High-temperature yeast fragrance reference sample and yeast fragrance liquid as well as preparation method and application of high-temperature yeast fragrance reference sample and yeast fragrance liquid

Abstract

The invention discloses a high-temperature yeast fragrance reference sample and yeast fragrance liquid as well as a preparation method and application thereof, and belongs to the field of food flavor and chemical engineering. The reference sample is prepared by dissolving 38 key aroma compounds such as isoamyl alcohol, isovaleric acid, 2-methylbutyraldehyde, 2, 5-dimethylpyrazine and the like in a solvent according to a specific ratio, and carrying out classified premixing, standing and fusion. The reference sample is harmonious in aroma and good in stability, successfully simulates typical yeast aroma characteristics of the high-temperature yeast, and can be used for quality evaluation, quality control training and wine brewing process optimization of the high-temperature yeast. On the basis, by adjusting the content of various compounds, the yeast fragrance liquid with the characteristic notes of nuts, cocoa, flower fragrance and the like can be derived and further applied to products such as blasting beads, fragrance smelling cards, tobaccos, compound wine and the like, and diversified expansion of the yeast fragrance value is achieved.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of food flavor and chemical engineering, and particularly relates to a high-temperature Daqu koji aroma reference sample and koji aroma, a preparation method and application thereof. BACKGROUND

[0002] Baijiu is one of the world's six major distilled liquors, and is known as brandy, whiskey, vodka, gin and rum. Baijiu has a long history of culture and is the largest liquor consumed globally, including 12 types of aroma such as Maotai-flavor, Luzhou-flavor and Qing-flavor. Maotai-flavor baijiu, as one of the typical representatives, is loved by consumers at home and abroad for its unique style and taste. Maotai-flavor baijiu is made of high-temperature Daqu as a fermentation agent and highland barley as the main raw material through solid-state fermentation. "Koji is the bone of liquor", and good Daqu is the basis for preparing good Maotai-flavor liquor. The usage of high-temperature Daqu and highland barley in the brewing process of Maotai-flavor baijiu reaches 1:1. High-temperature Daqu provides enzymes and microorganisms that play a key role in fermentation, as well as part of the raw materials (wheat and other koji-making raw materials) and aroma compounds. The aroma of these aroma compounds is the aroma of koji.

[0003] On the one hand, in QB / T 4259-2011, koji aroma is an important indicator for judging the quality of Daqu. At present, the evaluation of Daqu aroma mainly relies on the sensory analysis and experience judgment of koji-making workers, and lacks unified physical and chemical standards.

[0004] On the other hand, as shown in the aroma profile diagram of superior and first-grade Maotai-flavor baijiu aroma characteristics shown in GB / T 10781.4-2024 Figure 1 ), koji aroma is an important part of the aroma quality evaluation of Maotai-flavor baijiu. In superior Maotai-flavor baijiu, the scoring requirements of koji aroma and Maotai aroma are basically the same, while in first-grade Maotai-flavor baijiu, the scoring requirements of koji aroma are correspondingly reduced, which shows the importance of koji aroma in the quality evaluation of Maotai-flavor baijiu.

[0005] In addition, research has found that CN119901556A discloses a koji aroma reference sample of medium-temperature Daqu and its preparation method and application, but there are essential differences between medium-temperature Daqu and high-temperature Daqu in koji-making process, microbial system and core aroma components, which leads to the fact that the aroma profile of the koji aroma reference sample cannot accurately represent and be applied to the quality evaluation of high-temperature Daqu represented by Maotai-flavor baijiu. CN113717805B provides a method for preparing a high-temperature Daqu reference sample by simulating fermentation, but the preparation quality of such Maotai Daqu reference sample depends on the quality of all high-temperature Daqu raw materials and strict control of the preparation process, and it is difficult to ensure the stability and consistency of Maotai Daqu reference samples of different preparation times and batches.

[0006] In summary, the existing medium-temperature Daqu reference sample is not suitable for high-temperature Daqu system, and the reference sample prepared by the existing high-temperature Daqu simulation fermentation method has the problems of stability and consistency. Therefore, it is of great significance to develop a preparation type koji aroma reference sample specially used for high-temperature Daqu and having stable properties, for guaranteeing the accuracy, stability and consistency of the reference sample, and the operation process is simple and controllable. SUMMARY

[0007] The technical problem to be solved by the present application is that the existing medium-temperature Daqu reference sample is not suitable for high-temperature Daqu evaluation, and the reference sample prepared by the existing high-temperature Daqu simulation fermentation method has the problems of stability and consistency.

[0008] To achieve the above application purposes, the technical solutions adopted by the present application are as follows.

[0009] In a first aspect, the present application provides a high-temperature Daqu flavor reference sample, which comprises, by weight percentage, isopentyl alcohol 0.002-0.010‰, n-hexanol 0.00005-0.0002‰, mushroom alcohol 0.0001-0.0007‰, 3-octanol 0.0005-0.0020‰, 2-methylbutyraldehyde 0.004-0.030‰, isovaleraldehyde 0.010-0.060‰, 2-octanone 0.0005-0.0015‰, isovaleric acid 0.050-0.300‰, isobutyric acid 0.020-0.200‰, methyl acetate 0.005-0.020‰, methyl hexanoate 0.00005-0.00020‰, methyl isovalerate 0.001-0.005‰, methyl laurate 0.0005-0.003‰, methyl palmitate 0.0005-0.0020‰, benzyl alcohol 0.005-0.050‰, phenethyl alcohol 0.005-0.050‰, benzaldehyde 0.001-0.005‰, phenylacetaldehyde 0.001-0.005‰, acetophenone 0.001-0.005‰, 1,2-dimethoxybenzene 0.0005-0.003‰, methyl benzoate 0.0001-0.0005‰, methyl phenylacetate 0.0001-0.0005‰, 2-methylpyrazine 0.0001-0.0005‰, 2,3-dimethylpyrazine 0.0001-0.0005‰, 2,5-dimethylpyrazine 0.005-0.030‰, 2,6-dimethylpyrazine 0.001-0.005‰, 2,3,5-trimethylpyrazine 0.002-0.010‰, ligustilide 0.005-0.050‰, 2-ethyl-6-methylpyrazine 0.0001-0.0005‰, 2,3-dimethyl-5-ethylpyrazine 0.0002-0.0006‰, 2,3,5-trimethyl-6-ethylpyrazine 0.0001-0.0005‰, 2-pyrrolecarboxaldehyde 0.0020-0.0100‰, 2-acetylpyrrole 0.003-0.010‰, coconut aldehyde 0.00001-0.00005‰, furfural 0.002-0.010‰, 4-vinylguaiacol 0.001-0.005‰, myrcenone 0.00005-0.00020‰, trimethylamine 0.0002-0.0010‰, and the balance is a solvent; the solvent is propylene glycol.

[0010] In the high-temperature Daqu flavor reference sample described above, the high-temperature Daqu is any one of white Daqu, yellow Daqu, and black Daqu.

[0011] Furthermore, the composition of the white koji fragrance reference liquid is as follows: based on the above-mentioned high-temperature koji fragrance reference sample composition, the total weight percentage of aldehydes is adjusted to 0.50~1.00‰, the total weight percentage of nitrogen-containing heterocyclic compounds is adjusted to 0.20~0.50‰, and the total weight percentage of acids is adjusted to 0.10~0.30‰; the adjustment includes, but is not limited to: deleting specific compounds, increasing or decreasing the content of specific compounds, so that the total content of this category in the final formula reaches the target range.

[0012] Furthermore, the composition of the aflatoxin reference solution is as follows: based on the above-mentioned high-temperature koji (fermented grain) reference sample composition, the total weight percentage of acids is adjusted to 0.50~1.00‰, the total weight percentage of nitrogen-containing heterocyclic compounds is adjusted to 0.20~0.50‰, and the total weight percentage of esters is adjusted to 0.10~0.20‰; the adjustment includes, but is not limited to: deleting specific compounds, increasing or decreasing the content of specific compounds, so that the total content of this category in the final formula reaches the target range.

[0013] Furthermore, the composition of the black yeast rice fragrance reference liquid is as follows: based on the above-mentioned high-temperature large yeast rice fragrance reference sample composition, the total weight percentage of nitrogen-containing heterocyclic compounds is adjusted to 0.20~0.50‰, the total weight percentage of oxygen-containing heterocyclic compounds is adjusted to 0.10~0.20‰, the total weight percentage of phenols is adjusted to 0.05~0.10‰, and the total weight percentage of esters is adjusted to 0.10~0.20‰; the adjustment includes, but is not limited to: deleting specific compounds, increasing or decreasing the content of specific compounds, so that the total content of this category in the final formula reaches the target range.

[0014] Secondly, the present invention provides a method for preparing the above-mentioned high-temperature Daqu (a type of starter culture) reference sample, comprising the following steps:

[0015] (1) Classification premixing: All compounds in the components of the above high-temperature Daqu koji reference sample, except for the solvent, are classified according to their chemical structure and mixed with a portion of the solvent to prepare multiple categories of premixed liquids;

[0016] (2) Standing and maturation: Let the various premixed liquids obtained in step (1) stand for 6 to 24 hours respectively;

[0017] (3) Final mixing: Mix the various premixed liquids after standing, and add solvent to make up the total amount. Stir evenly and let stand for 24-48 hours to obtain the high temperature Daqu koji reference sample.

[0018] In step (1) of the above preparation method, the classification includes alcohols, aldehydes, ketones, acids, esters, aromatics, nitrogen-containing heterocycles, oxygen-containing heterocycles, phenols, terpenes and amines.

[0019] In step (3) of the above preparation method, various premixed solutions are mixed in the following order: alcohols, acids, esters, aromatics, aldehydes, ketones, oxygen-containing heterocycles, nitrogen-containing heterocycles, phenols, terpenes and amines.

[0020] Thirdly, the present invention provides a koji-scented liquid, which is based on the components of the above-mentioned high-temperature koji-scented reference sample, and by adjusting the content of specific compounds therein and / or introducing other aroma compounds, thereby forming a koji-scented liquid with high-temperature koji-scented aroma as the base tone and possessing a special aroma and experience.

[0021] Furthermore, based on the components of the high-temperature Daqu (a type of Chinese koji) reference sample, the total weight percentage of nitrogen-containing heterocyclic compounds is adjusted to 0.80~1.00‰, and the total weight percentage of amines is adjusted to 0~0.0010‰, to obtain a koji liquid with nutty / cocoa / chocolate aromas; the adjustments include, but are not limited to: deleting specific compounds, increasing or decreasing the content of specific compounds, so that the total content of that category in the final formula reaches the target range.

[0022] Furthermore, based on the components of the high-temperature Daqu (a type of starter culture) reference sample, the weight percentage of coconut aldehyde was adjusted to 0.001~0.005‰ to obtain a starter culture liquid with a coconut aroma.

[0023] Furthermore, based on the components of the high-temperature Daqu (a type of Chinese liquor) fragrance reference sample, the total weight percentage of benzyl alcohol and phenylethanol was adjusted to 0.10~0.20‰, and the proportion of phenylethanol exceeded 50%, resulting in a fragrance liquid with a rose aroma.

[0024] Furthermore, based on the components of the high-temperature Daqu (a type of Chinese liquor) reference sample, the total weight percentage of benzaldehyde and phenylacetaldehyde was adjusted to 0.10~0.20‰, with phenylacetaldehyde accounting for more than 50%, resulting in a Daqu fragrance liquid with an almond aroma.

[0025] Furthermore, based on the components of the high-temperature Daqu (a type of starter culture) reference sample, at least two aroma compounds from the following sources are added: 0.01~0.05‰ of terpineol, 0.01~0.05‰ of linalool, 0.01~0.05‰ of eucalyptol, and 0.01~0.05‰ of lanolinol, to obtain a Daqu aroma liquid with prominent floral and fruity aroma, refreshing and pleasant.

[0026] Fourthly, the present invention provides the application of the above-mentioned high-temperature Daqu (a type of starter culture) reference sample or Daqu liquid in the preparation of aroma bottles or aroma cards for sensory training, quality assessment or promotional display.

[0027] Fifthly, the present invention provides the application of the above-mentioned high-temperature Daqu (a type of starter culture) reference sample or starter culture liquid in the preparation of alcoholic beverages or tobacco products.

[0028] The beneficial effects of the present invention are as follows: The high-temperature Daqu (a type of starter culture) aroma reference sample and related high-temperature Daqu aroma liquid prepared by the present invention are developed to meet the needs of liquor brewing and scientific research enterprises. At present, there are no related technical products on the market, which has the following significance.

[0029] (1) Compared with the prior art, the present invention has for the first time achieved the chemical standardization reconstruction of the typical aroma characteristics of high-temperature Daqu. The reference sample of the present invention is obtained through chemical formulation, which fundamentally overcomes the inherent defects of traditional simulated fermentation method in batch consistency and stability of reference sample preparation, thus providing a stable and reliable sensory evaluation benchmark for the quality control of core raw materials of sauce-flavored liquor.

[0030] (2) Through systematic aroma component analysis and screening, this invention successfully identified only 38 key aroma active compounds from the complex volatile system of high-temperature koji and determined their optimal ratio range. The formula provided by this invention simulates the aroma of high-temperature koji with "sour fermented soybean aroma" and "roasted nut aroma" as the main aroma components, greatly reducing the technical complexity and cost, while providing a key tool for related scientific research and technical training.

[0031] (3) Furthermore, based on the basic formula of the high-temperature Daqu (a type of Chinese liquor) reference sample of this invention, the content and total proportion of specific compounds can be quantitatively adjusted to derive a liquor with special aroma characteristics. This predictable and controllable aroma design method lays a solid technical foundation for the innovative introduction of the traditional flavor characteristics of high-temperature Daqu into a wider range of fields such as tobacco, modern blended wines, and food. Attached Figure Description

[0032] Figure 1 This is a schematic diagram of the aroma characteristics of premium and first-grade sauce-flavored baijiu as shown in GB / T 10781.4-2024. Detailed Implementation

[0033] To make the technical problems, solutions, and beneficial effects of this application clearer, the following detailed description is provided in conjunction with the embodiments. Unless otherwise defined, all technical terms used herein have the same meaning as understood by one of ordinary skill in the art.

[0034] This invention measures and analyzes the aroma compounds of dozens of typical high-temperature Daqu samples from different production areas across the country; conducts extensive literature reviews; engages in in-depth discussions and exchanges with experts and technicians from brewing enterprises; and purchases standard compounds to conduct aroma reconstruction, loss, and addition experiments. Ultimately, it formulates a high-temperature Daqu aroma reference sample that is stable, has a realistic aroma, and a harmonious fragrance. The high-temperature Daqu aroma reference sample prepared by this invention is stable, has a realistic aroma, and a harmonious fragrance, providing important support for the standardization and normalization of an aroma-oriented high-temperature Daqu quality assessment system.

[0035] This invention provides a high-temperature Daqu (a type of Chinese liquor) reference sample, the components of which include 38 compounds and a solvent by weight percentage, wherein the solvent is propylene glycol; the 38 compounds are shown in Table 1.

[0036] Table 1. Reference Samples of High-Temperature Daqu Fermentation

[0037] All 38 compounds in Table 1 are widely present in high-temperature Daqu and are the main aroma compounds of high-temperature Daqu. This invention obtained the high-temperature Daqu aroma reference sample formula shown in Table 1 by repeatedly preparing monomer raw materials. With this formula, a standard aroma reference sample of medium-temperature Daqu with rich aroma, realistic aroma and stable properties can be prepared.

[0038] In one embodiment of the present invention, the formulations of the 38 compounds in Table 1 are standard formulations for preparing high-temperature Daqu (a type of starter culture) aroma reference samples. These formulations can be adjusted to obtain aroma reference liquids with typical aromas of white, yellow, and black Daqu. White, yellow, and black Daqu are three types of Daqu whose colors range from light to dark due to differences in their placement during the preparation of high-temperature Daqu. While possessing the basic aroma of high-temperature Daqu, these three types of Daqu each have their own unique aroma profiles.

[0039] Among them, white koji has a more prominent roasted and grain aroma, but a weaker sour aroma. Preferably, by adjusting the total weight percentage of aldehydes in Table 1 to 0.50~1.00‰, the total weight percentage of nitrogen-containing heterocyclic compounds (mainly pyrazines) to 0.20~0.50‰, and the acid content to 0.10~0.30‰, a white koji aroma liquid with prominent roasted and grain aroma can be prepared. Yellow koji has a prominent sour aroma, roasted aroma, and rich floral and fruity aroma. Preferably, by adjusting the total weight percentage of acids in Table 1 to 0.50~1.00‰, the total weight percentage of nitrogen-containing heterocyclic compounds (mainly pyrazines) to 0.20~0.50‰, and the total weight percentage of esters to 0.10~0.20‰, a yellow koji aroma liquid with prominent sour and roasted aroma and rich floral and fruity aroma can be prepared. The black koji has a prominent roasted and charred aroma, and a rich floral and fruity aroma. Preferably, the total weight percentage of nitrogen-containing heterocyclic compounds (mainly pyrazines) in Table 1 is adjusted to 0.20~0.50‰, the total weight percentage of oxygen-containing heterocyclic compounds is adjusted to 0.10~0.20‰, the phenols are adjusted to 0.05~0.10‰, and the total weight percentage of esters is adjusted to 0.10~0.20‰, thus obtaining a black koji fragrance liquid with a prominent roasted and charred aroma and a rich floral and fruity aroma.

[0040] In one embodiment of the present invention, the formulation of the 38 compounds in Table 1 is a standard formulation for preparing a high-temperature Daqu (a type of Chinese koji) fragrance reference sample. The formulation can be adjusted based on this to obtain a koji fragrance liquid with a certain typical characteristic aroma and flavor, based on the high-temperature Daqu fragrance. Preferably, adjusting the total weight percentage of nitrogen-containing heterocyclic compounds (mainly pyrazines) in Table 1 to 0.80~1.00‰ and the total weight percentage of amines to 0~0.0010‰ will yield a koji liquid with typical nutty / cocoa / chocolate aromas; adjusting the weight percentage of coconut aldehyde to 0.001~0.005‰ will yield a koji liquid with typical coconut aromas; adjusting the total weight percentage of benzyl alcohol and phenylethanol (where the phenylethanol content must exceed 50%) to 0.10~0.20‰ will yield a koji liquid with typical rose aromas; and adjusting the total weight percentage of benzaldehyde and phenylacetaldehyde (where the phenylacetaldehyde content must exceed 50%) to 0.10~0.20‰ will yield a koji liquid with typical almond aromas.

[0041] In one embodiment of the present invention, the "adjustment" of the formulation includes, but is not limited to: deleting or reducing the content of specific compounds, increasing or decreasing the content of specific compounds, so that the total content of that category in the final formulation reaches the target range. Taking the preparation of a flavoring liquid with typical nutty / cocoa / chocolate aromas as an example, this flavoring liquid is an adjustment to the standard formulation of a high-temperature koji (fermented grain) flavoring reference sample. Specifically, the total weight percentage of nitrogen-containing heterocyclic compounds (mainly pyrazines) is adjusted to 0.80~1.00‰, and the total weight percentage of amines is adjusted to 0~0.0010‰. This adjustment can be achieved by increasing the content of core pyrazine compounds, such as 2-methylpyrazine, 2,3-dimethylpyrazine, 2,5-dimethylpyrazine, etc. The aroma liquid with typical nutty / cocoa / chocolate aroma can be prepared by using one or more of 2,6-dimethylpyrazine, 2,3,5-trimethylpyrazine, tetramethylpyrazine, 2-ethyl-6-methylpyrazine, and 2-acetylpyrrole, and optionally by deleting some compounds of nitrogen-containing heterocyclic compounds that are present in very small amounts or contribute little to the aroma, such as one or more of 2,3-dimethyl-5-ethylpyrazine, 2-pyrrolecarboxaldehyde, and 2,3,5-trimethyl-6-ethylpyrazine.

[0042] In one embodiment of the present invention, the 38 compounds in Table 1 are the basic formula for preparing the high-temperature Daqu (a type of Chinese liquor) fragrance reference sample. Other aroma compounds can be added to this formula to obtain a fragrance liquid with a special aroma and experience based on the high-temperature Daqu fragrance. For example, adding all or 2-3 of the following compounds to the formula, such as linalool (0.01-0.05‰), eucalyptol (0.01-0.05‰), and eucalyptol (0.01-0.05‰), can produce a fragrance liquid with prominent floral and fruity aroma, refreshing and pleasant.

[0043] This invention provides a method for preparing the above-mentioned high-temperature Daqu (a type of starter culture) reference sample, comprising the following steps:

[0044] (1) Classification premixing: All compounds in the above high-temperature Daqu koji reference sample, except for the solvent, are classified according to their chemical structure and mixed with a portion of the solvent to prepare multiple categories of premixed liquids;

[0045] (2) Standing and maturation: Let the various premixed liquids obtained in step (1) stand for 6 to 24 hours respectively;

[0046] (3) Final mixing: Mix the various premixed liquids after standing, and add solvent to make up the total amount. Stir evenly and let stand for 24-48 hours to obtain a high-temperature Daqu aroma reference sample with a realistic, harmonious and rich aroma.

[0047] In one embodiment of the present invention, the classification in step (1) includes alcohols, aldehydes, ketones, acids, esters, aromatics, nitrogen-containing heterocycles, oxygen-containing heterocycles, phenols, terpenes, and amines. Mixing the raw material compounds separately according to their classification is the optimal mixing method for preparing high-temperature Daqu reference samples. Classified premixing allows similar compounds to fully integrate according to the principle of "like dissolves like," resulting in a richer aroma while maintaining harmony and stability. Experiments show that it is also possible to directly mix the raw materials to form high-temperature Daqu reference samples without classification, but the effect is not as good as classified premixing.

[0048] In one embodiment of the present invention, the time for the premixed liquid to stand for 6 to 24 hours in step (2) is the time for various raw material compounds to combine, react, and finally reach a steady state. Among them, 12 hours is the optimal time. Alternatively, the various premixed liquids can be directly mixed without standing, but the effect is not as good as the premixed liquid after standing.

[0049] In one embodiment of the present invention, the optimal order for mixing the premix in step (3) is to first mix compounds with weak aroma or atypical odor, followed by compounds with strong odor or typical odor characteristics. The recommended mixing order is: alcohols, acids, esters, aromatic compounds, aldehydes, ketones, oxygen-containing heterocycles, nitrogen-containing heterocycles, phenols, terpenes, and amines. Experimental results show that mixing in this order yields the best results. After the premix is ​​thoroughly mixed, it can be used directly, and the effect is even better after standing for 24-48 hours.

[0050] The following specific embodiments will be provided to explain the solution of the present invention. Those skilled in the art will understand that the following embodiments are for illustrative purposes only and should not be considered as limiting the scope of the invention. Where specific techniques or conditions are not specified in the embodiments, they are performed according to the techniques or conditions described in the literature in the field or according to the product instructions. Reagents or instruments whose manufacturers are not specified are all conventional products that can be obtained commercially.

[0051] Example 1: Preparation of High-Temperature Daqu Fermentation Reference Sample

[0052] (1) First, premix the compounds according to the categories shown in Table 1: Prepare 11 100mL fragrance bottles (numbered 1~11), corresponding to alcohols, acids, esters, aromatics, aldehydes, ketones, oxygen-containing heterocycles, nitrogen-containing heterocycles, phenols, terpenes, and amines, respectively. Add 50 g of propylene glycol to each bottle as a solvent, and then accurately add the corresponding aroma compounds according to the category. After the addition is complete, use a clean stirring rod to stir the solution in each bottle until it is evenly mixed, and let it stand at room temperature for 12 hours to obtain the premixed solution of each category, which is ready for use.

[0053] The specific amounts of aroma compounds added to each perfume bottle are as follows: Bottle 1 contains 0.50g isoamyl alcohol, 0.01g n-hexanol, 0.03g mushroom alcohol, and 0.08g 3-octanol; Bottle 2 contains 15.00g isovaleric acid and 5.00g isobutyric acid; Bottle 3 contains 1.00g methyl acetate, 0.01g methyl hexanoate, 0.20g methyl isovalerate, and 0.1g methyl laurate. 0g, methyl palmitate 0.10g; Add benzyl alcohol 2.00g, phenylethanol 2.00g, benzaldehyde 0.20g, phenylacetaldehyde 0.20g, acetophenone 0.20g, 1,2-dimethoxybenzene 0.10g, methyl benzoate 0.02g, methyl phenylacetate 0.02g to bottle 4; Add 2-methylbutyraldehyde 1.00g, isovaleraldehyde 2.00g to bottle 5; Add 2-methylbutyraldehyde to bottle 6 Add 0.10g of 2-octanone to bottle 7; add 0.002g of coconut aldehyde and 0.50g of furfural to bottle 8; add 0.02g of 2-methylpyrazine, 0.02g of 2,3-dimethylpyrazine, 1.00g of 2,5-dimethylpyrazine, 0.20g of 2,6-dimethylpyrazine, 0.50g of 2,3,5-trimethylpyrazine, 2.00g of tetramethylpyrazine, 0.02g of 2-ethyl-6-methylpyrazine, 0.03g of 2,3,5-trimethyl-6-ethylpyrazine, 0.50g of 2-pyrrolecarboxaldehyde, and 0.50g of 2-acetylpyrrole to bottle 9; add 0.20g of 4-vinylguaiacol to bottle 10; add 0.01g of geraniol to bottle 11; and add 0.05g of trimethylamine to bottle 11.

[0054] (2) Transfer all the premixed liquids to a main container in the order of the fragrance bottles numbered 1 to 11. Then add propylene glycol to the container until the total mass of the mixture reaches 1 kg, and stir with a clean stirring rod until completely homogeneous. Let this mixture stand at room temperature for 48 hours to mature, and obtain a 100-fold concentration of high-temperature Daqu (a type of Chinese liquor) fragrance concentrate. Take 1 part of this concentrate, add 99 parts of propylene glycol for dilution, mix well, and let it stand at room temperature again for 24 hours to obtain a high-temperature Daqu fragrance reference sample that can be used directly.

[0055] Example 2: Sensory evaluation and acceptance of high-temperature Daqu (a type of Chinese liquor) reference sample

[0056] The inventor assembled a sensory evaluation team of 60 people, including 20 national and provincial judges and researchers of baijiu, 20 koji-making and brewing workers, and 20 strong-aroma baijiu consumers. The participants were aged between 22 and 45, with 40 men and 20 women. They were all in good health and had no olfactory impairment. The inventor signed informed consent forms with all volunteers who participated in the sensory experiment.

[0057] (1) First, all volunteers participating in the experiment received three weeks of training in sensory description and analysis, five times a week for two hours each time. The training content included basic knowledge of sensory analysis, identification of sensory characteristics, and the establishment and use of scales;

[0058] (2) By reviewing literature, national standards and sensory group discussions, the aroma of high-temperature Daqu is divided into 10 aromas: roasted / nut aroma, grain aroma, floral / fruit aroma, fermented black bean / sour aroma, grass / wood aroma, smoked / caramel aroma, sweet / honey aroma, oily aroma, earthy / mold aroma, and unpleasant aroma. The percentage of their scores is shown in Table 2.

[0059] (3) The sensory group scored the high-temperature Daqu and the prepared high-temperature Daqu aroma reference sample on a 10-point scale. The aroma intensity was divided into five levels: 1-2 is "very weak" aroma, 3-4 is "slightly weak" aroma, 5-6 is "medium" aroma, 7-8 is "slightly strong" aroma, and 9-10 is "very strong" aroma. Finally, the average value was taken and one significant figure was retained. The sensory evaluation results of the high-temperature Daqu aroma reference sample prepared in Example 1 are shown in Table 2.

[0060] Table 2 Sensory evaluation results of the high-temperature Daqu (a type of starter culture) reference sample prepared in Example 1

[0061] As shown in Table 2, the reference sample prepared by the method of the present invention has a distinct aroma of high-temperature Daqu (a type of starter culture). The aroma profile is basically the same as that of high-temperature Daqu, with the main aromas being fermented soybean / sour, roasted / nutty, oily, grain, and floral / fruity, followed by sweet / honey, smoky / caramel, and grassy / woody aromas.

[0062] (4) The sensory panel evaluated whether the reference sample prepared by the method of the present invention could be used as a reference sample for high-temperature Daqu (a type of Chinese liquor) and calculated the percentage of samples that were accepted as reference samples for high-temperature Daqu. The results are shown in Table 3.

[0063] Table 3. Evaluation Results of Acceptance of High-Temperature Daqu Fermentation Reference Sample

[0064] As shown in Table 3, the approval rate of the three types of sensory evaluators was higher than 85%, with the approval rate of national and provincial judges of baijiu, scientific researchers, and koji-making and brewing workers reaching 90%. This indicates that the reference sample is highly consistent with the aroma of high-temperature daqu koji and can be used as a reference sample for the aroma of high-temperature daqu koji.

[0065] Example 3: Preparation of a flavoring liquid with typical nutty / cocoa / chocolate aromas

[0066] Prepare 1 kg of a 100x concentrated liquid with a koji-based aroma and typical nutty / cocoa / chocolate notes. This formula does not contain 2,3-dimethyl-5-ethylpyrazine, 2-pyrrolecarboxaldehyde, 2,3,5-trimethyl-6-ethylpyrazine, or trimethylamine. The remaining 34 compounds are all on the list of permitted synthetic flavorings for food use as specified in GB 2760-2024. The specific steps are as follows:

[0067] (1) First, premix the compounds according to the categories shown in Table 1: Prepare 10 100mL fragrance bottles (numbered 1~10), corresponding to alcohols, acids, esters, aromatics, aldehydes, ketones, oxygen-containing heterocycles, nitrogen-containing heterocycles, phenols, and terpenes in sequence. Add 50 g of propylene glycol to each bottle as a solvent, and then accurately add the corresponding aroma compounds according to the category. After the addition is complete, use a clean stirring rod to stir the solution in each bottle until it is evenly mixed, and let it stand at room temperature for 12 hours to obtain the premixed solution of each category for later use.

[0068] The specific amounts of aroma compounds added to each perfume bottle are as follows: Bottle 1 contains 0.50g of isoamyl alcohol, 0.01g of n-hexanol, 0.03g of mushroom alcohol, and 0.08g of 3-octanol; Bottle 2 contains 15.00g of isovaleric acid and 5.00g of isobutyric acid; Bottle 3 contains 1.00g of methyl acetate, 0.01g of methyl hexanoate, 0.20g of methyl isovalerate, 0.10g of methyl laurylate, and 0.10g of methyl palmitate; Bottle 4 contains 2.00g of benzyl alcohol, 2.00g of phenethyl alcohol, 0.20g of benzaldehyde, 0.20g of phenylacetaldehyde, 0.20g of acetophenone, 0.10g of 1,2-dimethoxybenzene, 0.02g of methyl benzoate, and methyl phenylacetate. 0.02g; Add 1.00g of 2-methylbutyraldehyde and 2.00g of isovaleraldehyde to bottle 5; Add 0.10g of 2-octanone to bottle 6; Add 0.002g of cocoaldehyde and 0.50g of furfural to bottle 7; Add 0.5g of 2-methylpyrazine, 0.5g of 2,3-dimethylpyrazine, 2.00g of 2,5-dimethylpyrazine, 1.00g of 2,6-dimethylpyrazine, 2.50g of 2,3,5-trimethylpyrazine, 2.50g of tetramethylpyrazine, 0.05g of 2-ethyl-6-methylpyrazine, and 0.50g of 2-acetylpyrrole to bottle 8; Add 0.20g of 4-vinylguaiacol to bottle 9; Add 0.01g of geraniol to bottle 10.

[0069] (2) Transfer all the premixed liquids to a master container in the order of the fragrance bottles numbered 1 to 10. Then add propylene glycol to the container until the total mass of the mixture reaches 1 kg, and stir with a clean stirring rod until completely homogeneous. Let this mixture stand at room temperature for 4 days to mature, and obtain a 100-fold concentration of fragrance liquid with a koji aroma as the base and a typical nutty / cocoa / chocolate flavor.

[0070] The flavoring liquid prepared by this method, which has typical nutty / cocoa / chocolate aromas, can be used in tobacco, tobacco capsules, e-cigarettes, prepared wines, chocolate, coffee, milk tea, puffed foods, and other fields.

[0071] Example 4: Preparation of flavored popping boba with typical nut / cocoa aromas

[0072] (1) Add 100g of glycerol to 200g of purified water, and then add 10g of the koji aroma liquid (100 times concentrated liquid) prepared in Example 3 with koji aroma as the base and typical nut / cocoa / chocolate aroma. Stir evenly, add a small amount of food coloring as needed to adjust the color, and stir with a magnetic stirrer at a speed of 500r / min for 20min until evenly mixed.

[0073] (2) Heat 670g of pure water to 60℃ and maintain the temperature. While stirring continuously, slowly add 20g of sodium alginate, maintain the temperature at 60℃ and continue stirring until the sodium alginate is completely dissolved to form a uniform, particle-free transparent colloidal solution.

[0074] (3) Mix the solutions prepared in steps (1) and (2) and stir continuously for 1 hour to ensure that a uniform colloidal solution is formed.

[0075] (4) Using a dripping device, the colloidal liquid obtained in step (3) is precisely dripped into a curing tank containing a 2% (w / v) calcium chloride (CaCl2) aqueous solution for curing to form spherical burst beads. The diameter of the formed burst beads is controlled at 2~3 mm.

[0076] (5) Remove the cured popping beads from the CaCl2 solution and rinse them 2-3 times with pure water to remove residual CaCl2. Place the popping beads in a dryer and dry them at 35°C for 30 minutes. Select qualified popping beads and store them in a sealed container to obtain popping beads with a koji aroma as the base and a typical nutty / cocoa / chocolate flavor.

[0077] The prepared flavor capsules can be used to make high-end cigarettes with a koji-based aroma and typical nutty / cocoa / chocolate notes.

[0078] Example 5: Sensory evaluation of a flavored menthol cigarette with typical nutty / cocoa aroma.

[0079] The flavor capsules prepared in Example 4 were placed in the middle section of a blank cigarette filter and evaluated by 13 professional cigarette sensory evaluators. The sensory evaluation method in this invention was formulated with reference to YC / T 497-2014 "Sensory Evaluation Method for Chinese Style Cigarettes". The score was based on a 10-point scale, and the average value of the results was taken, with one significant figure retained. The results are shown in Table 4.

[0080] Table 4 Sensory evaluation of cigarettes with a koji-based aroma and typical nutty / cocoa / chocolate notes.

[0081] According to the sensory evaluation results: compared with blank cigarettes, the addition of the flavor capsules prepared according to this invention, which are based on a koji aroma and have typical nutty / cocoa / chocolate flavors, significantly improved the aroma and richness, with sensory scores increasing by more than 0.5 points. The cocoa and nutty aromas in the smoke were significantly enhanced, with scores increasing by more than 2.0 points. The fruity, woody, fresh, floral, herbal, balsamic, and caramel sweet aromas were also significantly enhanced. These results indicate that the flavor capsules prepared according to this invention, which are based on a koji aroma and have typical nutty / cocoa / chocolate flavors, can not only highlight the cocoa, nutty, and roasted aroma characteristics of cigarettes, but also significantly enhance the floral, fruity, and woody aromas, effectively improving the quality of the smoke.

[0082] Example 6: Preparation of High-Temperature Daqu Slow-Release Fragrance Card

[0083] (1) Carrier treatment: a quantitative method of 200 g / m³ was selected. 2 Cellulose paper is used as the carrier substrate and is dusted before use to ensure uniform coating adhesion and enhance its durability and reusability.

[0084] (2) Pattern printing: Design the logo and text description related to high temperature koji according to the size of the finished card (5cm×7cm); use environmentally friendly UV ink for printing, and use UV curing lamp to fully cure the ink to ensure that the pattern is clear, stable and free of solvent residue.

[0085] (3) Preparation of coating solution: Prepare the slow-release coating solution according to the following weight percentages:

[0086] The composition of the sustained-release agent is polyvinyl alcohol (PVA) 5.0%, the film-forming agent is acrylic emulsion 2.0%, the flexibility agent is propylene glycol 1.0%, the crosslinking agent is glutaraldehyde 0.5%, the high-temperature Daqu koji concentrate prepared in Example 1 and aged for ≥1 month is 1.0%, and the remainder is deionized water.

[0087] (4) Solution preparation: First, slowly add polyvinyl alcohol to deionized water at 60°C while stirring, and continue stirring until completely dissolved to obtain a transparent solution, then cool to room temperature. While stirring continuously, add acrylic emulsion, propylene glycol and glutaraldehyde in sequence, and mix evenly. Finally, slowly add high-temperature Daqu (a type of Chinese liquor) concentrated liquor under low-speed stirring to avoid the volatilization of aroma components caused by vigorous stirring, until the system is evenly mixed.

[0088] (5) Coating and drying: Use a coating machine to evenly coat the prepared coating solution onto the surface of the printed cellulose paper, controlling the wet film thickness within the range of 20~50μm. Then dry at 50~60℃ for 1~2h to allow the coating to fully form a film and the base liquid to be firmly embedded in the slow-release coating.

[0089] (6) Cutting and Packaging: Cut the dried coated substrate into standard sizes of 5cm×7cm and remove irregular edges. Seal the qualified fragrance cards individually in aluminum foil bags or polyethylene sealed bags to prevent fragrance loss and facilitate storage, transportation and use.

[0090] According to the evaluation of the professional sensory panel, the aroma card prepared in this embodiment has a pure aroma and has the typical characteristics of high-temperature Daqu (a type of Chinese koji). The aroma release is stable and long-lasting. Combined with customized high-temperature Daqu-related patterns and text descriptions, it is suitable for domestic and international application scenarios such as quality control training, technical exchanges, and market promotion of high-temperature Daqu.

Claims

1. A high-temperature Daqu koji aroma reference sample, characterized in that, The components include, by weight percentage: isopentyl alcohol 0.002-0.010‰, n-hexanol 0.00005-0.0002‰, mushroom alcohol 0.0001-0.0007‰, 3-octanol 0.0005-0.0020‰, 2-methylbutyraldehyde 0.004-0.030‰, isovaleraldehyde 0.010-0.060‰, 2-octanone 0.0005-0.0015‰, isovaleric acid 0.050-0.300‰, isobutyric acid 0.020-0.200‰, methyl acetate 0.005-0.020‰, methyl hexanoate 0.00005-0.00020‰, methyl isovalerate 0.001-0.005‰, methyl laurate 0.0005-0.003‰, methyl palmitate 0.0005-0.0020‰, benzyl alcohol 0.005-0.050‰, phenethyl alcohol 0.005-0.050‰, benzaldehyde 0.001-0.005‰, phenylacetaldehyde 0.001-0.005‰, acetophenone 0.001-0.005‰, 1,2-dimethoxybenzene 0.0005-0.003‰, methyl benzoate 0.0001-0.0005‰, methyl phenylacetate 0.0001-0.0005‰, 2-methylpyrazine 0.0001-0.0005‰, 2,3-dimethylpyrazine 0.0001-0.0005‰, 2,5-dimethylpyrazine 0.005-0.030‰, 2,6-dimethylpyrazine 0.001-0.005‰, 2,3,5-trimethylpyrazine 0.002-0.010‰, ligustilide 0.005-0.050‰, 2-ethyl-6-methylpyrazine 0.0001-0.0005‰, 2,3-dimethyl-5-ethylpyrazine 0.0002-0.0006‰, 2,3,5-trimethyl-6-ethylpyrazine 0.0001-0.0005‰, 2-pyrrolecarboxaldehyde 0.0020-0.0100‰, 2-acetylpyrrole 0.003-0.010‰, coconut aldehyde 0.00001-0.00005‰, furfural 0.002-0.010‰, 4-vinylguaiacol 0.001-0.005‰, geranon 0.00005-0.00020‰, trimethylamine 0.0002-0.0010‰, and the balance is a solvent; the solvent is propylene glycol.

2. The high-temperature Daqu flavor reference sample according to claim 1, characterized in that: The high-temperature Daqu is any one of white Daqu, yellow Daqu and black Daqu; The components of the white Daqu aroma reference liquid are: on the basis of the components of the high-temperature Daqu aroma reference sample, the total weight percentage of aldehydes is adjusted to 0.50-1.00‰, the total weight percentage of nitrogen-containing heterocyclic compounds is adjusted to 0.20-0.50‰, and the total weight percentage of acids is adjusted to 0.10-0.30‰; The components of the yellow Daqu aroma reference liquid are: on the basis of the components of the high-temperature Daqu aroma reference sample, the total weight percentage of acids is adjusted to 0.50-1.00‰, the total weight percentage of nitrogen-containing heterocyclic compounds is adjusted to 0.20-0.50‰, and the total weight percentage of esters is adjusted to 0.10-0.20‰. The components of the black koji aroma reference liquid are: on the basis of the components of the high-temperature daqu aroma reference sample, adjusting the total weight percentage of nitrogen-containing heterocyclic compounds to 0.20-0.50‰, the total weight percentage of oxygen-containing heterocyclic compounds to 0.10-0.20‰, the total weight percentage of phenols to 0.05-0.10‰, and the total weight percentage of esters to 0.10-0.20‰.

3. The preparation method of the high-temperature Daqu flavor reference sample, characterized in that, The method comprises the following steps: (1) classified premixing: all compounds except solvent in the components of the high-temperature daqu aroma reference sample according to claim 1 or 2 are classified according to their chemical structures, and are mixed with part of the solvent respectively to prepare a plurality of category premixing liquids; (2) standing and maturing: each category premixing liquid obtained in step (1) is respectively stood for 6-24 hours; (3) final mixing: the category premixing liquids after standing are mixed, and the total amount is supplemented with solvent, and after stirring uniformly, standing for 24-48 hours to obtain the high-temperature daqu aroma reference sample.

4. The method for preparing the high-temperature Daqu flavor reference sample according to claim 3, characterized in that: In step (1), the classification includes alcohols, aldehydes, ketones, acids, esters, aromatics, nitrogen-containing heterocyclic compounds, oxygen-containing heterocyclic compounds, phenols, terpenes and amines.

5. The method for preparing the high-temperature Daqu flavor reference sample according to claim 3, characterized in that: In step (3), the category premixing liquids are mixed in the order of alcohols, acids, esters, aromatics, aldehydes, ketones, oxygen-containing heterocyclic compounds, nitrogen-containing heterocyclic compounds, phenols, terpenes and amines.

6. A liquid for flavoring, characterized by: It is based on the components of the high-temperature daqu aroma reference sample according to claim 1, by adjusting the content of specific compounds and / or introducing other aroma compounds, thereby forming a daqu aroma liquid with high-temperature daqu aroma as the base tone and special aroma and experience.

7. The liquid according to claim 6, wherein: On the basis of the components of the high-temperature daqu aroma reference sample, the total weight percentage of nitrogen-containing heterocyclic compounds is adjusted to 0.80-1.00‰, and the total weight percentage of amines is adjusted to 0-0.0010‰, to obtain a daqu aroma liquid with nut / cocoa / chocolate aroma; or the weight percentage of coconut aldehyde is adjusted to 0.001-0.005‰, to obtain a daqu aroma liquid with coconut aroma; or the total weight percentage of benzyl alcohol and phenethyl alcohol is adjusted to 0.10-0.20‰, and the proportion of phenethyl alcohol is more than 50%, to obtain a daqu aroma liquid with rose flower aroma; or the total weight percentage of benzaldehyde and phenylacetaldehyde is adjusted to 0.10-0.20‰, and the proportion of phenylacetaldehyde is more than 50%, to obtain a daqu aroma liquid with almond aroma.

8. The liquid according to claim 6, wherein: On the basis of the components of the high-temperature daqu aroma reference sample, at least two aroma compounds of 0.01-0.05‰ of lahnzhu tea alcohol, 0.01-0.05‰ of linalool, 0.01-0.05‰ of blue eucalyptus alcohol, and 0.01-0.05‰ of lanhxian alcohol are added, to obtain a daqu aroma liquid with prominent fruit aroma, refreshing and comfortable.

9. Use of the high-temperature daqu aroma reference sample according to any one of claims 1-2 or the daqu aroma liquid according to any one of claims 6-8 in the preparation of a smell bottle or smell card for sensory training, quality evaluation or promotional display.

10. Use of the high-temperature daqu aroma reference sample according to any one of claims 1-2 or the daqu aroma liquid according to any one of claims 6-8 in the preparation of liquor or tobacco products.

Images