CN103399009A - Method for detecting contents of glucose and starch in fermented grains - Google Patents
Method for detecting contents of glucose and starch in fermented grains Download PDFInfo
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Abstract
The invention discloses a method for detecting the contents of glucose and starch in fermented grains. The method for detecting the content of the glucose in fermented grains comprises the following steps: preparing fehling A liquid; preparing fehling B liquid; preparing a standard glucose solution with a concentration of 0.1%; calibrating a mixed solution of the fehling A liquid and the fehling B liquid by using the standard glucose solution, and recording the total consumption amount V1 of the standard glucose solution; respectively taking the fehling A liquid, the fehling B liquid and a fermented grain sample to be detected, mixing the three, and carrying out titration on the obtained mixture by using the standard glucose solution, and recording the use volume V3 of the fermented grain sample to be detected and the volume V2 of the standard glucose solution used for titration; and calculating to obtain the content of the glucose in the fermented grain sample according to the quantities of V1, V2 and V3 as well as the total mass of the fermented grain sample, and the total volume of sample preparation. According to the detecting method, the content of the glucose in the fermented grains can be accurately calculated, even if the content value is less than 1%.
Description
Technical field
The present invention relates to the brewed spirit field, in particular to the detection method of glucose content in a kind of wine unstrained spirits and content of starch.
Background technology
The white wine that uses solid state fermentation to produce, its saccharification, fermentation and distillation are all to carry out in the wine unstrained spirits under solid state, therefore the quality control of wine unstrained spirits is normally carried out and to produce Quality of Liquors significant guaranteeing to produce, and moisture, acidity, residual sugar and the analysis of starch physical and chemical index carried out in the wine unstrained spirits are importances of quality control, can grasp the content of These parameters in the wine unstrained spirits and find the problem in production, timely adjusting process parameter, production has positive directive function to white wine.
At present, the moisture of wine unstrained spirits and acidity analysis belong to classical analytical approach, and the analysis of grape sugar and starch is adopted, are reducing sugar methods, are to utilize oxygenant copper sulphate and the method that glucose response generates the copper oxidule precipitation of redness to measure.
The Fei Linshi standard solution that analysis grape sugar and starch is used is comprised of first liquid (cupric sulfate pentahydrate) and second liquid (sodium potassium tartrate tetrahydrate and NaOH), and its concentration is as follows:
Fei Linshi first liquid: the concentration of cupric sulfate pentahydrate is 69.278g/L;
Fei Linshi second liquid: the concentration of sodium potassium tartrate tetrahydrate and NaOH is respectively 349g/L and 100g/L;
Indicator: methylene blue;
Criterion: become redness as titration end-point by blueness take directing terminal.
Analytic process: get each 5mL of first, second liquid and certain volume solution to be measured and mix, standard glucose solution is vs, after micro-the boiling of heating on electric furnace, carries out pre-titration and formal titrimetry, and solution to be measured becomes redness by blueness, and titration finishes.
Wherein: while analyzing in solution to be measured content of starch, every 5.00g sample is that 20% hydrochloric acid solution becomes glucose sugar by the Starch Hydrolysis in the wine unstrained spirits with 100 ml concns, then carries out titration.
Analysis result: the content that calculates glucose or starch according to titration liquid glucose consumption.
The problem that exists: in wine brewing process usually, in wine unstrained spirits after fermentation, the content of glucose is only 2% left and right, particularly before secondary wine and six later wine unstrained spirits of wine, wherein the content of glucose is lower, and existing analytical approach can not be carried out quantitative measurement to content at the glucose below 1%.
Summary of the invention
The object of the present invention is to provide the detection method of glucose content in a kind of wine unstrained spirits, to address the above problem.
Another object of the present invention is to provide the detection method of content of starch in a kind of wine unstrained spirits.
The detection method of glucose content in a kind of wine unstrained spirits that provides in an embodiment of the present invention specifically comprises the following steps:
Preparing Fei Linshi first liquid, is the cupric sulfate pentahydrate solution of 15g/L and the methylene blue solution composition that concentration is 0.05g/L by concentration;
Preparing Fei Linshi second liquid, is the potassium sodium tartrate solution of 50g/L by concentration, and concentration is that the sodium hydroxide solution of 54g/L and potassium ferrocyanide solution that concentration is 8g/L form;
Preparation concentration is 0.1% standard glucose solution;
Use the mixed solution of described standard glucose standardization of solution described Fei Linshi first liquid and described Fei Linshi second liquid, the blueness of mixed solution sports light yellow, demarcates and finishes, and records the total amount consumed V of described standard glucose solution
1
Take respectively described Fei Linshi first liquid, described Fei Linshi second liquid and wine unstrained spirits sample to be measured, and mix, uses described standard glucose solution to carry out titration to it, in solution blueness sport light yellow, the titration end; The use volume V of record wine unstrained spirits sample described to be measured wherein
3The volume V of the described standard glucose solution that uses with titration
2
Wherein, described Fei Linshi first liquid and described Fei Linshi second liquid are long-pending identical, described V
2With described V
3In the glucose content summation equal described V
1Middle glucose content, and described V
31/2 of the long-pending summation of≤described Fei Linshi first liquid and described Fei Linshi second liquid;
According to described V
1, V
2, V
3Amount, and the gross mass M of wine unstrained spirits sample to be measured and sample prepare cumulative volume V
0Calculate the content of glucose in wine unstrained spirits sample.
In a kind of wine unstrained spirits provided by the invention, in the detection method of glucose content, record in demarcating the volume V of the sugared total amount that consumes
1, and by the volume V of the standard glucose solution that consumes in wine unstrained spirits sample titration process to be measured
2, be recorded in simultaneously the volume V of the wine unstrained spirits sample to be measured that adds in titration process
3, according to three bulking values of record, by the computing formula of glucose content in the wine unstrained spirits:
Can accurately calculate the content of glucose in the wine unstrained spirits, even content value also can record lower than 1%, in formula:
V
1-Fei Linshi first liquid and second liquid is quota of expenditure glucose solution volume in demarcation, mL;
V
2Quota of expenditure glucose solution volume in the formal titration of-sample, mL;
C-standard glucose solution concentration, g/mL;
V
3The volume that the pre-titration of-sample or formal titration add, mL;
The gross mass of M-wine unstrained spirits sample to be measured;
V
0-sample prepares cumulative volume.
The principle of drop reaction: the glucose that contains in wine unstrained spirits sample to be measured has reductibility, cupric in Fei Linshi first liquid can be reduced to monovalence copper, and generation copper oxidule precipitation, after cupric all is reduced, micro-excessive glucose can be reduced to methylene blue colourless by blueness, the cuprous oxide that generates simultaneously again with Fei Linshi second liquid in the ferrocyanide nak response generate the light yellow compound of solubility, ie in solution is changed into light yellow by blueness, the indication titration end-point arrives.Record thus the content of the reducing sugars such as glucose.Wherein because of the wine unstrained spirits, have acidity, and tartrate first sodium and potassium ferrocyanide are the alkalescent materials, use in NaOH and the acid in the wine unstrained spirits, make whole reaction carry out under alkali condition.
The detection method of content of starch in a kind of wine unstrained spirits specifically comprises the following steps:
Preparing Fei Linshi first liquid, is the cupric sulfate pentahydrate solution of 15g/L and the methylene blue solution composition that concentration is 0.05g/L by concentration;
Preparing Fei Linshi second liquid, is the potassium sodium tartrate solution of 50g/L by concentration, and concentration is that the sodium hydroxide solution of 54g/L and potassium ferrocyanide solution that concentration is 8g/L form;
Preparation concentration is the standard glucose solution of 0.1% (m/v);
Preparation concentration is 20%(v/v) hydrochloric acid solution;
Preparation concentration is 20% sodium hydroxide solution;
Use described hydrochloric acid solution hydrolysis wine unstrained spirits sample, through described sodium hydroxide solution, regulate the pH value and obtain wine unstrained spirits sample solution to be measured to neutrality;
Use described standard glucose standardization of solution described Fei Linshi second liquid and described Fei Linshi second liquid, record the total amount consumed V of described standard glucose solution
1
Take respectively the wine unstrained spirits sample described to be measured after described Fei Linshi first liquid, described Fei Linshi second liquid and hydrolysis, mix, uses described standard glucose solution to carry out titration to it, in solution blueness sport light yellow, the titration end; The use volume V of the wine unstrained spirits sample described to be measured after record hydrolysis wherein
3The volume V of the described standard glucose solution that uses with titration
2
Wherein, described Fei Linshi first liquid and described Fei Linshi second liquid are long-pending identical, described V
2With described V
3In the glucose content summation equal described V
1Middle glucose content, and described V
31/2 of the long-pending summation of≤described Fei Linshi first liquid and described Fei Linshi second liquid;
According to described V
1, V
2, V
3Amount, and use amount, gross mass and the cumulative volume of wine unstrained spirits sample to be measured calculate the content of starch in wine unstrained spirits solution.
In a kind of wine unstrained spirits provided by the invention in the detection method of content of starch, first give in wine unstrained spirits sample to be measured and add hydrochloric acid, by the Starch Hydrolysis in wine unstrained spirits sample to be measured, be glucose, re-use afterwards with titration wine unstrained spirits in the method for glucose, use the standard glucose solution of configuration to carry out titration to it, according to formula:
Finally calculate the content of starch in the wine unstrained spirits.In formula:
V
1Quota of expenditure glucose solution volume in-Fei Linshi standardization of solution, mL;
V
2Quota of expenditure glucose solution volume in the formal titration of-sample, mL;
C-standard glucose solution concentration, g/mL;
V
3The volume of sample that the pre-titration of-sample or formal titration add, mL;
0.9-glucose is scaled the coefficient of starch;
M-wine unstrained spirits sample use amount;
K-sample uses the ratio of volume and sample cumulative volume;
V
4The final constant volume that uses after the hydrolysis of-wine unstrained spirits.
Namely, starch in the wine unstrained spirits, under heating condition, by watery hydrochloric acid, be hydrolyzed to glucose, and the glucose that generates has reductibility, the cupric in the Fei Linshi agent can be reduced to monovalence copper, and generation copper oxidule precipitation, after cupric all was reduced, micro-excessive liquid glucose was reduced to methylene blue colourless by blueness, and the cuprous oxide of generation generates the light yellow compound of solubility with the ferrocyanide nak response again, ie in solution is changed into light yellow by blueness, the indication titration end-point arrives.Record thus the content of the reducing sugars such as glucose, and then obtain the content of starch in the wine unstrained spirits.
The accompanying drawing explanation
Fig. 1 is the detection method process flow diagram of glucose content in a kind of wine unstrained spirits of embodiment 1 provided by the invention;
Fig. 2 is the detection method process flow diagram of content of starch in a kind of wine unstrained spirits of embodiment 2 provided by the invention.
Embodiment
Below by specific embodiment, also by reference to the accompanying drawings the present invention is described in further detail.
Embodiment 1:
The detection method of glucose content in a kind of wine unstrained spirits as shown in Figure 1, specifically comprises the following steps:
101. prepare Fei Linshi first liquid, by concentration, be the cupric sulfate pentahydrate solution of 15g/L and the methylene blue solution composition that concentration is 0.05g/L;
102. prepare Fei Linshi second liquid, by concentration, be the potassium sodium tartrate solution of 50g/L, concentration is that the sodium hydroxide solution of 54g/L and potassium ferrocyanide solution that concentration is 8g/L form;
103. preparation concentration is 0.1% standard glucose solution;
104. use the mixed solution of described standard glucose standardization of solution described Fei Linshi first liquid and described Fei Linshi second liquid, the blueness of mixed solution sports light yellow, demarcates and finishes, and records the total amount consumed V of described standard glucose solution
1
105. take respectively described Fei Linshi first liquid, described Fei Linshi second liquid and wine unstrained spirits sample to be measured, and mix, uses described standard glucose solution to carry out titration to it, in solution blueness sport light yellow, the titration end; The use volume V of record wine unstrained spirits sample described to be measured wherein
3The volume V of the described standard glucose solution that uses with titration
2
Wherein, described Fei Linshi first liquid and described Fei Linshi second liquid are long-pending identical, described V
2With described V
3In the glucose content summation equal described V
1Middle glucose content, and described V
31/2 of the long-pending summation of≤described Fei Linshi first liquid and described Fei Linshi second liquid;
106. according to described V
1, V
2, V
3Amount, and the gross mass M of wine unstrained spirits sample to be measured and sample prepare cumulative volume V
0Calculate the content of glucose in wine unstrained spirits sample.
In a kind of wine unstrained spirits provided by the invention, in the detection method of glucose content, record in demarcating the volume V of the standard glucose solution that consumes
1, and by the volume V of the standard glucose solution that consumes in wine unstrained spirits sample titration process to be measured
2, be recorded in simultaneously the volume V of the wine unstrained spirits sample to be measured that adds in titration process
3, according to three bulking values of record, by the computing formula of glucose content in the wine unstrained spirits:
Can accurately calculate the content of glucose in the wine unstrained spirits, even content value also can record lower than 1%, in formula:
V
1-Fei Linshi first liquid and second liquid is quota of expenditure glucose solution volume in demarcation, mL;
V
2Quota of expenditure glucose solution volume in the formal titration of-sample, mL;
C-standard glucose solution concentration, g/mL.
V
3The volume that the pre-titration of-sample or formal titration add, mL.
The gross mass of M-wine unstrained spirits sample to be measured;
V
0-sample prepares cumulative volume.
The principle of drop reaction: the glucose that contains in wine unstrained spirits sample to be measured has reductibility, cupric in Fei Linshi first liquid can be reduced to monovalence copper, and generation copper oxidule precipitation, after cupric all is reduced, micro-excessive glucose can be reduced to methylene blue colourless by blueness, the cuprous oxide that generates simultaneously again with Fei Linshi second liquid in the ferrocyanide nak response generate the light yellow compound of solubility, ie in solution is changed into light yellow by blueness, the indication titration end-point arrives.Record thus the content of the reducing sugars such as glucose.Wherein because of the wine unstrained spirits, have acidity, and tartrate first sodium and potassium ferrocyanide are the alkalescent materials, use in NaOH and the acid in the wine unstrained spirits, make whole reaction carry out under alkali condition.
Embodiment 2:
The detection method of content of starch in a kind of wine unstrained spirits as shown in Figure 2, specifically comprises the following steps:
201. prepare Fei Linshi first liquid, by concentration, be the cupric sulfate pentahydrate solution of 15g/L and the methylene blue solution composition that concentration is 0.05g/L;
202. prepare Fei Linshi second liquid, by concentration, be the potassium sodium tartrate solution of 50g/L, concentration is that the sodium hydroxide solution of 54g/L and potassium ferrocyanide solution that concentration is 8g/L form;
203. preparation concentration is the standard glucose solution of 0.1% (m/v);
204. preparation concentration is 20% hydrochloric acid solution;
205. preparation concentration is 20% sodium hydroxide solution;
206. use described hydrochloric acid solution hydrolysis wine unstrained spirits sample, through described sodium hydroxide solution, regulate the pH value and obtain wine unstrained spirits sample solution to be measured to neutrality;
207. use described standard glucose standardization of solution described Fei Linshi first liquid and described Fei Linshi second liquid, record the total amount consumed V of described standard glucose solution
1
208. take respectively the wine unstrained spirits sample described to be measured after described Fei Linshi first liquid, described Fei Linshi second liquid and hydrolysis, mix, uses described standard glucose solution to carry out titration to it, in solution blueness sport light yellow, the titration end; The use volume V of the wine unstrained spirits sample described to be measured after record hydrolysis wherein
3The volume V of the described standard glucose solution that uses with titration
2
Wherein, described Fei Linshi first liquid and described Fei Linshi second liquid are long-pending identical, described V
2With described V
3In the glucose content summation equal described V
1Middle glucose content, and described V
31/2 of the long-pending summation of≤described Fei Linshi first liquid and described Fei Linshi second liquid;
209. according to described V
1, V
2, V
3Amount, and use amount, gross mass and the cumulative volume of wine unstrained spirits sample to be measured calculate the content of starch in wine unstrained spirits solution.
In a kind of wine unstrained spirits provided by the invention in the detection method of content of starch, first give in wine unstrained spirits sample to be measured and add hydrochloric acid, by the Starch Hydrolysis in wine unstrained spirits sample to be measured, be glucose, re-use afterwards with titration wine unstrained spirits in the method for glucose, use the standard glucose solution of configuration to carry out titration, according to formula:
Finally calculate the content of starch in the wine unstrained spirits.In formula:
V
1Quota of expenditure glucose solution volume in-Fei Linshi standardization of solution, mL;
V
2Quota of expenditure glucose solution volume in the formal titration of-sample, mL;
C-standard glucose solution concentration, g/mL.
V
3The volume of sample that the pre-titration of-sample or formal titration add, mL;
0.9-glucose is scaled the coefficient of starch;
M-wine unstrained spirits sample use amount;
K-sample uses the ratio of volume and sample cumulative volume;
V
4The final constant volume that uses after the hydrolysis of-wine unstrained spirits.
Starch in the wine unstrained spirits, under heating condition, by watery hydrochloric acid, be hydrolyzed to glucose, and the glucose that generates has reductibility, cupric in the Fei Linshi agent can be reduced to monovalence copper, and generate copper oxidule precipitation, after cupric all is reduced, micro-excessive liquid glucose is reduced to methylene blue colourless by blueness, the cuprous oxide that generates generates the light yellow compound of solubility with the ferrocyanide nak response again, and ie in solution is changed into light yellow by blueness, and the indication titration end-point arrives.Record thus the content of the reducing sugars such as glucose, and then obtain the content of starch in the wine unstrained spirits.
Embodiment 3:
The detection method of glucose content in a kind of wine unstrained spirits specifically comprises the following steps:
301. take 15g copper sulphate (CuSO
45H
2O), 0.050g methylene blue indicator is soluble in water, and be diluted to 1000mL and make Fei Linshi first liquid;
302. take 50.00g sodium potassium tartrate tetrahydrate (KNaC
4H
4O
64H
2O), 54g NaOH and 8.00g potassium ferrocyanide [K
4Fe(CN)
63H
2O] soluble in water and the dilution as for 1000.00mL, make Fei Linshi second liquid;
303. take 5g, in 103～105 ℃ of baking ovens, dry by the fire pure glucose cooling after 2 hours, after water dissolves, add 25mL hydrochloric acid, add water and be settled to 5000mL and make standard glucose solution;
304. Fei Linshi first liquid and Fei Linshi second liquid are respectively got 5ml, mix, insert in the 250mL conical flask, add water 10mL, with buret, add 9mL0.1% (m/v) standard glucose solution, shake up.Be placed on electric furnace and heat, be controlled in 2 minutes boiling, and keep micro-and boiled 2 minutes, under fluidized state, with the speed of 0.1% (m/v) standard glucose solution with 1 of per second, be titrated to blue disappearance and be light yellow.
This titration operation must complete in 1 minute, total boiling time is no more than 3 minutes, and the liquid glucose of dropping is no more than 1mL, otherwise the standard glucose amount of solution that once adds before should suitably increasing, titration again.And the sugared total amount V of the average consumption of record
1ML;
305. pre-titration: draw each 5mL of Fei Linshi solution first, second liquid, insert in the 250mL conical flask, add water 10mL, then the sample that adds 5.00mL to prepare, shake up.Put on electric furnace and heat, be controlled in 2 minutes boiling, and keep micro-and boiled 2 minutes, under fluidized state, with the speed of 0.1% (m/v) standard glucose solution with 1 of per second, be titrated to blue disappearance and be light yellow, record standard glucose solution consumption;
306. formal titration: draw each 5mL of Fei Linshi solution first, second liquid, insert in the 250mL conical flask, add water 10mL, then the sample that adds 5.00mL to prepare, then add 0.1% glucose standard solution than the few 1mL of pre-titration, shake up.Heating was seethed with excitement in 2 minutes on electric furnace, and kept boiling 2 minutes.Under fluidized state with 0.1% (m/v) standard glucose solution with the speed of 1 of per second be titrated to blueness sport light yellow, record standard glucose solution total amount consumed V
2ML.
307. calculate
In formula:
V
1Quota of expenditure glucose solution volume in-Fei Linshi standardization of solution, mL;
V
2Quota of expenditure glucose solution volume in the formal titration of-sample, mL;
C-standard glucose solution concentration, g/mL.
V
3The volume of sample that the pre-titration of-sample or formal titration add, mL.
Report the test is 2 significant digits.
Embodiment 4:
The detection method of content of starch in a kind of wine unstrained spirits specifically comprises the following steps:
401. take 15g copper sulphate (CuSO
45H
2O), 0.050g methylene blue indicator is soluble in water, and be diluted to 1000mL and make Fei Linshi first liquid;
402. take 50.00g sodium potassium tartrate tetrahydrate (KNaC
4H
4O
64H
2O), 54g NaOH and 8.00g potassium ferrocyanide [K
4Fe(CN)
63H
2O] soluble in water and the dilution as for 1000.00mL, make Fei Linshi second liquid;
403. take 5g, in 103～105 ℃ of baking ovens, dry by the fire pure glucose cooling after 2 hours, after water dissolves, add 25mL hydrochloric acid, add water and be settled to 5000mL and make standard glucose solution;
404. measure 4L water with the 1L graduated cylinder, put into the 5L beaker, then measure 1L hydrochloric acid, slowly add in beaker, and in adding the process of hydrochloric acid, constantly stir with glass bar that to make concentration be 20% hydrochloric acid solution;
405. take 100g NaOH, put into the 500ml beaker, water is dissolved to 500ml, and to make concentration be 20% sodium hydroxide solution;
406. the hydrolysis of wine unstrained spirits:
Accurately take the 5.0g sample, be placed in the 250mL conical flask, add the hydrochloric acid solution of 100mL water and 30mL, 6moL/L, shake gently conical flask, make sample fully moistening;
Bottleneck is loaded onto the bottle stopper that condenser pipe or band are about 1 meter glass-tube, puts in boiling water bath and refluxes 30 minutes, takes out, and is cooling with flowing water.With absorbent cotton, filter, filtrate receives with the 500mL volumetric flask, and water fully washs conical flask and residue, and washing lotion is all filtered in volumetric flask, is diluted with water to scale, shakes up;
Then use 50mL pipette, extract 50mL hydrolyzate in the 100mL volumetric flask, with 20% sodium hydroxide solution neutralization, with the accurate pH test paper test, make the pH value of aqueous solution be about 7, finally add water to scale, shake up;
407. Fei Linshi standardizing of solution:
Draw each 5mL of Fei Linshi solution first, second liquid, insert in the 250mL conical flask, add water 10mL, with buret, add 9mL0.1% (m/v) standard glucose solution, shake up;
Be placed on electric furnace and heat, be controlled in 2 minutes boiling, and keep micro-and boiled 2 minutes;
Under fluidized state, with 0.1% (m/v) standard glucose solution, with the speed of 1 of per second, being titrated to blueness sports light yellow;
This titration operation must complete in 1 minute, total boiling time is no more than 3 minutes, and the liquid glucose of dropping is no more than 1mL, otherwise the glucose standard solution amount that once adds before should suitably increasing, titration again.And the sugared total amount V of the average consumption of record
1ML;
408. the pre-titration of sample:
Draw each 5mL of Fei Linshi solution first, second liquid, insert in the 250mL conical flask, add water 10mL, then the sample that adds 2.00ml to prepare, shake up;
Put on electric furnace and heat, be controlled in 2 minutes boiling, and keep micro-and boiled 2 minutes, under fluidized state, with the speed of 0.1% (m/v) standard glucose solution with 1 of per second, be titrated to blue disappearance and be light yellow, record standard glucose solution consumption;
409. formal titration:
Draw each 5mL of Fei Linshi solution first, second liquid, insert in the 250mL conical flask, add water 10mL, then the sample that adds 2.00mL to prepare, then add 0.1% glucose standard solution than the few 1mL of pre-titration, shake up;
Heating was seethed with excitement in 2 minutes on electric furnace, and kept boiling 2 minutes.Under fluidized state, with the speed of 0.1% (m/v) standard glucose solution with 1 of per second, be titrated to blue the disappearance and be light yellow, record standard glucose solution total amount consumed V
2ML;
410. calculate
In formula:
V
1Quota of expenditure glucose solution volume in-Fei Linshi standardization of solution, ml;
V
2Quota of expenditure glucose solution volume in the formal titration of-sample, ml;
C-standard glucose solution concentration, g/ml.
5-sample mass, g;
V
3The volume of sample that the pre-titration of-sample or formal titration add, ml;
0.9-glucose is scaled the coefficient of starch.
Report the test is 2 significant digits.
The invention provides glucose content in a kind of wine unstrained spirits and the detection method of content of starch, can carry out quantitative test to low residual sugar below 1%, simultaneously, measure while reaching terminal analyzing, change color is more directly perceived, more accurately judges terminal.
Embodiment 5
By the replicate analysis to 10 samples (precision test) and glucose sugar mark-on test (recovery test), and with former analytical approach contrast test (former analytical approach test 3 times, average), draw following 3 tables of data:
Table 1 precision test tables of data
Conclusion: draw from analyzing 10 sample datas, residual sugar index determining absolute error maximal value is that relative average debiation is followed successively by: 1.0%, 1.1%, 2.0%, 1.1%, 1.3%, 0.93%, 0.84%, 0.81%, 1.08%, 0.67%, starch index determining absolute error maximal value is that the 0.28%(analysis requires as ± 0.3%), relative average debiation is followed successively by: 0.16%, 0.14%, 0.12%, 0.16%, 0.12%, 0.09%, 0.10%, 0.08%, 0.11%, 0.08%, analysis requires relative average debiation to be no more than 2% according to test method, reaches the analysis requirement.
Table 2 residual sugar recovery test tables of data
Conclusion: after adding the glucose titer, measure, calculate the rear average recovery rate of mark-on 2% equal 99.1%, the rear average recovery rate 99.4% of mark-on 5%, illustrate that this analytical approach accuracy is high.
Table 3 and the former test method table of comparisons
Conclusion: by two analytical approach contrasts, residual sugar and starch index analysis error be (the residual sugar analysis requires to be less than or equal to 0.5) between 0～± 0.5, starch index analysis error is (the starch analysis requires to be less than or equal to 1.0) between 0～± 0.7, meets and analyzes requirement.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. the detection method of glucose content in a wine unstrained spirits, is characterized in that, specifically comprises the following steps:
Preparing Fei Linshi first liquid, is the cupric sulfate pentahydrate solution of 15g/L and the methylene blue solution composition that concentration is 0.05g/L by concentration;
Preparing Fei Linshi second liquid, is the potassium sodium tartrate solution of 50g/L by concentration, and concentration is that the sodium hydroxide solution of 54g/L and potassium ferrocyanide solution that concentration is 8g/L form;
Preparation concentration is 0.1% standard glucose solution;
Use the mixed solution of described standard glucose standardization of solution described Fei Linshi first liquid and described Fei Linshi second liquid, the blueness of mixed solution sports light yellow, demarcates and finishes, and records the total amount consumed V of described standard glucose solution
1
Take respectively described Fei Linshi first liquid, described Fei Linshi second liquid and wine unstrained spirits sample to be measured, and mix, uses described standard glucose solution to carry out titration to it, in solution blueness sport light yellow, the titration end; The use volume V of record wine unstrained spirits sample described to be measured wherein
3The volume V of the described standard glucose solution that uses with titration
2
Wherein, described Fei Linshi first liquid and described Fei Linshi second liquid are long-pending identical, described V
2With described V
3In the glucose content summation equal described V
1Middle glucose content, and described V
31/2 of the long-pending summation of≤described Fei Linshi first liquid and described Fei Linshi second liquid;
According to described V
1, V
2, V
3Amount, and the gross mass of wine unstrained spirits sample to be measured and sample prepare the content that cumulative volume calculates glucose in wine unstrained spirits sample.
2. the detection method of glucose content in a kind of wine unstrained spirits according to claim 1, is characterized in that, the concrete grammar of preparing described Fei Linshi first liquid comprises:
Ratio according to 300:1 takes respectively cupric sulfate pentahydrate and methylene blue;
By the two soluble in water stirring;
Wherein in every 1000mL solution, add 15g cupric sulfate pentahydrate and 0.05g methylene blue.
3. the detection method of glucose content in a kind of wine unstrained spirits according to claim 1, is characterized in that, the concrete grammar of preparing described Fei Linshi second liquid comprises:
Ratio according to 25:27:4 takes respectively sodium potassium tartrate tetrahydrate, NaOH and potassium ferrocyanide;
By equal soluble in water the stirring of described sodium potassium tartrate tetrahydrate, NaOH and potassium ferrocyanide;
Wherein in every 1000mL solution, add 50g sodium potassium tartrate tetrahydrate, 54g NaOH and 8g potassium ferrocyanide.
4. the detection method of glucose content in a kind of wine unstrained spirits according to claim 1, is characterized in that,
Preparation concentration is in the step of 0.1% standard glucose solution, specifically comprises:
Take 5g and in 103 ℃～105 ℃ baking ovens, toast cooling pure glucose after 2 hours;
After being dissolved, described pure glucose water adds 25mL hydrochloric acid;
Add water and be settled to 5000mL.
5. the detection method of glucose content in a kind of wine unstrained spirits according to claim 1, is characterized in that,
Use in the step of mixed solution of described standard glucose standardization of solution described Fei Linshi first liquid and described Fei Linshi second liquid, specifically comprise:
Get described Fei Linshi first liquid and described each 5mL of Fei Linshi second liquid, insert in the 250mL conical flask;
Add 10mL water, and add the described standard glucose solution of 9mL with buret, shake up;
Be placed on electric furnace and be heated to boiling;
Under fluidized state, with described standard glucose solution, continue to be titrated to the solution blueness and sport light yellowly, stop titration, record the total amount consumed V of described standard glucose solution
1ML.
6. the detection method of glucose content in a kind of wine unstrained spirits according to claim 1, is characterized in that,
Take respectively described Fei Linshi first liquid, described Fei Linshi second liquid and wine unstrained spirits sample to be measured, and mix, use described standard glucose solution to carry out, in the step of titration, specifically comprising to it:
Pre-titration and formal titration.
7. the detection method of glucose content in a kind of wine unstrained spirits according to claim 6, is characterized in that,
Described pre-titration specifically comprises the steps:
Get described Fei Linshi first liquid and described each 5mL of Fei Linshi second liquid, insert in the 250mL conical flask, add water 10mL, then add described V
3The wine unstrained spirits solution described to be measured of volume, shake up;
Be placed on electric furnace and be heated to boiling;
Under fluidized state, with described standard glucose solution volumetric soiutions color, by blueness, sported light yellowly, stop titration, record standard glucose solution consumption.
8. the detection method of glucose content in a kind of wine unstrained spirits according to claim 6, is characterized in that,
Described formal titration specifically comprises the steps:
Get described Fei Linshi first liquid and described each 5mL of Fei Linshi second liquid, insert in the 250mL conical flask, add water 10mL, add with described pre-titration in add the wine unstrained spirits solution V described to be measured that volume is identical
3ML, then add the described standard glucose solution than the few 1mL of volume of the described standard glucose solution that consumes in described pre-titration, shake up;
On electric furnace, be heated to boiling;
Under fluidized state, with described standard glucose solution, with the speed of 1 drops/sec, be titrated to blueness and sport light yellowly, stop titration, record the total amount consumed V of described standard glucose solution
2ML.
9. the detection method of content of starch in a wine unstrained spirits, is characterized in that, specifically comprises the following steps:
Preparing Fei Linshi first liquid, is the cupric sulfate pentahydrate solution of 15g/L and the methylene blue solution composition that concentration is 0.05g/L by concentration;
Preparing Fei Linshi second liquid, is the potassium sodium tartrate solution of 50g/L by concentration, and concentration is that the sodium hydroxide solution of 54g/L and potassium ferrocyanide solution that concentration is 8g/L form;
Preparation concentration is the standard glucose solution of 0.1% (m/v);
Preparation concentration is 20%(v/v) hydrochloric acid solution;
Preparation concentration is 20% sodium hydroxide solution;
Use described hydrochloric acid solution hydrolysis wine unstrained spirits sample, through described sodium hydroxide solution, regulate the pH value and obtain wine unstrained spirits sample solution to be measured to neutrality;
Use described standard glucose standardization of solution described Fei Linshi second liquid and described Fei Linshi second liquid, record the total amount consumed V of described standard glucose solution
1
Take respectively the wine unstrained spirits sample described to be measured after described Fei Linshi first liquid, described Fei Linshi second liquid and hydrolysis, mix, uses described standard glucose solution to carry out titration to it, in solution blueness sport light yellow, the titration end; The use volume V of the wine unstrained spirits sample described to be measured after record hydrolysis wherein
3The volume V of the described standard glucose solution that uses with titration
2
Wherein, described Fei Linshi first liquid and described Fei Linshi second liquid are long-pending identical, described V
2With described V
3In the glucose content summation equal described V
1Middle glucose content, and described V
31/2 of the long-pending summation of≤described Fei Linshi first liquid and described Fei Linshi second liquid;
According to described V
1, V
2, V
3Amount, and use amount, gross mass and the cumulative volume of wine unstrained spirits sample to be measured calculate the content of starch in wine unstrained spirits solution.
10. the detection method of content of starch in a kind of wine unstrained spirits according to claim 9, is characterized in that,
Use described hydrochloric acid solution hydrolysis wine unstrained spirits sample, through described sodium hydroxide solution, regulate the pH value and obtain, in the step of wine unstrained spirits sample solution to be measured, specifically comprising to neutrality:
Take described wine unstrained spirits sample 5.0g to be measured, be placed in the 250mL conical flask, add the described hydrochloric acid solution of 100mL water and 30mL, with absorbent cotton, filter, receive filtrate;
Water fully washs conical flask and residue, and washing lotion is all filtered in volumetric flask, is diluted with water to 500mL, shakes up;
With 50mL pipette, extract 50mL hydrolyzate, in the 250mL volumetric flask, with described sodium hydroxide solution neutralization, with the accurate pH test paper test, make the pH value of aqueous solution be about 7, add water to 250mL, shake up.
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| CN111398213A (en) * | 2020-04-08 | 2020-07-10 | 四川虹微技术有限公司 | Method for judging eligibility of fermented grain model |
| CN112505128A (en) * | 2020-11-30 | 2021-03-16 | 北方民族大学 | Method and device for nondestructive testing of reducing sugar of wine |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103698328A (en) * | 2013-12-31 | 2014-04-02 | 中国农业科学院柑桔研究所 | Reducing sugar direct titration method capable of improving titration accuracy |
| CN103698328B (en) * | 2013-12-31 | 2017-07-18 | 中国农业科学院柑桔研究所 | A kind of reduced sugar direct titrimetric method for improving titration precision |
| CN103728269A (en) * | 2014-01-14 | 2014-04-16 | 安徽古井贡酒股份有限公司 | Method for near infrared rapid detection of physical and chemical indicators in wine stock |
| CN104215737A (en) * | 2014-09-01 | 2014-12-17 | 梁山正大菱花生物科技有限公司 | Revertose detection method |
| CN104215737B (en) * | 2014-09-01 | 2016-02-17 | 梁山正大菱花生物科技有限公司 | A kind of reducing sugar detection method |
| CN105548077A (en) * | 2015-12-07 | 2016-05-04 | 中国水稻研究所 | Method for determining total starch content of rice by refractive index |
| CN105548077B (en) * | 2015-12-07 | 2018-05-15 | 中国水稻研究所 | Utilize the method for total starch content in index determination rice |
| CN106468662A (en) * | 2016-10-10 | 2017-03-01 | 江南大学 | The assay method of content of starch in a kind of high sugar meat productss |
| CN110133179A (en) * | 2019-06-20 | 2019-08-16 | 邹文海 | A kind of reduced sugar Test paper and its application method |
| CN111398213A (en) * | 2020-04-08 | 2020-07-10 | 四川虹微技术有限公司 | Method for judging eligibility of fermented grain model |
| CN112505128A (en) * | 2020-11-30 | 2021-03-16 | 北方民族大学 | Method and device for nondestructive testing of reducing sugar of wine |
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