CN105733909B - A kind of method of urea in reduction yellow rice wine - Google Patents
A kind of method of urea in reduction yellow rice wine Download PDFInfo
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- CN105733909B CN105733909B CN201610260227.9A CN201610260227A CN105733909B CN 105733909 B CN105733909 B CN 105733909B CN 201610260227 A CN201610260227 A CN 201610260227A CN 105733909 B CN105733909 B CN 105733909B
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12H—PASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
- C12H1/00—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
- C12H1/02—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material
- C12H1/04—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material with the aid of ion-exchange material or inert clarification material, e.g. adsorption material
- C12H1/0416—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material with the aid of ion-exchange material or inert clarification material, e.g. adsorption material with the aid of organic added material
- C12H1/0424—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material with the aid of ion-exchange material or inert clarification material, e.g. adsorption material with the aid of organic added material with the aid of a polymer
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Abstract
The invention discloses a kind of methods of urea in reduction yellow rice wine, belong to food technology technology and field of food safety.Single batch, multiple batches of and pillar continuous processing is respectively adopted to the preferable resin material of adsorption effect using the urea in specific resins material adsorption treatment yellow rice wine in the present invention.The results show that the removal rate of single treatment urea, between 32%~49%, the wine sample of high urea concentration is through multiple adsorption treatment, and the removal rate of urea is 75% or more.The removal rate of pillar continuous processing urea is between 25%~37%.The basic physical and chemical index of wine sample and main flavor are kept preferably after absorption, this technology can be used for the removal of urea in yellow rice wine, are provided safeguard for the control of EC.
Description
Technical field
The present invention relates to a kind of methods of urea in reduction yellow rice wine, belong to food technology technology and field of food safety.
Background technique
Urethanes (Ethyl carbamate, abbreviation EC) is widely present in fermented food and alcoholic beverage, is
A kind of spontaneous substance.2007, EC was set to 2A class carcinogen by international cancer research institution (IARC), with acryloyl
The equivalent danger of amine.Traditional zymotic wine of the yellow rice wine as China, the content of EC are generally greater than other brewing Wines.Control EC's
Content is most important for the development for improving the quality and industry of yellow rice wine.
EC in yellow rice wine is mainly to be formed by urea, and the concentration for reducing urea is the key that control EC content.Common city
The concentration range for selling urea in yellow rice wine is 7mg/L~35mg/L, both at home and abroad according to the source of urea mainly using the acid urea of addition
The methods of enzyme, yeast genes transformation reduce urea content.Although these methods have the removal of urea according to the literature
Certain effect, but there is also certain problems, and such as: country's acid urease not yet realizes industrialized production at present, and addition is acid
Urase increases the economic cost of yellow rice wine, and when urea concentration is lower than 10mg/L, the catalytic efficiency of enzyme becomes extremely low；The base of yeast
Because there may be certain safety issues for transformation, it is also possible to change the flavor and taste etc. of yellow rice wine.
Summary of the invention
In view of the problems of the existing technology, it is an object of the invention to not change the existing production technology of yellow rice wine and make micro-
Biology is simultaneously kept under the precursor of rice wine flavor and basic physical and chemical index, provides a kind of economic, safe and effective method reduction Huang
The concentration of urea in wine, mainly including the use of resin adsorption material.Handle urea concentration range 5mg/L~40mg/L, pH 4.0
The concentration that left and right, effectively absorption reduce urea, provides safeguard for the control of EC content.
Technical solution of the present invention: urea-NH is utilized2Ion exchange can occur with resin adsorption material with-CO group
Characteristic, select adsorbent material appropriate, do not changing the existing production technology of yellow rice wine and brewing and keeps rice wine flavor at microorganism
Under the precursor of basic physical and chemical index, the urea content in yellow rice wine is reduced in absorption, to reduce the formation of EC in yellow rice wine.
A kind of method reducing urea in alcoholic drink provided by the invention, is to handle yellow rice wine with adsorbent material；The processing
It is to vibrate adsorption treatment 4h~40h at 10 DEG C~50 DEG C, 120-180r/min or chromatographic column is added in adsorbent material, 10
DEG C~50 DEG C at, with the continuous processing yellow rice wine of 0.5-2BV/h.
In one embodiment of the invention, the skeleton of the adsorbent material is acrylic copolymer, and type is weak acid
Property resin cation material, including C258FD, 117,112, D113 etc..
In one embodiment of the invention, the additive amount of the adsorbent material is the 10%~30% of yellow rice wine.
In one embodiment of the invention, the adsorbent material will be pre-processed first, be used further to processing yellow rice wine；Institute
Stating pretreatment is to clean adsorbent material, is then impregnated with NaOH and NaCl solution, then wash to neutrality, then soaked with HCl solution
Bubble, then washing, ethyl alcohol are impregnated, are washed again.
In one embodiment of the invention, the pretreatment of the adsorbent material, specifically: the absorption of 50mL humid volume
Material is cleaned to water outlet with deionized water without muddy, free from admixture, impregnates 8h with the NaCl solution of the NaOH of 100mL 3% and 7%
After be washed with deionized water to neutrality, then 8h is impregnated with the HCl solution of 100mL 3%, deionized water is washed till pH=4.0,90% second
It is spare that no alcohol taste is washed to after alcohol immersion 4h.
In one embodiment of the invention, the processing is to carry out batch processing, carries out oscillation absorption more than twice
Processing.
In one embodiment of the invention, the urea concentration range in the yellow rice wine is between 5mg/L~40mg/L.
In one embodiment of the invention, the method is specifically:
(1) pretreatment adsorbed: the adsorbent material of 50mL humid volume is cleaned to water outlet with deionized water without muddiness, without miscellaneous
Matter is washed with deionized water after impregnating 8h with the NaCl solution of the NaOH of 100mL 3% and 7% to neutrality, then with 100mL's 3%
HCl solution impregnates 8h, and deionized water is washed till pH=4.0, and it is spare to be washed to no alcohol taste after 90% ethyl alcohol immersion 4h；
(2) batch processing or continuous processing；Wherein, batch processing is: taking 100mL yellow rice wine, addition step (1) pretreatment
Good adsorbent material (additive amount 10%~30%) handles 4h~40h in 10 DEG C~50 DEG C, 150r/min；Continuous processing is: will
Chromatographic column is added in the adsorbent material that step (1) is handled well, at 40 DEG C, with the flow velocity adsorption treatment yellow rice wine of 1.5BV/h；
(3) multiple adsorption treatment: the higher yellow rice wine of urea concentration is handled multiple according to step (2).
In one embodiment of the invention, in yellow rice wine handled by step (2) removal rate of urea 32%~49%
Between, the physical and chemical index of wine sample and flavor are close with former wine sample after processing.Wherein pillar continuous processing is easy to operate, treating capacity
Greatly, it can effectively reduce the concentration of urea in yellow rice wine.
In one embodiment of the invention, step (3) treated yellow rice wine, the removal rate of urea is 75% or more.
Preferable is kept to the flavor of yellow rice wine and physical and chemical index after absorption.
In one embodiment of the invention, step (4) processing after, the removal rate of urea between 25%~37%,
The physical and chemical index of wine sample and flavor are close with former wine sample after processing.Pillar continuous processing is easy to operate, efficiently reduces and urinates in yellow rice wine
The concentration of element.
Beneficial effects of the present invention:
(1) method of the invention haves no need to change the existing production technology of yellow rice wine and brewing microorganism, but also is able to maintain Huang
Wine taste and basic physical and chemical index；
(2) the method for the present invention can handle yellow rice wine of the urea concentration between 5mg/L~40mg/L, and removal rate is up to 75%
More than；
(3) adsorbent material of the invention is commercially available product, and source is wide, is not needed using specific
Technique is voluntarily prepared, and industrial applications are conducive to.
Detailed description of the invention:
Fig. 1: mixed packing column formula processing unit of the invention；
Fig. 2: the selection result figure of adsorbent material；
Fig. 3: influence of the treatment conditions to adsorption effect；(a) treatment temperature, (b) processing time, (c) resin content,
(d) urea concentration；
Specific embodiment
1, yellow rice wine wine sample: commercially available yellow rice wine (semi-sweet or half-dry type, urea concentration 5.0~40.0mg/L of range, alcoholic strength model
Enclose 10.0~16.8%vol).
2, it is molten that urea titer, 1.5mol/L hydrochloric acid solution, 0.02mol/L 9- hydroxyl ton the measurement of urea concentration: are prepared
Liquid and sodium acetate solution.Sample pre-treatments: 500 μ L wine samples are diluted to 1000 μ L with chromatography straight alcohol, and 100 μ L 1.5mol/ are added
L HCl and 400 μ L 0.02mol/L 9- hydroxyl tons, whirlpool concussion 1min are uniformly mixed it, and room temperature is protected from light derivative 30min, adopts
It is to be measured with 0.22 μm of organic system syringe filter.Chromatographic condition: chromatographic column: C18 chromatographic column (Zorbax SB-Aq250mm
× 4.6mm, 5 μm), column temperature: 35 DEG C, sample temperature: 25 DEG C, fluorescence detector: λex=234nm, λem=600nm, sample volume:
10μL.Mobile phase A: 0.02mol/L sodium acetate (pH:7.2), Mobile phase B: acetonitrile, flow velocity: 0.8mL/min.Standard curve: with
The alcohol water blend of 15%vol prepares the urea titer with a certain concentration gradient, according to processing method identical with sample
Analysis measurement.Using the peak area of urea as abscissa, the concentration of urea is ordinate, establishes standard curve.
3, the measurement measurement of total acid, total amino acid state nitrogen content is referring to national standard GB/T 13662-2008 yellow rice wine.
4, flavor substance measures: taking 8mL wine sample in 20mL ml headspace bottle, 3.1g NaCl is added and is saturated, and in addition
Mark solution 10uL (octyl propionate, 55.8 μ g/L of final concentration；Methyl caproate, 95.6 μ g/L of final concentration), bottle cap is screwed, HS- is carried out
SPME.Extraction conditions: using three phase extraction head (DVB/CAR/PDMS, 50/30 μm), reserve 5min at 50 DEG C, and rear extraction is inhaled
Attached 45min, and GC desorbs 5min at 250 DEG C.
GC condition: chromatographic column is DB-Wax (60m × 0.32mm × 0.25 μm)；Temperature program: keeping 2min at 50 DEG C, with
The rate of 4 DEG C/min is warming up to 230 DEG C, and keeps 15min；250 DEG C of injector temperature, carrier gas He, flow velocity 2mL/min；Sample introduction
1 μ L is measured, is not shunted.MS condition: EI ionization source, 230 DEG C of ion source temperature, electron energy 70eV, scanning range 35.0~
350.0。
5, adsorbent material: heavy metal chelating material (Cu2+Type and Zn2+Type) and macroreticular resin material won honour for industry by Zhejiang
Limited liability company and Jiangsu Suqing Water Treatment Engineering Group Co., Ltd. provide, and are food-grade.
Embodiment 1: the screening of adsorbent material
Adsorbent material: it is mentioned by Zhejiang Province Zhengguan Industry Co., Ltd and Jiangsu Suqing Water Treatment Engineering Group Co., Ltd.
For being food-grade, material type and property are as shown in table 1.
1 adsorbent material property of table
The urea in yellow rice wine is reduced using following steps:
(1) pretreatment adsorbed: the adsorbent material of 50mL humid volume is cleaned to water outlet with deionized water without muddiness, without miscellaneous
Matter is washed with deionized water after impregnating 8h with the NaCl solution of the NaOH of 100mL 3% and 7% to neutrality, then with 100mL's 3%
HCl solution impregnates 8h, and deionized water is washed till pH=4.0, and it is spare to be washed to no alcohol taste after 90% ethyl alcohol immersion 4h；
(2) it takes 10mL humid volume material into 250mL ground triangular flask, and adds 100mL yellow rice wine, 30 DEG C of shaking table temperature,
Revolving speed 150r/min, concussion are handled for 24 hours.It takes supernatant to measure its urea concentration, is calculated with adsorbing the content of front and back urea concentration
Urea clear index.Treated wine sample makees preliminary analysis from color and fragrance compared with former wine sample simultaneously.
Different adsorbent materials are as shown in Figure 2 to the removal rate of urea.Resin material N, R (R C258FD, 117,112 or
D113 (being greater than 40%)) higher to the removal rate of urea, the influence to physical and chemical index is investigated respectively.
Treated that yellow rice wine physical and chemical index is as shown in table 2 by resin N, R.Although resin N is higher than resin to the removal rate of urea
R, the influence to ethyl alcohol and total reducing sugar is smaller (change rate is less than 10%), but (becomes to total amino acid state nitrogen and being affected for total acid
40%) rate is greater than.And the total amino acid state nitrogen of wine sample and total acid change rate are less than 14% after resin R processing, it contains after absorption
Amount (light half-dried yellow rice wine: total amino acid state nitrogen >=0.5g/L still within the scope of national standard；2.5~7.0g/L of total acid), and locate
The color of wine sample and former wine be relatively after reason.
The main conventional index analysis of yellow rice wine before and after 2 adsorption treatment of table
Embodiment 2: influence of the resin treatment condition to removal yellow rice wine urea effect
On the basis of embodiment 1, using R resin as adsorbent material, it is dense that temperature, time, adsorbent amount, urea are had studied
The influence to effect is spent, as a result as shown in Figure 3.
For the higher yellow rice wine sample (urea concentration 37.5mg/L) of urea concentration, the removal rate of urea is with treatment temperature
As shown in Fig. 3 (a), 40 DEG C are used as optimum treatmenting temperature for variation.
Further, urea is handled shown in the variation such as Fig. 3 (b) of removal rate with the processing time in 40 DEG C of resin adsorptions to use
It is used as the most suitable processing time for 24 hours.
Further, 40 DEG C of resin adsorptions for 24 hours under, have studied influence of the resin content to urea clear index, as a result such as
Shown in Fig. 3 (c), it is advisable using 10% resin content.
In addition, be investigated 40 DEG C, additive amount be 10% resin adsorption for 24 hours under, the yellow rice wine sample of different urea concentrations
The removal rate of urea in product, as a result such as table 3 and Fig. 3 (d), it can keep 32% under the urea concentration of 5~40mg/L~
49% removal rate.
The different urea concentration yellow rice wine resin adsorption effects of table 3
Embodiment 3: removal effect of the multiple adsorption treatment to high urea concentration yellow rice wine
On the basis of embodiment 1, using R resin as adsorbent material, 40 DEG C, resin content 10%, adsorption time for 24 hours
Under, carry out multiple absorption method processing, the urea concentration of wine sample 3 and wine sample 6, main physical and chemical index, main flavor such as table 4,
Shown in table 5.
The result of more than 4 adsorption treatments of table compares
Note: before 0 processing；1 single treatment；2 are handled twice；3 are handled three times.
Influence of 5 adsorption treatment of table to yellow rice wine main flavor
As shown in Table 4, the method for the present invention can not only significantly reduce the concentration of urea, and will not influence yellow rice wine substantially
Main physical and chemical index.As shown in Table 5, it is handled even across multiple, main flavor ingredient total difference in two groups of yellow rice wine samples
Less, flavor skeleton system of the wine sample after absorption than more fully maintaining former wine sample.As it can be seen that this resin sorption processes energy
Enough compared with the urea in specific adsorption yellow rice wine, the flavor of yellow rice wine still can preferably be kept after multiple adsorption treatment.
Embodiment 4:
To yellow rice wine use pillar continuous processing, by adsorbent material pre-process addition chromatographic column, 40 DEG C for the treatment of temperature,
Under flow velocity 1.5BV/h, 1.2 times of column volumes are handled, the removal rate of urea is up to 37%；When handling 7-10 times of column volume, urea
Removal rate is up to 32% or so.
Although the present invention has been described by way of example and in terms of the preferred embodiments, it is not intended to limit the invention, any to be familiar with this skill
The people of art can do various change and modification, therefore protection model of the invention without departing from the spirit and scope of the present invention
Enclosing subject to the definition of the claims.
Claims (5)
1. a kind of method for reducing urea in alcoholic drink, which is characterized in that the method is to handle yellow rice wine with adsorbent material；It is described
Processing is to vibrate adsorption treatment for 24 hours at 40 DEG C, 120-180r/min；It is described processing be carry out batch processing, carry out twice with
Upper oscillation adsorption treatment；The skeleton of the adsorbent material is acrylic copolymer, and type is acidulous cation resin material；Institute
Stating resin material is C258FD, 117,112 or D113, and the additive amount of the adsorbent material is the 10% of yellow rice wine.
2. being used further to locate the method according to claim 1, wherein the adsorbent material will be pre-processed first
Manage yellow rice wine；The pretreatment is to clean adsorbent material, is then impregnated with NaOH and NaCl solution, then wash to neutrality, then use
HCl solution impregnates, and then washing, ethyl alcohol are impregnated, washed again.
3. according to the method described in claim 2, it is characterized in that, the pretreatment of the adsorbent material, specifically: the wet body of 50mL
Long-pending adsorbent material is cleaned to water outlet with deionized water without muddy, free from admixture, molten with the NaCl of the NaOH of 100mL 3% and 7%
Liquid is washed with deionized water after impregnating 8h to neutrality, then impregnates 8h with the HCl solution of 100mL3%, and deionized water is washed till pH=4.0,
It is spare that no alcohol taste is washed to after 90% ethyl alcohol immersion 4h.
4. the method according to claim 1, wherein urea concentration range in the yellow rice wine 5mg/L~
Between 40mg/L.
5. the method according to claim 1, wherein the method is specifically:
(1) pretreatment adsorbed: the adsorbent material of 50mL humid volume is cleaned to water outlet with deionized water without muddy, free from admixture, with
The NaCl solution of the NaOH of 100mL 3% and 7% is washed with deionized water after impregnating 8h to neutrality, then molten with the HCl of 100mL 3%
Liquid impregnates 8h, and deionized water is washed till pH=4.0, and it is spare to be washed to no alcohol taste after 90% ethyl alcohol immersion 4h；
(2) 100mL yellow rice wine, the adsorbent material that addition step (1) has pre-processed, the addition of the adsorbent material batch processing: are taken
Amount is 10%, is handled for 24 hours in 40 DEG C, 150r/min；
(3) multiple adsorption treatment: the higher yellow rice wine of urea concentration is handled multiple according to step (2).
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| CN110656008B (en) * | 2019-10-24 | 2022-04-26 | 浙江农林大学 | Method for reducing content of urea and ethyl carbamate in yellow wine brewing process |
| CN112725130A (en) * | 2021-01-29 | 2021-04-30 | 浙江农林大学 | Device for removing protein precipitate of yellow rice wine by using external electric field and using method thereof |
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| CN103525803A (en) * | 2013-10-28 | 2014-01-22 | 江南大学 | Preparation method and application of natural material composite system immobilized bifunctional enzyme used for wine |
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| CN103525803A (en) * | 2013-10-28 | 2014-01-22 | 江南大学 | Preparation method and application of natural material composite system immobilized bifunctional enzyme used for wine |
Non-Patent Citations (3)
| Title |
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| 中国黄酒中氨基甲酸乙酯控制策略及机制的研究;刘俊;《中国博士学位论文全文数据库 工程科技Ⅰ辑》;20130415(第4期);B024-24 |
| 黄酒中氨基甲酸乙酯直接减除技术的研究;刘俊，等;《食品科技》;20121231(第2期);第171-176页 |
| 黄酒宽中氨基甲酸乙酯和尿素的处理方法与工艺条件;林文浩，等;《酿酒科技》;20150831(第8期);第40-43页 |
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