CN101303333A - Method for evaluating beer aging degree with high-efficiency liquid phantom method - Google Patents

Abstract

The invention relates to a method for assessing the aging degree of beer by high performance liquid chromatograph, which pertains to the field of beer quality assessment. With the high performance liquid chromatographic (HPLC) method, which is established by the invention, for separating various iso-alpha-acids from quantitative beer, T/C value indexes relevant with aging are extracted, and the correlation coefficients R<2> between T/C values and mouth feeling assessments of different types of beers are all in the range of 0.72-0.92, which reveal that the T/C values can overcome the differences between production batches or even brands to reflect the aging degree of the beers, and finally the corresponding relations between the T/C values and feeling assessments are used as a tool to determine the specific corresponding relations between aging indexes T/C values and beer aging degrees: when the T/C value is more than 33.4, the beer is considered as fresh, when the T/C value is between 26.1 and 33.4, the beer is considered as moderately aged, and the when T/C value is less than 26.1, the beer is considered as highly aged. The method of the invention can be used for objective and effective assessments of finished product beers with different quality and aging conditions, thus avoiding the shortcomings of mouth feeling assessment to a certain extent.

Description

A kind of method with evaluating beer aging degree with high-efficiency liquid phantom method

Technical field

A kind of method with evaluating beer aging degree with high-efficiency liquid phantom method belongs to beer quality and estimates the field.

Background technology

Beer is after packing, and along with the prolongation of time, can form some materials influences its original fresh flavor, and make beer flavor take place slowly and significantly to worsen: original fresh fragrance and taste are lost gradually, produce Cooked Taste.Because this is to be produced by oxidation of beer flavoring substances, therefore be called " Cooked Taste " or " activated flavour ", this process is called the aging of beer.The flavor stability of beer just refers to the local flavor freshness date of beer, and flavor stability is good more, and freshness date is just long more, and the ageing resistance of beer is also just correspondingly strong more.

Beer flavor stability is the focal issue that extremely brewing industry is paid close attention to for a long time always, but at present in the world except that sensory evaluation, lacks other and generally acknowledge objective and effective beer aging evaluation method.Though sensory evaluation can directly be described beer flavor, it mainly relies on people's subjective sensation, and high to the professional requirement of judging personnel, the subjective differences of judging the result is big.In order to improve the flavor stability of beer, it is very necessary to seek the objective indicator relevant with sensory evaluation.

The present invention relies on the high performance liquid chromatogram that can be used for each iso-in the separation and quantitative beer (HPLC) method of foundation, proposes this objective indicator of T/C ratio, has fine corresponding relation between this index and beer sensory evaluation, is applicable to the evaluation to the beer aging degree.

Summary of the invention

The purpose of this invention is to provide a kind of method with evaluating beer aging degree with high-efficiency liquid phantom method, be used for the finished beer of different quality and aging conditions is estimated, this method is a kind of objective effective beer aging evaluation method, thereby avoids mouthfeel to judge the defective of existence to a certain extent.

Technical scheme of the present invention: a kind of method with evaluating beer aging degree with high-efficiency liquid phantom method, rely on the high performance liquid chromatogram that can be used for each iso-in the separation and quantitative beer (HPLC) method of setting up, the T/C value index that proposes that ageing-related, the T/C value and the mouthfeel of dissimilar beer are judged a coefficient R ²All in 0.72～0.92 scope, and be tie finally with the corresponding relation between T/C value and sensory evaluation, determine the concrete corresponding relation of aging index T/C value and beer aging degree: when T/C value＞33.4, think that beer is in fresh state, when the T/C value in 26.1～33.4 scopes, think that beer is in the mittlere alterung state,, think that beer is in the height ageing state when T/C value＜26.1;

(1) aging index T/C value

A, sample preparation:

Activate with the 5mL methyl alcohol Solid-Phase Extraction sepak pillar of flowing through, use 60: 40: 0.1 the methanol-water-phosphoric acid mixed liquor of volume ratio of 5mL to carry out balance then through Solid-Phase Extraction sepak pillar, 20mL degasification beer sample to be measured is by pillar, again with 2mL ultrapure water washing pillar, room temperature CO ₂Dry 10s, used volume ratio then 50: 40: 10: 0.1 acetonitrile-methanol-water-phosphoric acid mixed liquor wash-out sepak post, collecting the eluent constant volume is 2mL, and before sample introduction with 0.45 μ m filtering with microporous membrane, micro-filtrate keeps in Dark Place in order to analysis for 4 ℃;

B, chromatographic condition:

Zorbax Eclipse XDB-C 18 (4.6 * 250nm, 5 μ m) chromatographic column; Moving phase consists of the A phase: the formic acid damping fluid of the pH ≈ 2.3 of ultrapure water preparation, B phase: acetonitrile; A: B volume ratio=41: 59; 20 ℃ of column temperatures; Detect wavelength 256nm; Flow velocity 2mL/min; Sample size 4 μ L; The moving phase wash-out; Obtain the content of six kinds of cis, trans iso-, be 1a: be anti--different cohumulone; 1b: suitable-different cohumulone; 2a: anti--isohumulone; 2b: suitable-isohumulone; 3a: anti--different adhumulone; 3b: suitable-different adhumulone;

The calculating of c, aging index T/C value

With the intensification of beer aging degree, six kinds of cis, trans iso-degraded situation difference in the beer aging process, its trans iso-degraded is very fast, and the degraded of cis iso-is not obvious.But, cause and to realize evaluation by the absolute value of single trans iso-, thereby proposition T/C index is weighed the aging conditions of beer different cultivars beer aging degree because there is beer variety difference in trans iso-absolute content.

T/C value (%)=[trans iso-total content/cis iso-total content] * 100%;

(2) sensory evaluation

Judge the subjective differences that beer flavor is described to dwindle mouthfeel as far as possible, invite the mouthfeel that has been trained for a long time to judge the expert the wine sample of research is judged marking.The personnel that judge judge by the marking of the beer aging shown in the table 1 rule, and net result is averaged.

Table 1 beer aging sensory evaluation scores standard

Annotate: 0 is fresh fully; 1 is very weak aging; 2 weak wearing out; 3 suitable wearing out; Wearing out of semi-finals; 5 very strong wearing out.

(3) aging index T/C value and beer aging degree relation

With the corresponding relation between T/C value and sensory evaluation is tie, the concrete corresponding relation of determining aging index T/C value and beer aging degree is: when T/C value＞33.4, think that beer is in fresh state, when the T/C value in 26.1～33.4 scopes, think that beer is in the mittlere alterung state, when T/C value＜26.1, think that beer is in the ageing state of height.

36 kinds of different brands wine sample results of study that are in different degree of agings of analysis-by-synthesis are tie with the corresponding relation between T/C value and sensory evaluation, set up the relation extents of T/C value and beer aging degree, and are as shown in table 2.

The relation extents of table 2T/C value and beer aging degree

(4) aging index T/C value is to the evaluation of all types of beer aging degree

The aging index T/C value that proposes that ageing-related, for dissimilar beer, the index T/C value that wears out and mouthfeel are judged a coefficient R ²All in 0.72～0.92 scope, show that difference that aging index T/C value can overcome production batch even brand reflects the degree of aging of beer.

The related coefficient that the different degree of agings of table 3 all types of beer T/C value and mouthfeel are judged

To judge subjective differences big because of mouthfeel, it is unsuitable narrow on reasonable basis to judge beer aging extent and scope that score intermediary delimit by mouthfeel, and the beer aging extent and scope that therefore will be used to set up T/C value and degree of aging relation is divided into fresh state, mittlere alterung state and ageing state Three Estate highly; With the corresponding relation between T/C value and sensory evaluation is tie, the concrete corresponding relation of determining this objective indicator and beer aging degree is: when T/C＞33.4, think that beer is in fresh state, when T/C in 26.1～33.4 scopes, think that beer is in the mittlere alterung state, when T/C＜26.1, think beer be in the height ageing state.

Beneficial effect of the present invention: the invention provides a kind of objective effective beer aging evaluation method, it is characterized in that relying on the high performance liquid chromatogram that can be used for each iso-in the separation and quantitative beer (HPLC) method of foundation, the T/C value index that proposes that ageing-related, the T/C value and the mouthfeel of dissimilar beer are judged a coefficient R ²All in 0.72～0.92 scope, show that difference that the T/C value can overcome production batch even brand reacts the degree of aging of beer, final is tie with the corresponding relation between T/C value and sensory evaluation, determine the concrete corresponding relation of this objective indicator and beer aging degree: when T/C＞33.4, think that beer is in fresh state, when T/C in 26.1～33.4 scopes, think that beer is in the mittlere alterung state, when T/C＜26.1, think beer be in the height ageing state.This method can be used for objectively effectively the finished beer of different quality and aging conditions being estimated, thereby avoids mouthfeel to judge the defective of existence to a certain extent.

Description of drawings

The high performance liquid chromatogram (HPLC) of each iso-figure in Fig. 1 separation and quantitative beer.

Embodiment

Embodiment 1

Choose 5 kinds of beer that are in different unaccelerated aging states, measure each suitable, trans isomer of iso-, calculate the corresponding T/C value of each wine sample, the result is as shown in table 4; Invitation is judged the expert and according to the sensory evaluation rule degree of aging of research wine sample is judged marking.According to aging index T/C value and the beer aging degree physical relationship set up, the degree of aging of each wine sample is judged in prediction, the actual degree of aging result that prediction degree of aging that contrast T/C value is determined and sensory evaluation are determined, as seen the two reaches consistent state substantially, see Table 5, show that this method can be used for objectively effectively the finished beer of different quality and aging conditions being estimated, thereby avoid mouthfeel to judge the defective of existence to a certain extent.

Each wine sample iso-of table 4 is suitable, trans isomer content and T/C value

The comparing result that table 5T/C ratio and sensory evaluation are estimated wine sample degree of aging

Claims (1)

1, a kind of method with evaluating beer aging degree with high-efficiency liquid phantom method, it is characterized in that relying on the high performance liquid chromatogram method that can be used for each iso-in the separation and quantitative beer of foundation, the T/C value index that proposes that ageing-related, the T/C value and the mouthfeel of dissimilar beer are judged a coefficient R ²All in 0.72～0.92 scope, and final be tie with the corresponding relation between T/C value and sensory evaluation, the concrete corresponding relation of determine to wear out index T/C value and beer aging degree; When T/C value＞33.4, think that beer is in fresh state, when the T/C value in 26.1～33.4 scopes, think that beer is in the mittlere alterung state, when T/C value＜26.1, think beer be in the height ageing state;

(1) aging index T/C value:

A, sample preparation:

Activate with the 5mL methyl alcohol Solid-Phase Extraction sepak pillar of flowing through, use 60: 40: 0.1 the methanol-water-phosphoric acid mixed liquor of volume ratio of 5mL to carry out balance then through Solid-Phase Extraction sepak pillar, 20mL degasification beer sample to be measured is by pillar, again with 2mL ultrapure water washing pillar, room temperature CO ₂Dry 10s, used volume ratio then 50: 40: 10: 0.1 acetonitrile-methanol-water-phosphoric acid mixed liquor wash-out sepak post, collecting the eluent constant volume is 2mL, and before sample introduction with 0.45 μ m filtering with microporous membrane, micro-filtrate keeps in Dark Place in order to analysis for 4 ℃;

B, chromatographic condition:

Zorbax Eclipse XDB-C18 (4.6 * 250nm, 5 μ m) chromatographic column; Moving phase consists of the A phase: the formic acid damping fluid of the pH ≈ 2.3 of ultrapure water preparation, B phase: acetonitrile; A: B volume ratio=41: 59; 20 ℃ of column temperatures; Detect wavelength 256nm; Flow velocity 2mL/min; Sample size 4 μ L; The moving phase wash-out; Obtain the content of six kinds of cis, trans iso-, be 1a: be anti--different cohumulone; 1b: suitable-different cohumulone; 2a: anti--isohumulone; 2b: suitable-isohumulone; 3a: anti--different adhumulone; 3b: suitable-different adhumulone;

The calculating of c, aging index T/C value

T/C value (%)=[trans iso-total content/cis iso-total content] * 100%;

(2) aging index T/C value and beer aging degree relation

With the corresponding relation between T/C value and sensory evaluation is tie, the concrete corresponding relation of determining aging index T/C value and beer aging degree is: when T/C value＞33.4, think that beer is in fresh state, when the T/C value in 26.1～33.4 scopes, think that beer is in the mittlere alterung state, when T/C value＜26.1, think that beer is in the ageing state of height;

(3) aging index T/C value is to the evaluation of all types of beer aging degree

The aging index T/C value that proposes that ageing-related, for dissimilar beer, the index T/C value that wears out and mouthfeel are judged a coefficient R ²All in 0.72～0.92 scope, show that difference that aging index T/C value can overcome production batch even brand reflects the degree of aging of beer.