CN111398524B - Identification threshold value of key flavor components of beer and evaluation method of harmony of key flavor components of beer and hop aroma - Google Patents
Identification threshold value of key flavor components of beer and evaluation method of harmony of key flavor components of beer and hop aroma Download PDFInfo
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Abstract
The invention discloses a recognition threshold value of key flavor components of beer and an evaluation method of harmony of the recognition threshold value and hop aroma. The existing threshold method cannot be completely suitable for testing the aroma substance recognition threshold in the beer matrix environment on one hand, and cannot effectively perform accurate screening and accurate evaluation of flavor harmony on key main flavor substances affecting a certain type of aroma on the other hand, so that optimization of the optimal flavor content ratio is realized. The method is simple to complex by a two-step method, is from a single simulation base liquid to complex solid beer, combines a beer analysis technology, systematically provides a set of sensory test evaluation system, establishes a main flavor substance identification threshold value in the beer, simultaneously proposes that the beer has the best state of ester aroma, flower aroma and flavor harmony, has the negative aroma at the lowest flavor intensity, and provides an effective tool for clearly revealing the harmony of the beer flavor substance and the hop aroma.
Description
Technical Field
The invention relates to a recognition threshold value of key flavor components of beer and an evaluation method of harmony of the key flavor components of beer and hop aroma, belonging to the technical field of food flavor sense and analysis.
Background
Beer flavor is a very complex system, which is produced by the interaction of hundreds of flavors, in addition to the main components ethanol and water. Obvious flavor and taste discordance in the beer can directly reduce the drinkability and the acceptability of the public consumers to the beer, thereby damaging the brand image of the beer. At present, the common phenomena that the actually detected content of hop aroma substances is higher but the actually smelling aroma intensity is not outstanding exist in the beer industry, namely the actual content of the hop aroma is not matched with the actually smelling intensity, which is mainly caused by the interference or interaction of the smelling intensity of the hop aroma by other flavor substances in a wine body. Therefore, based on a technical system combining quantitative analysis and smell of beer flavor compounds, a set of method for systematically analyzing key, characteristic and important aroma compounds influencing the smell intensity of the hop aroma in the beer is established, and a technical guidance scheme for the optimal flavor proportion of the hop aroma intensity and the flavor harmony in the beer is provided.
The evaluation of the aroma intensity of the hop of the beer needs to be measured by using an index of a threshold value. The minimum content of flavor substances at the beginning of smelling the fragrance is taken as a unit for representing the intensity of the fragrance, and is called a threshold value (unit is g/m) 3 ). Recognition threshold alcohol body purity of same substanceDifferent from the difference of factors such as interaction with other flavors of the wine body, the substance can be obviously smelled and identified when the actual content of the wine body exceeds the threshold value of the substance in the wine body. For example: when the purity of the wine body is higher, the threshold value of the hop aroma substances is lower, and the smell intensity of the hop aroma is higher; under the condition that other flavor substances in the wine body are not changed, the higher the content of the hop aroma substances in the wine body is, the more remarkable the smell intensity of the hop aroma can be.
In the patent application published by Von Tao et al (a method for measuring olfaction threshold of volatile flavor substance and its application), a method for measuring olfaction threshold of volatile flavor substance is provided, so as to measure olfaction threshold of volatile flavor substance
Collecting and preparing flavor monomers in a bag, and determining a smell threshold value by combining a dynamic flavor dilution and smell identification instrument. The patent application published by enbergy et al (method of determining the threshold of detection of volatile flavour substances in cheese) provides a threshold of detection of flavour substances in cheese based on a simulated substrate study. The existing research mainly adopts different means to carry out research aiming at measuring methods of smell threshold values of different flavors, and important flavor substances in a beer body or cheese are screened out, but the problems exist in two aspects, on one hand, the method is not completely suitable for testing the identification threshold value of the aroma substances in a beer matrix environment, on the other hand, an accurate evaluation method of flavor interaction harmony is lacked, namely, an effective method for determining the optimal hop aroma content proportioning scheme when the important positive main body flavor intensity and the integral flavor harmony in the beer are ensured to be optimal and the negative flavor intensity is minimum is lacked.
Disclosure of Invention
In order to solve the problems, the invention provides a set of systematic sensory test design scheme from simple to complex steps from a single ideal simulation base liquid to an actual wine body, establishes an identification threshold value of main flavor components in the beer under the influence of hop aroma components, and provides and optimizes a key hop aroma substance content proportioning scheme under the condition that the positive flavor intensity and the overall flavor harmony of the beer reach the optimal state and the negative flavor intensity reaches the minimum state by combining a response surface analysis means.
The invention mainly relates to a recognition threshold, which is the minimum content which can be perceived to recognize olfactory stimuli.
Because the flavor components in the beer have promoting, reducing and overlapping effects, the invention selects the main flavor components with positive effects, such as acetaldehyde, ethyl acetate, isoamyl alcohol, isobutanol and the like, which play an important smell contribution to the flavor of the beer, and the flavor with negative effects, such as diacetyl, DMS and the like, as research objects, and establishes a mathematical evaluation model by combining quantitative flavor analysis, sensory evaluation and response surface analysis means, thereby realizing the optimal content ratio of three typical substances, namely linalool, geraniol and beta-citronellol, in the aroma of the hop under the conditions of optimal positive aroma intensity and flavor harmony and minimum negative aroma intensity in the beer.
The key flavor component identification threshold value of the wine and the evaluation method of the key flavor component identification threshold value and the harmony of the key flavor component identification threshold value and the hop aroma provided by the invention comprise the following steps:
(1) Selecting the benchmarking beer with the style and the alcoholic strength similar to those of the beer to be researched, wherein the benchmarking beer has good harmony and purity; measuring the contents of flavor components and hop aroma components of the beer to be researched and the benchmarking beer;
therefore, the contents of the flavor components and the hop flavor components in the benchmarking beer are lower than the contents of the corresponding components in the beer to be researched;
(2) Respectively adding single hop aroma components into the ethanol water solution to serve as single hop aroma component simulation base solution;
the content of the single hop aroma component simulation base solution is equal to the content of the corresponding component in the beer to be researched;
the content of ethanol in the single hop aroma component simulation base solution is equal to the content of ethanol in the beer to be researched;
(3) Respectively adding single flavor components into the single hop aroma component simulation base liquid to obtain solutions with different single flavor component content gradients, gradually increasing the content gradients by a specific coefficient, taking the single hop aroma component simulation base liquid without the added flavor components as a blank control, and performing sensory evaluation by adopting a three-point test method based on the perception and recognition of each flavor to obtain a recognition threshold value of the flavor components under each single hop aroma component simulation base liquid; further obtaining key flavor components influencing the aroma intensity of the hops of the beer to be researched;
(4) Adding the key flavor components into the benchmarking beer to enable the content of the key flavor components to be equal to that of corresponding components in the beer to be researched; adding single or combined hop aroma and flavor components into the benchmarking beer according to 3-4 gradient modes, and performing multi-factor and multi-level experimental design through response surface analysis software; the highest limit amount of each hop aroma and flavor component is not more than the content difference between the beer to be researched and the benchmarking beer, and the benchmarking beer without the hop aroma and flavor components is used as a blank control; performing sensory evaluation on all the beers, and grading indexes;
the indicators include ester aroma, hops aroma, higher alcohols, other off-notes, sulfury, swishing and flavor coordination;
(5) Based on response surface analysis software, the optimal content of the hop aroma and flavor components in the beer to be researched is obtained by taking ester aroma, hop aroma and flavor harmony as the highest scoring targets.
In the above method for evaluating the compatibility, the flavor components include acetaldehyde, ethyl acetate, isoamyl alcohol, isobutanol, diacetyl and dimethyl sulfide;
the flos Lupuli aroma components comprise linalool, geraniol and beta-citronellol.
In the harmony evaluation method, the contents of the flavor component and the hop aroma component are measured by adopting a headspace-gas chromatography-plasma flame detector method and a solid phase microextraction-gas chromatography-mass spectrometry combined method.
In the above-described harmony evaluation method, in step (3), determination of the recognition threshold is performed by a three-point forced selection method common to ASTM679, wherein four men and four women are used as panelists, the average age is 35 years old, 4 national professional judges and 4 senior professional judges, and fragrance intensity rating is performed by 9-point division: 0 means no flavour was recognised, 1-2 means that the aroma was just recognised: 3-5 indicates moderate recognition intensity of aroma, and 6-9 indicates strong recognition intensity of aroma. "+" indicates correct selection in the three-point test; "-" indicates a selection error in the three-point test method; the experiment was terminated when the three-point test method allowed the selection of the correct and just recognizable bouquet flavour, i.e. when the sample content rated "1+" was taken as the just recognizable content. The individual recognition threshold of the panelist is the geometric mean of the content (labeled "0 +") which is judged to be correct at the last but not recognized and the content (labeled "1 +") which is judged to be correct at the next, and the group recognition threshold is the geometric mean of the individual recognition thresholds.
In the above-described harmony evaluation method, in step (3), the content gradient gradually increases with a coefficient of 2 to 6.
In the above-described method for evaluating the harmony, in the step (3), the key flavor component is determined based on the OAV (object activity value) value of the flavor component, and a component having an OAV value of more than 1 is usually selected as the key component;
the OAV value is a ratio of the amount of the flavor component to an identification threshold of the flavor component.
The single hop aroma component simulation base solution is mainly used for eliminating comprehensive interference of various components, is simple in preparation method, can quickly and accurately excavate key characteristic flavor components and key hop aroma components which affect the hop aroma intensity in the beer, and lays a foundation for further evaluating the hop aroma intensity, key characteristic flavor substances and integral flavor harmony of the hop aroma intensity and the key characteristic flavor substances and the beer.
In the above-described method for evaluating the compatibility, in the step (4), the content gradient gradually increases with a coefficient of 2 to 6.
The evaluation personnel adopt four men and four women, the average age is 35 years old, 4 national professional judges and 4 senior professional judges, and the fragrance intensity grade evaluation is carried out by adopting 9 grades: 1-2 indicates that the fragrance is just recognizable: 3-5 means that the intensity of fragrance recognition is medium, and 6-9 means that the intensity of fragrance recognition is high.
In the harmony evaluation method, in the step (5), a batch of wine samples are screened out by taking the flavor harmony as a grading target, and then ester aroma and bouquet aroma are taken as a second sequence grading target and a third sequence grading target in sequence, namely, the batch of wine samples are screened out by taking the flavor harmony as the grading target, then the batch of wine samples are screened out by taking the ester aroma as the grading target, preferably the bouquet aroma as the grading target, and the best wine sample is obtained by screening the wine samples.
The invention has the following beneficial effects:
the invention provides a set of sensory test evaluation system systematically from simple to complex, from single simulated base liquid to complex solid beer through a two-step method and by combining a beer analysis technology, and provides an effective tool for clearly revealing the compatibility of beer flavor substances and hop aroma, wherein the beer has the advantages that the ester aroma, the flower aroma and the flavor compatibility reach the optimal state, the negative aroma is at the lowest flavor intensity, and the optimal content proportion of the hop aroma substances is provided while the identification threshold of the main flavor substances in the beer is established.
Detailed Description
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
A benchmarking beer similar in style and alcohol and having excellent consistency and purity was selected, requiring a lower flavor content than the study beer. A headspace-gas chromatography-plasma flame detector method and a solid phase microextraction-gas chromatography-mass spectrometry combined method are adopted, and the contents of main flavor components including acetaldehyde, ethyl acetate, isoamyl alcohol, isobutanol, diacetyl, dimethyl sulfide, hop aroma components linalool, geraniol, beta-citronellol and the like in the beer are analyzed and measured. Wherein, the alcoholic strength of the beer is between 3 percent and 5 percent.
TABLE 1 main flavour content of benchmarking and research beer
Adding single components of acetaldehyde, ethyl acetate, isoamyl alcohol, isobutanol, diacetyl and dimethyl sulfide into a hop aroma component simulation base solution to prepare a group of solutions with different single flavor content gradients, wherein the content gradients are gradually increased step by step in a mode of a coefficient of 2, the hop aroma component simulation base solution without single flavor is used as a blank control, a three-point inspection method is adopted, sensory evaluation is carried out by taking each main characteristic flavor sensed and identified as a standard, and an identification threshold value of each single main flavor component under the various single hop aroma component simulation base solutions is calculated; wherein, the appraisers adopt four men and four women, the average age is 35 years old, 4 national professional judges and 4 senior professional judges.
Table 2 hop aroma-4% ethanol-ethyl acetate in water solution recognition threshold, ethyl acetate units: mg/L (for example, one grade evaluator)
Remarking: the fragrance intensity rating was carried out by 9 min: 0 means no flavour was recognised, 1-2 means that the aroma was just recognised: 3-5 indicates moderate recognition intensity of aroma, and 6-9 indicates strong recognition intensity of aroma. "+" indicates correct selection in the three-point test; "-" indicates a selection error in the three-point test method; the experiment can be terminated when the three-point test method can select the correct and just recognizable odorous substance, i.e. when the sample content rated as "1+" is taken as the just recognizable content. The individual recognition threshold of the panelist is the geometric mean of the content (labeled "0 +") which is judged to be correct at the last but not recognized and the content (labeled "1 +") which is judged to be correct at the next, and the group recognition threshold is the geometric mean of the individual recognition thresholds.
Taking this as an example, the recognition threshold results for each of the subject flavors by eight panelists were analyzed systematically by the ASTM-679 method as follows:
TABLE 3 recognition threshold value unit of each single flavor substance in the hop aroma simulation base liquid mg/L
As can be seen from the data in table 3, the interference effect of linalool on the main flavor compared to geraniol and β -citronellol is the most different, and the main flavor is ranked from large to small by the influence of linalool as calculated from the OAV value of the flavor intensity: isoamyl alcohol (6.61) > isoamyl acetate (5.24) > diacetyl (2.67) > DMS (2.00) > acetaldehyde (1.40) > ethyl acetate (0.88) > isobutanol (0.71); wherein key main flavor components with OAV value larger than 1 are isoamyl alcohol, isoamyl acetate, diacetyl, DMS and acetaldehyde in sequence.
In order to ensure the compatibility of ester aroma, hop aroma and overall flavor of beer, the optimization of the optimal hop aroma content ratio in the actual beer is needed.
A benchmarking beer was selected that was similar in style to the studied beer and was very consistent and clean, as the benchmarking beer had a lower flavor content than the studied beer. In the benchmarking beer, the five key flavor components with OAV value >1 are supplemented, namely 11.12mg/L isoamyl alcohol, 0.45mg/L isoamyl acetate, 0.01mg/L diacetyl, 0.015mg/LDMS and 2.13mg/L acetaldehyde are added externally (the content difference of flavor substances between the beer and the benchmarking beer is studied), so that the key flavor component content in the benchmarking beer is the same as the key flavor component content in the beer under study. A three-factor three-level experiment is designed through Design-Expert analysis software, single or combined hop aroma components with different content levels are added into the benchmarking beer with five key flavors, wherein the highest limit quantity delta C3 of each hop aroma component externally added into the benchmarking beer is used for researching the content difference of the hop aroma components in the beer and the benchmarking beer, the delta C1 and the delta C2 are added in a decreasing manner by a multiple with a coefficient of 2, the lowest limit quantity is the actual content of each hop aroma component in the benchmarking beer, namely, no hop aroma component is externally added into the benchmarking beer (blank control), and the table 4 shows.
Taking linalool as an example, the maximum addition amount of linalool is C Research beer -C Mark bar beer (ii) a All beer is subjected to sensory evaluation, including indexes such as ester aroma, hop aroma, high alcohol, other abnormal aroma, sulfur aroma, rice-swishing flavor, flavor harmony and the like, and according to the national evaluation personnel, 9-point system is adopted for carrying out aroma intensity grade evaluation, wherein 1-2 represents that the aroma can be just identified: 3-5 means that the intensity of fragrance recognition is medium, and 6-9 means that the intensity of fragrance recognition is high.
Table 4 response surface experimental design unit of hop aroma in benchmarking wine sample with additional key body flavors: mu g/L
Remarking: the fragrance intensity rating was carried out by 9 points 1-2, which means that the fragrance was just recognizable: 3-5 indicates moderate recognition intensity of aroma, and 6-9 indicates strong recognition intensity of aroma.
By taking ester fragrance, flower fragrance and flavor harmony as the highest scoring target and negative fragrance such as mellow fragrance, abnormal fragrance and other abnormal fragrance, sulfur fragrance and swoosh smell as the lowest scoring target, the optimal optimized proportion of the final hop fragrance is as follows: the contents of linalool, geraniol and beta-citronellol were 10.93. Mu.g/L, 3.66. Mu.g/L and 2.50. Mu.g/L, respectively, which were the most preferable, and the wine-like flavor harmony was scored as 8.5, the ester aroma was scored as 6.5 and the hop aroma intensity was scored as 4.5.
Claims (1)
1. A method for evaluating the recognition threshold of key flavor components of beer and the harmony between the key flavor components and the aroma of hops comprises the following steps:
(1) Selecting benchmarking beer with the style and the alcoholic strength similar to those of beer to be researched; measuring the contents of flavor components and hop aroma components of the beer to be researched and the benchmarking beer;
the contents of the flavor components and the hop aroma components in the benchmarking beer are lower than the contents of the corresponding components in the beer to be researched;
the flavor components comprise acetaldehyde, ethyl acetate, isoamyl alcohol, isobutanol, diacetyl and dimethyl sulfide;
the hop aroma components comprise linalool, geraniol and beta-citronellol;
determining the content of the flavor components and the content of the hop aroma components by adopting a headspace-gas chromatography-plasma flame detector method and a solid phase microextraction-gas chromatography-mass spectrometry combined method;
(2) Respectively adding single hop aroma components into an ethanol water solution to serve as single hop aroma component simulation base solution;
the content of the single hop aroma component simulation base solution is equal to the content of the corresponding component in the beer to be researched;
the content of ethanol in the single hop aroma component simulation base solution is equal to the content of ethanol in the beer to be researched;
(3) Respectively adding single flavor components into the single hop aroma component simulation base liquid to obtain solutions with different single flavor component content gradients, wherein the content gradients are gradually increased by specific coefficients, the single hop aroma component simulation base liquid without the added flavor components is used as a blank control, and sensory evaluation is carried out by adopting a three-point test method and taking each flavor sensed and recognized as a standard to obtain a recognition threshold value of the flavor components under each single hop aroma component simulation base liquid; further obtaining key flavor components influencing the aroma intensity of the hops of the beer to be researched;
determining the identification threshold value by adopting a three-point forced selection method commonly used in an ASTM679 method, wherein a plus sign indicates that the selection is correct in the three-point test method; "-" indicates a selection error in the three-point test method; the fragrance intensity rating is evaluated by adopting 9 minutes, when a three-point test method can select correct fragrance and can just identify the fragrance of the wine, namely when the content of the sample which is evaluated as '1 +' is taken as the content which can just be identified, the experiment can be stopped;
the individual identification threshold of the panelist is the geometric mean of the content which is judged correctly but can not be identified at the last time and the content which is judged correctly and can be just identified at the next time, and the group identification threshold is the geometric mean of the individual identification threshold;
determining the key flavor component from the OAV value of the flavor component;
the OAV value is a ratio of the amount of the flavor component to an identification threshold of the flavor component;
(4) Adding the key flavor components into the benchmarking beer to enable the content of the key flavor components to be equal to that of corresponding components in the beer to be researched; adding single or combined hop aroma components into the benchmark beer according to 3 to 4 gradient modes, and carrying out multi-factor and multi-level experimental design through response surface analysis software; the highest limit amount of each hop aroma component is not more than the content difference between the beer to be researched and the benchmarking beer, the benchmarking beer without the hop aroma components is used as a blank control, sensory evaluation is carried out on all the beers, and the indexes are graded;
the indicators include ester aroma, hops aroma, higher alcohols, other off-notes, sulfury, swishing and flavor coordination;
(5) Based on response surface analysis software, the best content of the hop aroma components in the beer to be researched is obtained by taking ester aroma, hop aroma and flavor harmony as the highest scoring targets.
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