination is heated to 100 ℃ of enzyme 10min that go out, then with the centrifugal 12min of speed of 3500r/min, obtain residue, this residue is washed till suspension with distilled water and under temperature is the condition of 50 ℃, dries to constant weight after without muddiness, obtains dry destarch deproteinated maize peel;
(6) in dry destarch deproteinated maize peel, add the sodium hydroxide solution that 30 times of its quality, volumetric concentration are 0.2%, in temperature, be under the condition of 60 ℃ after water bath with thermostatic control 2h, the centrifugal 12min of speed with 3500r/min obtains respectively supernatant A and filter residue, twice of this filter residue washing, obtain supernatant liquor B, merge supernatant A and supernatant liquor B, obtain forulic acid extracting solution;
(7) after the standing 1h of forulic acid extracting solution lucifuge, the centrifugal 12min of speed with 3500r/min, is then settled to 100mL by this forulic acid extracting solution;
(8) by the forulic acid extracting solution of constant volume, in temperature, be to concentrate under 45 ℃, the vacuum tightness condition that is 0.05MPa, until liquid, reduce at 3/4 o'clock, obtain forulic acid concentrated solution; Forulic acid concentrated solution is to dry to constant weight under the condition of 40 ℃ in temperature, obtains forulic acid meal.
embodiment 2a preparation method for forulic acid in maize peel, comprises the following steps:
(1), after maize peel being cleaned and being dried, in temperature, be the enzyme 3h that goes out under the condition of 110 ℃, and pulverized 40 mesh sieves, the maize peel after being processed;
(2) in the maize peel after processing, add the water of 10 times of its quality, after stirring, obtain slip;
(3) the maize peel after processing by every 1000g in slip adds the high temperature resistant α-amylase of 0.7mL, and the Water Under that is 95 ℃ in temperature is bathed 60min, and every 5min vibration once, obtains removing the maize peel of starch;
(4) the maize peel that removes starch is cooled to after room temperature, and the maize peel after processing by every 1000g adds the compound protease of 0.8g, and the Water Under that is 45 ℃ in temperature is bathed insulation 60min, and does not stop to stir, and obtains the maize peel of deproteination;
(5) the maize peel of deproteination is heated to 100 ℃ of enzyme 10min that go out, then with the centrifugal 8min of speed of 4500r/min, obtain residue, this residue is washed till suspension with distilled water and under temperature is the condition of 60 ℃, dries to constant weight after without muddiness, obtains dry destarch deproteinated maize peel;
(6) in dry destarch deproteinated maize peel, add the sodium hydroxide solution that 100 times of its quality, volumetric concentration are 2.5%, in temperature, be under the condition of 60 ℃ after water bath with thermostatic control 8h, the centrifugal 8min of speed with 4500r/min obtains respectively supernatant A and filter residue, twice of this filter residue washing, obtain supernatant liquor B, merge supernatant A and supernatant liquor B, obtain forulic acid extracting solution;
(7) after the standing 1h of forulic acid extracting solution lucifuge, the centrifugal 8min of speed with 4500r/min, is then settled to 100mL by this forulic acid extracting solution;
(8) by the forulic acid extracting solution of constant volume, in temperature, be to concentrate under 55 ℃, the vacuum tightness condition that is 0.10MPa, until liquid, reduce at 3/4 o'clock, obtain forulic acid concentrated solution; Forulic acid concentrated solution is to dry to constant weight under the condition of 50 ℃ in temperature, obtains forulic acid meal.
embodiment 3a preparation method for forulic acid in maize peel, comprises the following steps:
(1), after maize peel being cleaned and being dried, in temperature, be the enzyme 4h that goes out under the condition of 105 ℃, and pulverized 40 mesh sieves, the maize peel after being processed;
(2) in the maize peel after processing, add the water of 6 times of its quality, after stirring, obtain slip;
(3) the maize peel after processing by every 1000g in slip adds the high temperature resistant α-amylase of 0.4mL, and the Water Under that is 95 ℃ in temperature is bathed 40min, and every 5min vibration once, obtains removing the maize peel of starch;
(4) the maize peel that removes starch is cooled to after room temperature, and the maize peel after processing by every 1000g adds the compound protease of 0.5g, and the Water Under that is 45 ℃ in temperature is bathed insulation 40min, and does not stop to stir, and obtains the maize peel of deproteination;
(5) the maize peel of deproteination is heated to 100 ℃ of enzyme 10min that go out, then with the centrifugal 10min of speed of 4000r/min, obtain residue, this residue is washed till suspension with distilled water and under temperature is the condition of 55 ℃, dries to constant weight after without muddiness, obtains dry destarch deproteinated maize peel;
(6) in dry destarch deproteinated maize peel, add the sodium hydroxide solution that 65 times of its quality, volumetric concentration are 1.5%, in temperature, be under the condition of 60 ℃ after water bath with thermostatic control 5h, the centrifugal 10min of speed with 4000r/min obtains respectively supernatant A and filter residue, twice of this filter residue washing, obtain supernatant liquor B, merge supernatant A and supernatant liquor B, obtain forulic acid extracting solution;
(7) after the standing 1h of forulic acid extracting solution lucifuge, the centrifugal 10min of speed with 4000r/min, is then settled to 100mL by this forulic acid extracting solution;
(8) by the forulic acid extracting solution of constant volume, in temperature, be to concentrate under 50 ℃, the vacuum tightness condition that is 0.07MPa, until liquid, reduce at 3/4 o'clock, obtain forulic acid concentrated solution; Forulic acid concentrated solution is to dry to constant weight under the condition of 45 ℃ in temperature, obtains forulic acid meal.
Above-mentioned
embodiment 1 ~ 3in, maize peel is farmland purchase; High temperature resistant α-amylase is provided by Jinan Jin Yuan beer raw material company limited; Compound protease is provided by Yi Xin bio tech ltd, Shanghai.
Claims (1)
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Claims (1)
Hide Dependent
translated from
1. a preparation method for forulic acid in maize peel, comprises the following steps:
(1), after maize peel being cleaned and being dried, in temperature, be the enzyme 3 ~ 5h that goes out under the condition of 100 ~ 110 ℃, and pulverized 40 mesh sieves, the maize peel after being processed;
(2) in the maize peel after described processing, add the water of 2 ~ 10 times of its quality, after stirring, obtain slip;
(3) in described slip, by the maize peel after processing described in every 1000g, add the high temperature resistant α-amylase of 0.1 ~ 0.7mL, the Water Under that is 95 ℃ in temperature is bathed 20 ~ 60min, and every 5min vibration once, obtains removing the maize peel of starch;
(4) the maize peel that removes starch described in is cooled to after room temperature, adds the compound protease of 0.2 ~ 0.8g by the maize peel after processing described in every 1000g, and the Water Under that is 45 ℃ in temperature is bathed insulation 20 ~ 60min, and does not stop to stir, and obtains the maize peel of deproteination;
(5) the maize peel of described deproteination is heated to 100 ℃ of enzyme 10min that go out, then centrifugal, obtains residue, and this residue is washed till suspension with distilled water and under temperature is the condition of 50 ~ 60 ℃, dries to constant weight after without muddiness, obtains dry destarch deproteinated maize peel;
(6) in described dry destarch deproteinated maize peel, add the sodium hydroxide solution that 30 ~ 100 times of its quality, volumetric concentration are 0.2% ~ 2.5%, in temperature, be under the condition of 60 ℃ after water bath with thermostatic control 2 ~ 8h, through centrifugal supernatant A and the filter residue of obtaining respectively, twice of this filter residue washing, obtain supernatant liquor B, merge described supernatant A and described supernatant liquor B, obtain forulic acid extracting solution;
(7) after the standing 1h of described forulic acid extracting solution lucifuge, the centrifugal 8 ~ 12min of speed with 3500 ~ 4500r/min, is then settled to 100mL by this forulic acid extracting solution;
(8) by the forulic acid extracting solution of described constant volume, in temperature, be to concentrate under 45 ~ 55 ℃, the vacuum tightness condition that is 0.05 ~ 0.10MPa, until liquid, reduce at 3/4 o'clock, obtain forulic acid concentrated solution; Described forulic acid concentrated solution is to dry to constant weight under the condition of 40 ~ 50 ℃ in temperature, obtains forulic acid meal.