CN106501471B - A method of prediction low alcohol white spirit shelf life - Google Patents

A method of prediction low alcohol white spirit shelf life Download PDF

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Publication number
CN106501471B
CN106501471B CN201610944637.5A CN201610944637A CN106501471B CN 106501471 B CN106501471 B CN 106501471B CN 201610944637 A CN201610944637 A CN 201610944637A CN 106501471 B CN106501471 B CN 106501471B
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shelf life
white spirit
low alcohol
alcohol white
content
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CN106501471A (en
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吕志远
苏宁
张梦梦
钟其顶
李国辉
孟镇
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Jinan Baotu Spring Wine Co ltd
China National Research Institute of Food and Fermentation Industries
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JINAN BAOTU SPRING WINE CO Ltd
China National Research Institute of Food and Fermentation Industries
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/02Food
    • G01N33/14Beverages
    • G01N33/146Beverages containing alcohol

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  • Food Science & Technology (AREA)
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  • General Health & Medical Sciences (AREA)
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  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The present invention relates to a kind of methods for predicting low alcohol white spirit shelf life, and this method comprises the following steps: 1) setting in national standard total ester and the minimum of ethyl hexanoate content as shelf life reference value;And the predictive coefficient under the total ester of above-mentioned shelf life and ethyl hexanoate reference value is set as n;2) room temperature (T is detected0), high temperature (T1) content of total ester and ethyl hexanoate does matched curve as axis of ordinates using the natural logrithm of content, obtain slope K using the time as axis of abscissas in low alcohol white spirit during storage0、K1;3) according to the approximate rule of Hough (van ' t Hoff), temperature is every to rise 10 DEG C, and reaction rate increases n times, then has K1=K0×n(T1‑T0)/10, n value is calculated;5) high temperature (T is detected1) during storage in low alcohol white spirit total ester and ethyl hexanoate content, obtain high temperature T1Under the conditions of shelf life t1;6) room temperature (T0) under low alcohol white spirit shelf life t0=t1×n(T1‑T0)/10.The present invention detects low alcohol white spirit shelf life with the content of total ester and ethyl hexanoate, can quick predict its shelf life.

Description

A method of prediction low alcohol white spirit shelf life
Technical field
The present invention relates to a kind of methods for predicting low alcohol white spirit shelf life.Specifically, the present invention relates to can be when shorter The method of the interior shelf life for determining white wine.
Background technique
Shelf life is food a period of time experienced in the case where recommending holding conditions, and food is safe in the meantime, and Sense organ, physics and chemistry and microorganism property that consumer is expected are remain, and meets defined nutrient index on Product labelling Time.In actual production, prediction Food Shelf-life is a pith in food development and production process.Shelf life adds Speed experiment (ASLT, Accelerated shelf-life testing) is a kind of effectively and quickly prediction Food Shelf-life side Method is applied in food scientific research in large quantities, and principle is to quantify environmental factor to change using chemical kinetics Product is placed in some accelerate the failure and as improved the mal-condition of storage temperature gets off that product is accelerated to become by the influence degree for learning reaction Matter.Under the conditions of reserve temperature, sampling analysis index when certain time interval detects shelf life under this condition, then to obtain Data Extrapolation, and then determine physical holding of the stock under the conditions of shelf-life.
In recent years, as the improvement of people's living standards, the consumption idea of white wine is also changing.(40 ° of low alcohol white spirit V/v or less) because its irritation is small, wake up fastly after drink, gradually by the favor of consumer.But low alcohol white spirit is inclined due to alcoholic strength It is low, if the too long taste of shelf life can become boring, coordinate to feel poor, some even will appear water taste, tart flavour, astringent taste, bitter taste etc..
There are hydrolysis in low alcohol white spirit (40 ° of v/v or less), Ester is reduced, and acid increases, acid esters ratio It is unbalance, lead to lightly seasoned thin, the unhappy smell of appearance of white wine storage deutostoma.In white wine hydrolysis, reaction rate and esters and water Concentration it is directly proportional, reaction rate equation i.e.:Since Ester relative water concentration is lower, reacted Water concentration changes very little relative to ester concentration in journey, therefore can be approximately considered k ' × CWaterFor constant, enable: K ' × CWater=k;Reaction rate Equation is regarded as pseudo-first-order reaction rate equation:Definite integral will be carried out after formula variables separation:Integral result is InCEster tLinear equation with time t is once linear curve, measures different moments t When reaction system in total ester concentration CEster t, straight slope k, constant InCEster 0
In the prior art, sample is placed in room mainly based on observation analysis method by investigation low alcohol white spirit shelf life It is every to do subjective appreciation at regular intervals under the conditions of temperature, and the variation of key component is detected, until the taste of white wine, mouthfeel are not It is acceptable and until key component is reduced to national standard or less.This determination method takes a long time, improve low alcohol white spirit and The time that needs are studied during exploitation new product is long, and drain on manpower and material resources is larger.Therefore, up to the present there are no needles The method that low alcohol white spirit shelf life is quickly detected.
Summary of the invention
The main purpose that the present invention studies is a kind of method for establishing prediction low alcohol white spirit shelf life, in this way, The shelf life of white wine can be determined within a short period of time.
One aspect of the present invention provides a kind of method for predicting low alcohol white spirit shelf life, includes the following steps:
1) total ester and the minimum of ethyl hexanoate content are set in low alcohol white spirit as shelf life reference value;And set above-mentioned goods Predictive coefficient under frame phase total ester and ethyl hexanoate reference value is n;
2) tracing detection high temperature (T1) during storage in low alcohol white spirit total ester and ethyl hexanoate content, be cross with the time Reference axis does matched curve as axis of ordinates using the natural logrithm of content, obtains slope K1
3) tracing detection room temperature (T0) during storage in low alcohol white spirit total ester and ethyl hexanoate content, be cross with the time Reference axis, the logarithm of content are that axis of ordinates does matched curve, obtain slope K0
4) according to the approximate rule of Hough (van ' t Hoff), temperature is every to rise 10 DEG C, and reaction rate increases n times, then has K1 =K0×n(T1-T0)/10;
5) tracing detection high temperature (T1) during storage in low alcohol white spirit total ester and ethyl hexanoate content, obtain high temperature T1 Under the conditions of shelf life t1
6) room temperature (T0) under low alcohol white spirit shelf life t0=t1×n(T1-T0)/10
T in the present invention0It can be 20 DEG C;T1It can be 60 DEG C.
Preferably, in the method for the invention, every 5 months, 4 months, 3 under room temperature (15 DEG C -30 DEG C, preferably 20 DEG C) Measurement in a month, 2 months or 1 month is primary, and high temperature (preferably, the high temperature is 40~90 DEG C) is primary every measurement in 1 day.
Optionally, for the shelf life reference value, total ester (in terms of ethyl acetate) can be 1000mg/L;Ethyl hexanoate can For 500mg/L.
Preferably, the predictive coefficient n under the shelf life reference value can also be between 1.50-3.00.
The method that total ester and ethyl hexanoate are detected in the present invention can refer to 10345 Liquor Analysis Methods of GBT.Obviously , in addition to this, those skilled in the art can refer to any other analysis method.
Second aspect of the present invention provides a kind of method for predicting low alcohol white spirit shelf life, includes the following steps:
1) minimum of total ester, ethyl lactate and ethyl hexanoate content in low alcohol white spirit is set as shelf life reference value;And The predictive coefficient under the total ester of above-mentioned shelf life and ethyl hexanoate reference value is set as n;
2) tracing detection high temperature (T1) during storage in low alcohol white spirit total ester, ethyl lactate and ethyl hexanoate content, Using the time as axis of abscissas, matched curve is done as axis of ordinates using the natural logrithm of content, obtains slope K1
3) tracing detection room temperature (T0) during storage in low alcohol white spirit total ester, ethyl lactate and ethyl hexanoate content, Using the time as axis of abscissas, the logarithm of content is that axis of ordinates does matched curve, obtains slope K0
4) according to the approximate rule of Hough (van ' t Hoff), temperature is every to rise 10 DEG C, and reaction rate increases n times, then has K1 =K0×n(T1-T0)/10;
5) tracing detection high temperature (T1) during storage in low alcohol white spirit total ester, ethyl lactate and ethyl hexanoate content, Obtain high temperature T1Under the conditions of shelf life t1
6) room temperature (T0) under low alcohol white spirit shelf life t0=t1×n(T1-T0)/10
T in the present invention0It can be 20 DEG C;T1It can be 60 DEG C.
Preferably, in the method for the invention, every 5 months, 4 months, 3 under room temperature (15 DEG C -30 DEG C, preferably 20 DEG C) Measurement in a month, 2 months or 1 month is primary, and high temperature (preferably, the high temperature is 40~90 DEG C) is primary every measurement in 1 day.
Optionally, for the shelf life reference value, total ester (in terms of ethyl acetate) can be 1000mg/L;Ethyl lactate can For 400mg/L;Ethyl hexanoate can be 500mg/L.
Preferably, the predictive coefficient n under the shelf life reference value can also be between 1.50-3.00.
The method that total ester, ethyl lactate and ethyl hexanoate are detected in the present invention can refer to 10345 Liquor Analysis Methods of GBT. It is readily apparent that in addition to this, those skilled in the art can refer to any other analysis method.
In second aspect, the minimum of total ester, ethyl lactate and ethyl hexanoate content can be country's mark in low alcohol white spirit The minimum of total ester, ethyl lactate and ethyl hexanoate content in low alcohol white spirit specified in standard.
Low alcohol white spirit described in second aspect is preferably 40 ° of v/v white wine below in the present invention.
In second aspect of the present invention, the minimum of total ester, ethyl lactate and ethyl hexanoate content can be in low alcohol white spirit The minimum of total ester, ethyl lactate and ethyl hexanoate content in low alcohol white spirit specified in national standard.
Low alcohol white spirit described in second aspect of the present invention is preferably 40 ° of v/v white wine below.
The present invention predicts the shelf life of low alcohol white spirit with the content of total ester and ethyl lactate and/or ethyl hexanoate, is opening When sending out low alcohol white spirit new product, can quick predict its shelf life, reduce the investment of R&D cycle and manpower and material resources.The present invention may be used also To be used to detect the shelf life of existing procucts, present invention detection speed is fast, and generally requiring 7 days or so can complete.
Specific embodiment
The present invention is described in further detail combined with specific embodiments below, content to better understand the invention, but The present invention is not limited to following embodiments.
Embodiment 1
Take the finished product low wine sample of two bottles of new productions, number A, B are wherein saved under the conditions of 20 DEG C of A room temperature, every 3 Total ester of moon detection wine sample and the content of ethyl hexanoate;Saved under the conditions of 60 DEG C of B high temperature, every 1 day detection wine sample total ester and The content of ethyl hexanoate, detecting step is as follows,
The method for detecting total ester are as follows:
Wine sample 50.0mL is drawn in 250mL conical flask, adds 2 drop phenolphthalein indicators, with 0.1mol/L sodium hydroxide standard Titration solution is titrated to pink (being sure not excess), ml of record consumption standard solution of sodium hydroxide, then accurate addition 0.1mol/L standard solution of sodium hydroxide 25.00mL, shakes up, and is put into several beades, and loading onto condenser pipe, (cooling water temperature is preferably low In 15 DEG C), in the 30min that flows back on boiling water bath (when solution boils, the condenser pipe first drop condensate liquid that drips starts timing), remove, It is cooled to room temperature.Then, it is titrated with 0.1mol/L sulfuric acid standard titration solution, completely disappears blush just for its end Point, the volume of record consumption 0.1mol/L sulfuric acid standard titration solution;Ethanol solution (no ester) 50mL is drawn simultaneously, according to above-mentioned Method equally operates and does blank test, the volume of record consumption 0.1mol/L sulfuric acid standard titration solution, as total ester content It calculates.
The calculating of total ester content:
In formula;The mass concentration (in terms of ethyl acetate) of X --- --- total ester in sample, unit are gram per liter (g/L);
The actual concentrations of c --- --- sulfuric acid standard titration solution, unit are mole every liter (mol/L);
V0--- --- blank test sample consumes the volume of sulfuric acid standard titration solution, and unit is milliliter (mL);
V1The volume of --- --- sample consumption sulfuric acid standard titration solution, unit are milliliter (mL);
The numerical value of the molal weight of 88 --- --- ethyl acetate, unit are gram every mole (g/mol);
The volume of 50.0 --- --- pipette samples, unit are milliliter (mL).
Formula is brought the data into, the content of total ester can be obtained.
The method of ethyl hexanoate content is detected in the present invention are as follows: gas chromatography;
Chromatographic column: CP-Wax 57CB;Carrier gas (High Purity Nitrogen): flow velocity 1.0mL/min;Split ratio are as follows: 60:1;Tail blow for 26mL/min;Hydrogen: flow velocity 30mL/min;Air: flow velocity 400mL/min;Detector temperature: 250 DEG C;Sample injector temperature Degree: 250 DEG C;Temperature programming: 35 DEG C, 4min is kept;60 DEG C are raised to 4 DEG C/min;130 DEG C are raised to 10 DEG C/min;With 15 DEG C/ Min is raised to 210 DEG C, keeps 20min.
It draws 1mL wine sample to be added in sample injection bottle, be added 0.1mL inner mark solution (0.02%, volume fraction), mix laggard Sample obtains the content of ethyl acetate and ethyl hexanoate.
The content (mg/L) of total ester and ethyl hexanoate under the conditions of 60 DEG C of 1. high temperature of table
Time (moon) 0 0.033 0.067 0.100 0.133 0.167
Total ester 2650 2550 2500 2470 2450 2430
Ethyl hexanoate 1267 1204 1195 1167 1159 1085
The content (mg/L) of total ester and ethyl hexanoate under the conditions of 20 DEG C of 2. room temperature of table
Time (moon) 0 3 6 9 12 15
Total ester 2340 1920 1840 1815 1685 1410
Ethyl hexanoate 1515 1238 1129 976 865 790
During (60 DEG C) of tracing detection high temperature storages in low alcohol white spirit total ester and ethyl hexanoate content, be cross with the time Reference axis, the logarithm of content are that axis of ordinates does matched curve, obtain slope K1
During (20 DEG C) of tracing detection room temperature storages in low alcohol white spirit total ester and ethyl hexanoate content, be cross with the time Reference axis, the logarithm of content are that axis of ordinates does matched curve, obtain slope K0
According to the approximate rule of Hough (van ' t Hoff), K0×n(60-20)/10=K1, n is calculatedTotal ester=2.04;nEthyl hexanoate =2.19.
By taking total ester as an example: obtaining the shelf life t of low alcohol white spirit under high temperature (60 DEG C) according to matched curve1=1.98;
According to: t0=t1×n(T1-T0)/10;Obtain t0=34.32;
The shelf life t=28.75 of low alcohol white spirit under room temperature (20 DEG C) is obtained according to matched curve.
By taking ethyl hexanoate as an example: obtaining the shelf life t of low alcohol white spirit under high temperature (60 DEG C) according to matched curve1=1.18;
According to: t0=t1×n(T1-T0)/10;Obtain t0=27.14;
The shelf life t=29.97 of low alcohol white spirit under room temperature (20 DEG C) is obtained according to matched curve.
In order to evaluate the method for the present invention to the forecasting accuracy of low alcohol white spirit shelf life, the sample of number A is tasted and appraised Identification forms comment to verify its organoleptic indicator's situation of change.The result shows that aroma is not pure good enough when storage was to 30 months, Wine body is pure and mild, sour-puckery flavor.Before 26 months, aroma is pure, wine body is pure and mild, not discoordination.That is, for low wine, With the extension of resting period, mouthfeel is being gradually changed, and wine body is thin out, taste is few, and the later period also shows slightly acerbity.
In fact, also carrying out alcoholic strength, total acid, ethyl lactate, ethyl butyrate and ethyl acetate for measurement.Hair Existing, for low wine, these physical and chemical indexes or a combination thereof and the correspondence of sensory evaluation be not good enough, and total ester and caproic acid second The correspondence of index variation with the sensory evaluation of ester is significantly relatively strong.
Although with above embodiments describe the present invention, it should be appreciated that before without departing substantially from spirit of the invention It puts, the present invention further can be modified and be changed, and these modifications and variation all belong to the scope of protection of the present invention it It is interior.

Claims (8)

1. a kind of method for predicting low alcohol white spirit shelf life, includes the following steps:
1) total ester and the minimum of ethyl hexanoate content are set in low alcohol white spirit as shelf life reference value;
2) during tracing detection high temperature (T1) storage in low alcohol white spirit total ester and ethyl hexanoate content, using the time as abscissa Axis does matched curve as axis of ordinates using the natural logrithm of content, obtains slope K 1;
3) during tracing detection room temperature (T0) storage in low alcohol white spirit total ester and ethyl hexanoate content, using the time as abscissa Axis, the logarithm of content are that axis of ordinates does matched curve, obtain slope K 0;
4) according to the approximate rule of Hough, temperature is every to rise 10 DEG C, and reaction rate increases n times, then has K1=K0 × n(T1-T0)/10
5) during tracing detection high temperature (T1) storage in low alcohol white spirit total ester and ethyl hexanoate content, obtain high temperature T1 condition Under shelf life t1;
6) under room temperature (T0) low alcohol white spirit shelf life t0=t1 × n(T1-T0)/10
Predictive coefficient n under the shelf life reference value, range is in 1.50-3.00.
2. the method for prediction low alcohol white spirit shelf life according to claim 1, it is characterised in that the high temperature is 40-90 ℃。
3. the method for prediction low alcohol white spirit shelf life according to claim 1, it is characterised in that the room temperature is 15-30 ℃。
4. the method for predicting low alcohol white spirit shelf life according to claim 3, wherein the room temperature is 20 DEG C.
5. the method for low alcohol white spirit shelf life is predicted described in any one of -4 according to claim 1, it is characterised in that under room temperature Measurement is primary at quarterly intervals, primary every measurement in 1 day under high temperature.
6. the method for prediction low alcohol white spirit shelf life according to claim 5, it is characterised in that total ester and ethyl hexanoate Unit is mass concentration or is molar concentration.
7. the method for prediction low alcohol white spirit shelf life according to claim 1, it is characterised in that the minuent of the setting is white Total ester and the minimum of ethyl hexanoate content are minimum specified in national standard in wine.
8. the method for prediction low alcohol white spirit shelf life according to claim 1, it is characterised in that the low alcohol white spirit is each The white wine of kind odor type.
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Address after: 53 Longshan Road, Zhonggong Town, Licheng District, Jinan City, Shandong Province

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Denomination of invention: A method for predicting the shelf life of low alcohol Baijiu

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