CN112280825B - Method for pretreatment of raw materials for fermentation wine production - Google Patents
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Abstract
The invention discloses a research method for pretreatment of raw materials for fermentation wine production, which comprises the following steps: step one: measuring the starch content of the residual rice; step two: selecting gelatinized rice solution; and step three, determining the fermentation process flow of the residual rice. According to the characteristics of the residual rice, the invention improves the original brewing process, innovates and improves the pretreatment process of raw materials, realizes full gelatinization of the residual rice in the secondary gelatinization process, expands the utilization rate, and realizes high-efficiency brewing.
Description
Technical Field
The invention relates to the technical field of fermentation wine production, in particular to a method for preprocessing raw materials for fermentation wine production.
Background
At present, the residual rice is mainly used for producing feeds, biogas, organic fertilizers and the like, the residual rice is recycled to a certain extent, and the residual rice is rich in a large amount of fermentable starch, so that compared with the production of alcohol, the treatment method has low value. The existing raw materials for fermenting and producing wine comprise grains such as corn, wheat, sorghum and the like, potato and cassava and other potato substances and fruits, and the effect of the secondary gelatinization process is poor because part of starch in the residual rice is regenerated; secondly, the residual rice may be infected with bacteria and generate toxins, so the residual rice is not used as a raw material for fermentation brewing, and no research on fermentation and wine production of the residual rice is carried out.
Disclosure of Invention
In order to overcome the problems, the invention provides a method for pretreatment of raw materials for fermentation wine production.
The technical scheme adopted by the invention is as follows:
the pretreatment method of the raw materials for fermenting and producing wine comprises the following steps:
step one: determination of starch content in the residual Rice: weighing 10g of residual rice, mixing with 50mL of water, pulping in a pulping machine, flushing the pulping machine with 50mL of water for three times, transferring the washing liquid and the slurry into a 250mL conical flask, heating in boiling water for 20 minutes to completely gelatinize the residual rice, adding 10mL of amylase solution, continuously boiling in a boiling water bath for 30 minutes, stirring constantly, then adding a drop of dilute iodine solution into the conical flask, observing whether the iodine solution changes color, continuously adding 5mL of amylase solution into the conical flask if the iodine solution changes color, continuously boiling in boiling water for 10 minutes, continuously adding amylase solution if the iodine solution still changes color, transferring the sample solution into a 250mL volumetric flask after cooling until the iodine solution does not change color, uniformly shaking with distilled water, filtering and discarding the primary filtrate; taking 50mL of filtrate, placing the filtrate into a 250mL conical flask, adding 5mL of hydrochloric acid, installing a spherical condenser tube at a flask mouth, refluxing in boiling water for 1 hour, cooling, adding two drops of phenolphthalein reagent, neutralizing the solution with 200g/L sodium hydroxide solution until the solution is just colored, adding one drop of hydrochloric acid solution to enable the solution to be acidic, adding 5mL of potassium ferrocyanide solution and 5mL of zinc acetate solution into the solution, standing for 30min, filtering with filter paper, and transferring the obtained filtrate into a 100mL volumetric flask to be constant volume with distilled water; preliminary test: sucking 5mL of the Fi Lin Jia liquid and the Fi Lin Yiye liquid, placing the solutions in a 250mL conical flask, adding 10mL of distilled water, adding three glass balls, heating to boil in 2min, adding the sample liquid at a speed of a buret for a period of time, keeping the solution in a boiling state all the time, titrating at a speed of one drop per 2 seconds after the solution becomes light in color until the solution just fades to an end point, recording the consumed volume of the sample solution, and properly diluting the sample when the concentration of the sample is too high, so that the volume of the sample solution consumed each time is controlled to be close to the volume of the standard glucose solution consumed by the calibrated alkaline copper tartrate solution; formal test: sucking 5mL of fibreglass Lin Jia liquid and fibreglass Lin Yiye, placing the liquid into a 250mL conical flask, adding 10mL of distilled water, adding three glass spheres, transferring the closest integral volume of sample liquid (for example, the predicted volume is 8.2mL, 7mL is transferred into the conical flask by a pipette) which is 1mL less than the predicted volume into the conical flask, placing the conical flask on a universal electric furnace, controlling the conical flask to boil within two minutes, keeping the boiling state, titrating the conical flask at the speed of one drop every two seconds until blue just disappears, recording the volume consumed by the sample liquid, performing three groups in parallel, controlling the error of each group within 0.1mL, and obtaining the average consumed volume;
step two: selection of gelatinized rice solution: raw material preparation: weighing 3 groups of 50g of residual rice, and adding distilled water, sodium hydroxide solution (5 g/L-7 g/L) and sodium carbonate solution (5 g/L-7 g/L); gelatinizing in a boiling water bath; liquefying in boiling water bath: adding hydrochloric acid to pre-adjust pH, adding amylase and hot water to adjust pH with a pH meter, and liquefying in boiling water bath for 30min; detection of amylase: detecting whether amylase is contained in the gelatinized liquid by using iodine liquid, and if the iodine liquid turns blue, adding amylase into the gelatinized liquid to continue liquefying until the gelatinized liquid does not turn blue; and (3) cooling: cooling to 35-40 deg.c and regulating pH to 4.2-4.8 with pH meter; determination of DE value of the gelatinized liquid: measuring the DE value of the gelatinized liquid by taking 50mL of the gelatinized liquid; measuring the DE value of saccharified liquid after saccharifying by saccharifying enzyme: adding saccharifying enzyme into 50mL of gelatinized liquid, preserving heat in a water bath, and measuring the DE value of saccharified liquid after saccharifying by saccharifying enzyme;
step three: determination of the fermentation process flow of the residual rice: determining the concentration of gelatinized liquid, gelatinization time, alpha-amylase addition amount and saccharifying enzyme addition amount by detecting the change of DE value in the liquefaction process and saccharification process, determining the fermentation time and optimal feed-liquid ratio by detecting the quality change of fermentation liquid, and determining the optimal temperature of fermentation and the optimal yeast addition amount by detecting the change of alcohol degree.
Wherein, in the second step, the weight ratio of distilled water, sodium hydroxide solution, sodium carbonate solution and the residual rice is 1.5:1.
Wherein, the gelatinization time of the medium boiling water bath in the second step is 30min.
Wherein the amylase liquefied in the boiling water bath in the second step is alpha-amylase and is added to the gelatinized liquid according to the proportion of 50 mu/g-100 mu/g.
Wherein, in the second step, the pH value of the liquefied boiling water bath is adjusted to 5.2-5.8.
Wherein, the saccharifying enzyme with DE value of saccharifying liquid after saccharifying by the saccharifying enzyme in the step two is added according to 150 mu/g-200 mu/g, the water bath temperature is 35 ℃, and the heat preservation time is 1 hour.
The invention has the following advantages:
according to the characteristics of the residual rice, the invention improves the original brewing process, innovates and improves the pretreatment process of raw materials, realizes full gelatinization of the residual rice in the secondary gelatinization process, expands the utilization rate, and realizes high-efficiency brewing.
Drawings
FIG. 1 is a process flow diagram of a method for pretreatment of raw materials for fermentation of wine production according to the present invention;
FIG. 2 is a schematic diagram showing the reducing sugar content, total sugar content and DE value of the gelatinized liquid according to the experimental result of the pretreatment method of raw material for fermentation and wine production of the present invention;
FIG. 3 is a schematic diagram showing the reducing sugar content, total sugar content and DE value of the saccharified liquid according to the experimental results of the pretreatment method of raw materials for fermentation production of wine according to the present invention.
Description of the embodiments
The invention is further described below, but is not limited to these.
Examples
The pretreatment method of the raw materials for fermenting and producing wine comprises the following steps:
step one: determination of starch content in the residual Rice: weighing 10g of residual rice, mixing with 50mL of water, pulping in a pulping machine, flushing the pulping machine with 50mL of water for three times, transferring the washing liquid and the slurry into a 250mL conical flask, heating in boiling water for 20 minutes to completely gelatinize the residual rice, adding 10mL of amylase solution, continuously boiling in a boiling water bath for 30 minutes, stirring constantly, then adding a drop of dilute iodine solution into the conical flask, observing whether the iodine solution changes color, continuously adding 5mL of amylase solution into the conical flask if the iodine solution changes color, continuously boiling in boiling water for 10 minutes, continuously adding amylase solution if the iodine solution still changes color, transferring the sample solution into a 250mL volumetric flask after cooling until the iodine solution does not change color, uniformly shaking with distilled water, filtering and discarding the primary filtrate; taking 50mL of filtrate, placing the filtrate into a 250mL conical flask, adding 5mL of hydrochloric acid, installing a spherical condenser tube at a flask mouth, refluxing in boiling water for 1 hour, cooling, adding two drops of phenolphthalein reagent, neutralizing the solution with 200g/L sodium hydroxide solution until the solution is just colored, adding one drop of hydrochloric acid solution to enable the solution to be acidic, adding 5mL of potassium ferrocyanide solution and 5mL of zinc acetate solution into the solution, standing for 30min, filtering with filter paper, and transferring the obtained filtrate into a 100mL volumetric flask to be constant volume with distilled water; preliminary test: sucking 5mL of the Fi Lin Jia liquid and the Fi Lin Yiye liquid, placing the solutions in a 250mL conical flask, adding 10mL of distilled water, adding three glass balls, heating to boil in 2min, adding the sample liquid at a speed of a buret for a period of time, keeping the solution in a boiling state all the time, titrating at a speed of one drop per 2 seconds after the solution becomes light in color until the solution just fades to an end point, recording the consumed volume of the sample solution, and properly diluting the sample when the concentration of the sample is too high, so that the volume of the sample solution consumed each time is controlled to be close to the volume of the standard glucose solution consumed by the calibrated alkaline copper tartrate solution; formal test: sucking 5mL of fibreglass Lin Jia liquid and fibreglass Lin Yiye, placing the liquid into a 250mL conical flask, adding 10mL of distilled water, adding three glass spheres, transferring the closest integral volume of sample liquid (for example, the predicted volume is 8.2mL, 7mL is transferred into the conical flask by a pipette) which is 1mL less than the predicted volume into the conical flask, placing the conical flask on a universal electric furnace, controlling the conical flask to boil within two minutes, keeping the boiling state, titrating the conical flask at the speed of one drop every two seconds until blue just disappears, recording the volume consumed by the sample liquid, performing three groups in parallel, controlling the error of each group within 0.1mL, and obtaining the average consumed volume;
step two: selection of gelatinized rice solution: raw material preparation: weighing 3 groups of 50g of residual rice, and adding distilled water, sodium hydroxide solution (6 g/L) and sodium carbonate solution (6 g/L) according to a ratio of 1:1.5; gelatinizing in boiling water bath for 30min; liquefying in boiling water bath: adding hydrochloric acid to pre-regulate pH after gelatinization in boiling water bath, adding amylase and hot water to regulate pH to 5.2-5.8 with pH meter, adding alpha-amylase to gelatinized liquid according to 50 mu/g, liquefying in boiling water bath for 30min; detection of amylase: detecting whether amylase is contained in the gelatinized liquid by using iodine liquid, and if the iodine liquid turns blue, adding a small amount of amylase into the gelatinized liquid to continue liquefying until the gelatinized liquid does not turn blue; and (3) cooling: cooling to 35-40 deg.c, and regulating pH value with pH meter to 4.2-4.8; determination of DE value of the gelatinized liquid: measuring the DE value of the gelatinized liquid by taking 50mL of the gelatinized liquid; measuring the DE value of saccharified liquid after saccharifying by saccharifying enzyme: taking 50mL of gelatinized liquid, adding saccharifying enzyme according to 200 mu/g, preserving heat for 1h in a water bath at 35 ℃, and measuring the DE value of saccharified liquid after saccharifying by saccharifying enzyme;
step three: determination of the fermentation process flow of the residual rice: determining the concentration of gelatinized liquid, gelatinization time, alpha-amylase addition amount and saccharifying enzyme addition amount by detecting the change of DE value in the liquefaction process and saccharification process, determining the fermentation time and optimal feed-liquid ratio by detecting the quality change of fermentation liquid, and determining the optimal temperature of fermentation and the optimal yeast addition amount by detecting the change of alcohol degree.
Examples
The pretreatment method of the raw materials for fermenting and producing wine comprises the following steps:
step one: determination of starch content in the residual Rice: weighing 10g of residual rice, mixing with 50mL of water, pulping in a pulping machine, flushing the pulping machine with 50mL of water for three times, transferring the washing liquid and the slurry into a 250mL conical flask, heating in boiling water for 20 minutes to completely gelatinize the residual rice, adding 10mL of amylase solution, continuously boiling in a boiling water bath for 30 minutes, stirring constantly, then adding a drop of dilute iodine solution into the conical flask, observing whether the iodine solution changes color, continuously adding 5mL of amylase solution into the conical flask if the iodine solution changes color, continuously boiling in boiling water for 10 minutes, continuously adding amylase solution if the iodine solution still changes color, transferring the sample solution into a 250mL volumetric flask after cooling until the iodine solution does not change color, uniformly shaking with distilled water, filtering and discarding the primary filtrate; taking 50mL of filtrate, placing the filtrate into a 250mL conical flask, adding 5mL of hydrochloric acid, installing a spherical condenser tube at a flask mouth, refluxing in boiling water for 1 hour, cooling, adding two drops of phenolphthalein reagent, neutralizing the solution with 200g/L sodium hydroxide solution until the solution is just colored, adding one drop of hydrochloric acid solution to enable the solution to be acidic, adding 5mL of potassium ferrocyanide solution and 5mL of zinc acetate solution into the solution, standing for 30min, filtering with filter paper, and transferring the obtained filtrate into a 100mL volumetric flask to be constant volume with distilled water; preliminary test: sucking 5mL of the Fi Lin Jia liquid and the Fi Lin Yiye liquid, placing the solutions in a 250mL conical flask, adding 10mL of distilled water, adding three glass balls, heating to boil in 2min, adding the sample liquid at a speed of a buret for a period of time, keeping the solution in a boiling state all the time, titrating at a speed of one drop per 2 seconds after the solution becomes light in color until the solution just fades to an end point, recording the consumed volume of the sample solution, and properly diluting the sample when the concentration of the sample is too high, so that the volume of the sample solution consumed each time is controlled to be close to the volume of the standard glucose solution consumed by the calibrated alkaline copper tartrate solution; formal test: sucking 5mL of fibreglass Lin Jia liquid and fibreglass Lin Yiye, placing the liquid into a 250mL conical flask, adding 10mL of distilled water, adding three glass spheres, transferring the closest integral volume of sample liquid (for example, the predicted volume is 8.2mL, 7mL is transferred into the conical flask by a pipette) which is 1mL less than the predicted volume into the conical flask, placing the conical flask on a universal electric furnace, controlling the conical flask to boil within two minutes, keeping the boiling state, titrating the conical flask at the speed of one drop every two seconds until blue just disappears, recording the volume consumed by the sample liquid, performing three groups in parallel, controlling the error of each group within 0.1mL, and obtaining the average consumed volume;
step two: selection of gelatinized rice solution: raw material preparation: weighing 3 groups of 50g of residual rice, and adding distilled water, sodium hydroxide solution (5 g/L) and sodium carbonate solution (5 g/L) according to a ratio of 1:1.5; gelatinizing in boiling water bath for 30min; liquefying in boiling water bath: adding hydrochloric acid to pre-regulate pH after gelatinization in boiling water bath, adding amylase and hot water to regulate pH to 5.2-5.8 with pH meter, adding alpha-amylase to gelatinized liquid according to 50 mu/g, liquefying in boiling water bath for 30min; detection of amylase: detecting whether amylase is contained in the gelatinized liquid by using iodine liquid, and if the iodine liquid turns blue, adding a small amount of amylase into the gelatinized liquid to continue liquefying until the gelatinized liquid does not turn blue; and (3) cooling: cooling to 35-40 deg.c, and regulating pH value with pH meter to 4.2-4.8; determination of DE value of the gelatinized liquid: measuring the DE value of the gelatinized liquid by taking 50mL of the gelatinized liquid;
measuring the DE value of saccharified liquid after saccharifying by saccharifying enzyme: taking 50mL of gelatinized liquid, adding saccharifying enzyme according to 150 mu/g, preserving heat for 1h in a water bath at 35 ℃, and measuring the DE value of saccharified liquid after saccharifying by saccharifying enzyme;
step three: determination of the fermentation process flow of the residual rice: determining the concentration of gelatinized liquid, gelatinization time, alpha-amylase addition amount and saccharifying enzyme addition amount by detecting the change of DE value in the liquefaction process and saccharification process, determining the fermentation time and optimal feed-liquid ratio by detecting the quality change of fermentation liquid, and determining the optimal temperature of fermentation and the optimal yeast addition amount by detecting the change of alcohol degree.
Examples
The pretreatment method of the raw materials for fermenting and producing wine comprises the following steps:
step one: determination of starch content in the residual Rice: weighing 10g of residual rice, mixing with 50mL of water, pulping in a pulping machine, flushing the pulping machine with 50mL of water for three times, transferring the washing liquid and the slurry into a 250mL conical flask, heating in boiling water for 20 minutes to completely gelatinize the residual rice, adding 10mL of amylase solution, continuously boiling in a boiling water bath for 30 minutes, stirring constantly, then adding a drop of dilute iodine solution into the conical flask, observing whether the iodine solution changes color, continuously adding 5mL of amylase solution into the conical flask if the iodine solution changes color, continuously boiling in boiling water for 10 minutes, continuously adding amylase solution if the iodine solution still changes color, transferring the sample solution into a 250mL volumetric flask after cooling until the iodine solution does not change color, uniformly shaking with distilled water, filtering and discarding the primary filtrate; taking 50mL of filtrate, placing the filtrate into a 250mL conical flask, adding 5mL of hydrochloric acid, installing a spherical condenser tube at a flask mouth, refluxing in boiling water for 1 hour, cooling, adding two drops of phenolphthalein reagent, neutralizing the solution with 200g/L sodium hydroxide solution until the solution is just colored, adding one drop of hydrochloric acid solution to enable the solution to be acidic, adding 5mL of potassium ferrocyanide solution and 5mL of zinc acetate solution into the solution, standing for 30min, filtering with filter paper, and transferring the obtained filtrate into a 100mL volumetric flask to be constant volume with distilled water; preliminary test: sucking 5mL of the Fi Lin Jia liquid and the Fi Lin Yiye liquid, placing the solutions in a 250mL conical flask, adding 10mL of distilled water, adding three glass balls, heating to boil in 2min, adding the sample liquid at a speed of a buret for a period of time, keeping the solution in a boiling state all the time, titrating at a speed of one drop per 2 seconds after the solution becomes light in color until the solution just fades to an end point, recording the consumed volume of the sample solution, and properly diluting the sample when the concentration of the sample is too high, so that the volume of the sample solution consumed each time is controlled to be close to the volume of the standard glucose solution consumed by the calibrated alkaline copper tartrate solution; formal test: sucking 5mL of fibreglass Lin Jia liquid and fibreglass Lin Yiye, placing the liquid into a 250mL conical flask, adding 10mL of distilled water, adding three glass spheres, transferring the closest integral volume of sample liquid (for example, the predicted volume is 8.2mL, 7mL is transferred into the conical flask by a pipette) which is 1mL less than the predicted volume into the conical flask, placing the conical flask on a universal electric furnace, controlling the conical flask to boil within two minutes, keeping the boiling state, titrating the conical flask at the speed of one drop every two seconds until blue just disappears, recording the volume consumed by the sample liquid, performing three groups in parallel, controlling the error of each group within 0.1mL, and obtaining the average consumed volume;
step two: selection of gelatinized rice solution: raw material preparation: weighing 3 groups of 50g of residual rice, and adding distilled water, sodium hydroxide solution (7 g/L) and sodium carbonate solution (7 g/L) according to a ratio of 1:1.5; gelatinizing in boiling water bath for 30min; liquefying in boiling water bath: adding hydrochloric acid to pre-regulate pH after gelatinization in boiling water bath, adding amylase and hot water to regulate pH to 5.2-5.8 with pH meter, adding alpha-amylase to gelatinized liquid according to 100 mu/g, liquefying in boiling water bath for 30min; detection of amylase: detecting whether amylase is contained in the gelatinized liquid by using iodine liquid, and if the iodine liquid turns blue, adding a small amount of amylase into the gelatinized liquid to continue liquefying until the gelatinized liquid does not turn blue; and (3) cooling: cooling to 35-40 deg.c, and regulating pH value with pH meter to 4.2-4.8; determination of DE value of the gelatinized liquid: measuring the DE value of the gelatinized liquid by taking 50mL of the gelatinized liquid;
measuring the DE value of saccharified liquid after saccharifying by saccharifying enzyme: taking 50mL of gelatinized liquid, adding saccharifying enzyme according to 200 mu/g, preserving heat for 1h in a water bath at 35 ℃, and measuring the DE value of saccharified liquid after saccharifying by saccharifying enzyme;
step three: determination of the fermentation process flow of the residual rice: determining the concentration of gelatinized liquid, gelatinization time, alpha-amylase addition amount and saccharifying enzyme addition amount by detecting the change of DE value in the liquefaction process and saccharification process, determining the fermentation time and optimal feed-liquid ratio by detecting the quality change of fermentation liquid, and determining the optimal temperature of fermentation and the optimal yeast addition amount by detecting the change of alcohol degree.
Examples
The pretreatment method of the raw materials for fermenting and producing wine comprises the following steps:
step one: determination of starch content in the residual Rice: weighing 10g of residual rice, mixing with 50mL of water, pulping in a pulping machine, flushing the pulping machine with 50mL of water for three times, transferring the washing liquid and the slurry into a 250mL conical flask, heating in boiling water for 20 minutes to completely gelatinize the residual rice, adding 10mL of amylase solution, continuously boiling in a boiling water bath for 30 minutes, stirring constantly, then adding a drop of dilute iodine solution into the conical flask, observing whether the iodine solution changes color, continuously adding 5mL of amylase solution into the conical flask if the iodine solution changes color, continuously boiling in boiling water for 10 minutes, continuously adding amylase solution if the iodine solution still changes color, transferring the sample solution into a 250mL volumetric flask after cooling until the iodine solution does not change color, uniformly shaking with distilled water, filtering and discarding the primary filtrate; taking 50mL of filtrate, placing the filtrate into a 250mL conical flask, adding 5mL of hydrochloric acid, installing a spherical condenser tube at a flask mouth, refluxing in boiling water for 1 hour, cooling, adding two drops of phenolphthalein reagent, neutralizing the solution with 200g/L sodium hydroxide solution until the solution is just colored, adding one drop of hydrochloric acid solution to enable the solution to be acidic, adding 5mL of potassium ferrocyanide solution and 5mL of zinc acetate solution into the solution, standing for 30min, filtering with filter paper, and transferring the obtained filtrate into a 100mL volumetric flask to be constant volume with distilled water; preliminary test: sucking 5mL of the Fi Lin Jia liquid and the Fi Lin Yiye liquid, placing the solutions in a 250mL conical flask, adding 10mL of distilled water, adding three glass balls, heating to boil in 2min, adding the sample liquid at a speed of a buret for a period of time, keeping the solution in a boiling state all the time, titrating at a speed of one drop per 2 seconds after the solution becomes light in color until the solution just fades to an end point, recording the consumed volume of the sample solution, and properly diluting the sample when the concentration of the sample is too high, so that the volume of the sample solution consumed each time is controlled to be close to the volume of the standard glucose solution consumed by the calibrated alkaline copper tartrate solution; formal test: sucking 5mL of fibreglass Lin Jia liquid and fibreglass Lin Yiye, placing the liquid into a 250mL conical flask, adding 10mL of distilled water, adding three glass spheres, transferring the closest integral volume of sample liquid (for example, the predicted volume is 8.2mL, 7mL is transferred into the conical flask by a pipette) which is 1mL less than the predicted volume into the conical flask, placing the conical flask on a universal electric furnace, controlling the conical flask to boil within two minutes, keeping the boiling state, titrating the conical flask at the speed of one drop every two seconds until blue just disappears, recording the volume consumed by the sample liquid, performing three groups in parallel, controlling the error of each group within 0.1mL, and obtaining the average consumed volume;
step two: selection of gelatinized rice solution: raw material preparation: weighing 3 groups of 50g of residual rice, and adding distilled water, sodium hydroxide solution (6 g/L) and sodium carbonate solution (6 g/L) according to a ratio of 1:1.5; gelatinizing in boiling water bath for 30min; liquefying in boiling water bath: adding hydrochloric acid to pre-regulate pH after gelatinization in boiling water bath, adding amylase and hot water to regulate pH to 5.2-5.8 with pH meter, adding alpha-amylase to gelatinized liquid according to 100 mu/g, liquefying in boiling water bath for 30min; detection of amylase: detecting whether amylase is contained in the gelatinized liquid by using iodine liquid, and if the iodine liquid turns blue, adding a small amount of amylase into the gelatinized liquid to continue liquefying until the gelatinized liquid does not turn blue; and (3) cooling: cooling to 35-40 deg.c, and regulating pH value with pH meter to 4.2-4.8; determination of DE value of the gelatinized liquid: measuring the DE value of the gelatinized liquid by taking 50mL of the gelatinized liquid;
measuring the DE value of saccharified liquid after saccharifying by saccharifying enzyme: taking 50mL of gelatinized liquid, adding saccharifying enzyme according to 150 mu/g, preserving heat for 1h in a water bath at 35 ℃, and measuring the DE value of saccharified liquid after saccharifying by saccharifying enzyme;
step three: determination of the fermentation process flow of the residual rice: determining the concentration of gelatinized liquid, gelatinization time, alpha-amylase addition amount and saccharifying enzyme addition amount by detecting the change of DE value in the liquefaction process and saccharification process, determining the fermentation time and optimal feed-liquid ratio by detecting the quality change of fermentation liquid, and determining the optimal temperature of fermentation and the optimal yeast addition amount by detecting the change of alcohol degree.
Examples
The pretreatment method of the raw materials for fermenting and producing wine comprises the following steps:
step one: determination of starch content in the residual Rice: weighing 10g of residual rice, mixing with 50mL of water, pulping in a pulping machine, flushing the pulping machine with 50mL of water for three times, transferring the washing liquid and the slurry into a 250mL conical flask, heating in boiling water for 20 minutes to completely gelatinize the residual rice, adding 10mL of amylase solution, continuously boiling in a boiling water bath for 30 minutes, stirring constantly, then adding a drop of dilute iodine solution into the conical flask, observing whether the iodine solution changes color, continuously adding 5mL of amylase solution into the conical flask if the iodine solution changes color, continuously boiling in boiling water for 10 minutes, continuously adding amylase solution if the iodine solution still changes color, transferring the sample solution into a 250mL volumetric flask after cooling until the iodine solution does not change color, uniformly shaking with distilled water, filtering and discarding the primary filtrate; taking 50mL of filtrate, placing the filtrate into a 250mL conical flask, adding 5mL of hydrochloric acid, installing a spherical condenser tube at a flask mouth, refluxing in boiling water for 1 hour, cooling, adding two drops of phenolphthalein reagent, neutralizing the solution with 200g/L sodium hydroxide solution until the solution is just colored, adding one drop of hydrochloric acid solution to enable the solution to be acidic, adding 5mL of potassium ferrocyanide solution and 5mL of zinc acetate solution into the solution, standing for 30min, filtering with filter paper, and transferring the obtained filtrate into a 100mL volumetric flask to be constant volume with distilled water; preliminary test: sucking 5mL of the Fi Lin Jia liquid and the Fi Lin Yiye liquid, placing the solutions in a 250mL conical flask, adding 10mL of distilled water, adding three glass balls, heating to boil in 2min, adding the sample liquid at a speed of a buret for a period of time, keeping the solution in a boiling state all the time, titrating at a speed of one drop per 2 seconds after the solution becomes light in color until the solution just fades to an end point, recording the consumed volume of the sample solution, and properly diluting the sample when the concentration of the sample is too high, so that the volume of the sample solution consumed each time is controlled to be close to the volume of the standard glucose solution consumed by the calibrated alkaline copper tartrate solution; formal test: sucking 5mL of fibreglass Lin Jia liquid and fibreglass Lin Yiye, placing the liquid into a 250mL conical flask, adding 10mL of distilled water, adding three glass spheres, transferring the closest integral volume of sample liquid (for example, the predicted volume is 8.2mL, 7mL is transferred into the conical flask by a pipette) which is 1mL less than the predicted volume into the conical flask, placing the conical flask on a universal electric furnace, controlling the conical flask to boil within two minutes, keeping the boiling state, titrating the conical flask at the speed of one drop every two seconds until blue just disappears, recording the volume consumed by the sample liquid, performing three groups in parallel, controlling the error of each group within 0.1mL, and obtaining the average consumed volume;
step two: selection of gelatinized rice solution: raw material preparation: weighing 3 groups of 50g of residual rice, and adding distilled water, sodium hydroxide solution (6 g/L) and sodium carbonate solution (6 g/L) according to a ratio of 1:1.5; gelatinizing in boiling water bath for 30min; liquefying in boiling water bath: adding hydrochloric acid to pre-regulate pH after gelatinization in boiling water bath, adding amylase and hot water to regulate pH to 5.2-5.8 with pH meter, adding alpha-amylase to gelatinized liquid according to 50 mu/g, liquefying in boiling water bath for 30min; detection of amylase: detecting whether amylase is contained in the gelatinized liquid by using iodine liquid, and if the iodine liquid turns blue, adding a small amount of amylase into the gelatinized liquid to continue liquefying until the gelatinized liquid does not turn blue; and (3) cooling: cooling to 35-40 deg.c, and regulating pH value with pH meter to 4.2-4.8; determination of DE value of the gelatinized liquid: measuring the DE value of the gelatinized liquid by taking 50mL of the gelatinized liquid;
measuring the DE value of saccharified liquid after saccharifying by saccharifying enzyme: taking 50mL of gelatinized liquid, adding saccharifying enzyme according to 150 mu/g, preserving heat for 1h in a water bath at 35 ℃, and measuring the DE value of saccharified liquid after saccharifying by saccharifying enzyme;
step three: determination of the fermentation process flow of the residual rice: determining the concentration of gelatinized liquid, gelatinization time, alpha-amylase addition amount and saccharifying enzyme addition amount by detecting the change of DE value in the liquefaction process and saccharification process, determining the fermentation time and optimal feed-liquid ratio by detecting the quality change of fermentation liquid, and determining the optimal temperature of fermentation and the optimal yeast addition amount by detecting the change of alcohol degree.
The experimental results are shown in fig. 2 and 3:
the experimental results showed that the total sugar content and the reducing sugar content of the gelatinized liquid of the residual rice were relatively high, and the reducing sugar content and the total sugar content of the saccharified liquid were relatively high, by gelatinizing the residual rice with the sodium hydroxide solution.
Comparing the three gelatinization modes, the method finds that gelatinization of the residual rice by using the alkaline solution can indeed promote the water swelling of starch in the residual rice, thereby promoting gelatinization and saccharification, solving the problem that the residual rice is not thoroughly gelatinized in the secondary process, and further can realize disinfection and sterilization under alkaline conditions, and reduce the generation of toxin.
The best pretreatment method of the residual rice comprises the following steps: adding 6g/L sodium hydroxide solution according to a ratio of 1:1.5, gelatinizing the residual rice for 30min, fully absorbing water and expanding the residual rice in the secondary gelatinization process, heating water and hydrochloric acid solution to pre-regulate the pH value, adding a small amount of alpha-amylase, regulating the pH value to 5.2-5.8, adding 50 mu/g amylase to liquefy for 30min, regulating the pH value to 4.2-4.8, adding 200 mu/g saccharifying enzyme to saccharify, subpackaging into light bottles after 15min saccharification, inoculating 4% yeast, and culturing at constant temperature of 28 ℃ for 75 h.
It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention.
Claims (6)
1. The method for preprocessing the raw materials for fermenting and producing wine is characterized by comprising the following steps:
step one: determination of starch content in the residual Rice: weighing 10g of residual rice, mixing with 50mL of water, pulping in a pulping machine, flushing the pulping machine with 50mL of water for three times, transferring the washing liquid and the slurry into a 250mL conical flask, heating in boiling water for 20 minutes to completely gelatinize the residual rice, adding 10mL of amylase solution, continuously boiling in a boiling water bath for 30 minutes, stirring constantly, then adding a drop of dilute iodine solution into the conical flask, observing whether the iodine solution changes color, continuously adding 5mL of amylase solution into the conical flask if the iodine solution changes color, continuously boiling in boiling water for 10 minutes, continuously adding amylase solution if the iodine solution still changes color, transferring the sample solution into a 250mL volumetric flask after cooling until the iodine solution does not change color, uniformly shaking with distilled water, filtering and discarding the primary filtrate; taking 50mL of filtrate, placing the filtrate into a 250mL conical flask, adding 5mL of hydrochloric acid, installing a spherical condenser tube at a flask mouth, refluxing in boiling water for 1 hour, cooling, adding two drops of phenolphthalein reagent, neutralizing the solution with 200g/L sodium hydroxide solution until the solution is just colored, adding one drop of hydrochloric acid solution to enable the solution to be acidic, adding 5mL of potassium ferrocyanide solution and 5mL of zinc acetate solution into the solution, standing for 30min, filtering with filter paper, and transferring the obtained filtrate into a 100mL volumetric flask to be constant volume with distilled water; preliminary test: sucking 5mL of the Fi Lin Jia liquid and the Fi Lin Yiye liquid, placing the solutions in a 250mL conical flask, adding 10mL of distilled water, adding three glass balls, heating to boil in 2min, adding the sample liquid at a speed of a buret for a period of time, keeping the solution in a boiling state all the time, titrating at a speed of one drop per 2 seconds after the solution becomes light in color until the solution just fades to an end point, recording the consumed volume of the sample solution, and properly diluting the sample when the concentration of the sample is too high, so that the volume of the sample solution consumed each time is controlled to be close to the volume of the standard glucose solution consumed by the calibrated alkaline copper tartrate solution; formal test: sucking 5mL of fibreglass Lin Jia liquid and fibreglass Lin Yiye, placing the liquid into a 250mL conical flask, adding 10mL of distilled water, adding three glass balls, transferring the sample liquid with the nearest whole volume which is 1mL less than the predicted volume into the conical flask by using a pipette, placing the sample liquid into a universal electric furnace, controlling the sample liquid to boil within two minutes, keeping the boiling state, titrating the sample liquid by using a burette at the speed of one drop every two seconds until blue just disappears, recording the consumed volume of the sample liquid, and performing three groups in parallel by the same operation, wherein the error of each group is controlled within 0.1mL to obtain the average consumed volume;
step two: selection of gelatinized rice solution: raw material preparation: weighing 3 groups of 50g of residual rice, and adding distilled water, 5g/L-7g/L of sodium hydroxide solution and 5g/L-7g/L of sodium carbonate solution; gelatinizing in a boiling water bath; liquefying in boiling water bath: adding hydrochloric acid to pre-adjust pH, adding amylase and hot water to adjust pH with a pH meter, and liquefying in boiling water bath for 30min; detection of amylase: detecting whether amylase is contained in the gelatinized liquid by using iodine liquid, and if the iodine liquid turns blue, adding amylase into the gelatinized liquid to continue liquefying until the gelatinized liquid does not turn blue; and (3) cooling: cooling to 35-40 deg.c and regulating pH to 4.2-4.8 with pH meter; determination of DE value of the gelatinized liquid: measuring the DE value of the gelatinized liquid by taking 50mL of the gelatinized liquid; measuring the DE value of saccharified liquid after saccharifying by saccharifying enzyme: adding saccharifying enzyme into 50mL of gelatinized liquid, preserving heat in a water bath, and measuring the DE value of saccharified liquid after saccharifying by saccharifying enzyme;
step three: determination of the fermentation process flow of the residual rice: determining the concentration of gelatinized liquid, the gelatinization time, the addition amount of alpha-amylase and the addition amount of saccharifying enzyme by detecting the change of DE value in the liquefaction process and the saccharification process, determining the fermentation time and the optimal feed-liquid ratio by detecting the quality change of fermentation liquid, and determining the optimal fermentation temperature and the optimal addition amount of yeast by detecting the change of alcohol degree;
the pretreatment method of the residual rice comprises the following steps: adding 6g/L sodium hydroxide solution according to a ratio of 1:1.5, gelatinizing the residual rice for 30min, fully absorbing water and expanding the residual rice in the secondary gelatinization process, heating water and hydrochloric acid solution to pre-regulate the pH value, adding a small amount of alpha-amylase, regulating the pH value to 5.2-5.8, adding 50 mu/g amylase to liquefy for 30min, regulating the pH value to 4.2-4.8, adding 200 mu/g saccharifying enzyme to saccharify, subpackaging into light bottles after 15min saccharification, inoculating 4% yeast, and culturing at constant temperature of 28 ℃ for 75 h.
2. The method for pretreatment of raw materials for fermentation production of wine according to claim 1, wherein: in the second step, the weight ratio of distilled water, sodium hydroxide solution, sodium carbonate solution and the residual rice is 1.5:1.
3. The method for pretreatment of raw materials for fermentation production of wine according to claim 1, wherein: and in the second step, the gelatinization time of the boiling water bath is 30min.
4. The method for pretreatment of raw materials for fermentation production of wine according to claim 1, wherein: the amylase liquefied in the boiling water bath in the second step is alpha-amylase, and the alpha-amylase is added to the gelatinized liquid according to the proportion of 50 mu/g-100 mu/g.
5. The method for pretreatment of raw materials for fermentation production of wine according to claim 1, wherein: and in the second step, the pH value of the boiling water bath liquefaction is adjusted to be 5.2-5.8.
6. The method for pretreatment of raw materials for fermentation production of wine according to claim 1, wherein: and in the second step, the saccharifying enzyme with the DE value of the saccharifying liquid after saccharifying by the saccharifying enzyme is added according to 150 mu/g-200 mu/g, the water bath temperature is 35 ℃, and the heat preservation time is 1 hour.
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