Preparation method and application of spice

Abstract

The preparation method comprises the following steps: a, carrying out enzymolysis on a fenugreek extract to obtain fenugreek extract enzymatic hydrolysate; b, the fenugreek extract enzymatic hydrolysate and amino acid are subjected to a Maillard reaction, and a Maillard reaction product is obtained; and c, filtering the Maillard reaction product, collecting filtrate, evaporating to remove the solvent under reduced pressure, and dissolving with a propylene glycol solution to obtain the perfume. The fenugreek extract is used as a sugar source, amino acid is added as a nitrogen source, the Maillard reaction is carried out, the prepared Maillard reaction product is used for cigarette flavoring and charging, cigarette fragrance can be enriched, smoke can be fine and smooth, offensive odor of cigarettes can be reduced, irritation can be reduced, and the overall smoking quality of the cigarettes can be improved.

Description

Technical Field

[0001] The present invention relates to the field of fragrance preparation, and in particular to a fragrance preparation method and application thereof. Background Art

[0002] As one of the core technologies of cigarette products, flavors and fragrances can give cigarettes unique aroma style and taste characteristics, and are an important support for improving the core competitiveness of brands. The main precursors of the Maillard reaction are amino acids and reducing sugars, which results in a darker color and a certain aroma for the target product. It is one of the main ways to form tobacco aroma components and accompanies the entire process of tobacco modulation, alcoholization and processing. Some people in China simply use reducing monosaccharides and specific amino acids to react to generate Maillard reaction products, but this kind of flavor has few varieties and a single aroma, and has limited improvement on the quality of tobacco smoking.

[0003] A domestic patent (CN1415717A) discloses a method for producing spices using tobacco extract as raw material, wherein sugar and amino acids are added to tobacco extract to produce Maillard reaction. Although this method utilizes the Maillard reaction, it is difficult to achieve a satisfactory aroma effect due to the single type of sugar added.

[0004] A domestic patent (CN103013665A) discloses a method for preparing a fenugreek extract Maillard reactant. The fenugreek extract obtained by concentrating the ethanol extract of fenugreek seed powder is subjected to a Maillard reaction: fenugreek extract: fructose or glucose or sorbitol: proline in a mass ratio of 10:1:0.6-0.8 to obtain a fenugreek extract Maillard reactant. It can be found that the added ratio of reducing sugar is relatively high, so the added reducing sugar is the sugar source of the Maillard reaction product.

[0005] As a natural tobacco flavor, natural extracts can make up for the lack of aroma in cigarettes. Using mixed sugars of natural flavors as the sugar source for the Maillard reaction can provide aroma substances for the Maillard reaction on the one hand, and on the other hand, it can also give the natural aroma of natural extracts in cigarettes, making the aroma of cigarettes richer, which plays an important role in improving the quality of cigarettes. At present, the use of natural extracts for Maillard reaction in China mainly focuses on using fruit extracts for Maillard reaction to make tobacco flavors.

[0006] Patent (CN106281688A) discloses a method for preparing tobacco flavoring using pineapple extract and aromatic β-amino acids. Pineapple can provide reducing sugar for Maillard reaction, increase fruity aroma and improve aroma quantity and quality, but the richness of aroma needs to be improved.

[0007] Patent (CN114525176A) adds activated yeast to fenugreek water, separates the filtrate after shaking fermentation and concentrates it to obtain fenugreek extract; heats the sugar solution in an oil bath to obtain a caramelized liquid as an external sugar source and reacts it with the Maillard reaction to obtain a fenugreek liquid flavor, which is then dried to obtain a fenugreek solid flavor. On the basis of the original fragrance of fenugreek, a special caramelized aroma and flavor are added, and it also has certain health care functions. Under high temperature heating conditions, the external sugar source may be caramelized, resulting in bitterness covering the sweetness of caramel and producing unpleasant odors, which in turn affects the smoke quality of cigarettes and increases impurities. Summary of the invention

[0008] In order to solve the above technical problems, the present application provides a method and application of preparing Maillard reaction tobacco flavoring using fenugreek extract. The present invention uses biological enzymes to hydrolyze macromolecular substances in fenugreek extract, convert them into reducing sugars, and add amino acids to the enzymatic solution to prepare tobacco flavoring through Maillard reaction, which can effectively prevent excessive caramelization of the sugar source. The present invention uses fenugreek extract as a sugar source and amino acids as a nitrogen source to carry out Maillard reaction. The prepared Maillard reaction product is used for flavoring and adding materials to cigarettes, which can not only enrich the tobacco aroma and make the smoke delicate and transparent, but also reduce the impurities of cigarettes, reduce irritation, and improve the overall smoking quality of cigarettes.

[0009] The present application provides a method for preparing a fragrance, comprising the following steps: a. enzymatically hydrolyzing a fenugreek extract to obtain a fenugreek extract hydrolyzate; b. subjecting the fenugreek extract hydrolyzate to a Maillard reaction with an amino acid to obtain a Maillard reaction product; and c. filtering the Maillard reaction product, collecting the filtrate, distilling off the solvent under reduced pressure, and dissolving the spice with a propylene glycol solution.

[0010] The present application also provides a fragrance prepared by the above preparation method.

[0011] The present application also provides the use of the above-mentioned flavor in tobacco products.

[0012] The beneficial effects brought by this application include but are not limited to: this application uses fenugreek extract as a sugar source for the first time, and adds amino acids as a nitrogen source to prepare Maillard reaction products for cigarette flavoring. The prepared Maillard reaction product is used for cigarette flavoring. After heating, it will crack to form a large amount of aroma substances, with significant roasted sweet, paste and sweet aromas, and it also has a certain effect on improving the aroma of baking and floral aromas, accompanied by weak fruity aromas and fresh aromas; at the same time, in addition to permeability, it has a good effect on the aroma characteristics and smoke characteristics of cigarettes, and the roasted sweet and sweet aromas are more prominent. The roasted sweet aroma is increased by 0.50 points, and it can significantly improve the aroma quality of cigarettes, increase the amount of aroma, reduce impurities, reduce irritation, reduce residues, and further increase the delicate and soft degree of smoke. The Maillard reaction product prepared using fenugreek extract helps to improve the overall smoking quality of cigarettes and has good application prospects in Chinese cigarettes. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] The present application will be further described in the form of exemplary embodiments, which will be described in detail with reference to the accompanying drawings. These embodiments are not restrictive, and include:

[0014] Figure 1 The sensory evaluation results of the Maillard reaction flavor of fenugreek extract (HLM) and the fenugreek extract (HL) according to some examples of the present application are shown. DETAILED DESCRIPTION

[0015] In order to more clearly illustrate the technical solutions of the embodiments of this specification, the following is a brief introduction to the drawings required for the description of the embodiments. Obviously, the drawings described below are only some examples or embodiments of this specification. For ordinary technicians in this field, this specification can also be applied to other similar scenarios based on these drawings without creative work. Unless it is obvious from the language environment or otherwise explained, the same reference numerals in the figures represent the same structure or operation.

[0016] As shown in this specification and claims, unless the context clearly indicates an exception, the words "a", "an", "an" and / or "the" do not refer to the singular and may also include the plural. Generally speaking, the terms "comprise" and "include" only indicate the inclusion of the steps and elements that have been clearly identified, and these steps and elements do not constitute an exclusive list. The method or device may also include other steps or elements.

[0017] Flowcharts are used in this specification to illustrate the operations performed by the system according to the embodiments of this specification. It should be understood that the preceding or following operations are not necessarily performed precisely in order. Instead, the steps may be processed in reverse order or simultaneously. At the same time, other operations may also be added to these processes, or one or more operations may be removed from these processes.

[0018] The present application provides a method for preparing a fragrance, comprising the following steps: a. enzymatically hydrolyzing a fenugreek extract to obtain a fenugreek extract hydrolyzate; b. subjecting the fenugreek extract hydrolyzate to a Maillard reaction with an amino acid to obtain a Maillard reaction product; and c. filtering the Maillard reaction product, collecting the filtrate, distilling off the solvent under reduced pressure, and dissolving the spice with a propylene glycol solution.

[0019] In some embodiments, the fenugreek extract can be prepared by ethanol extraction and cold extraction.

[0020] Ethanol extraction method: Take a certain mass of fenugreek seeds, crush and sieve them, add ethanol solution according to a certain solid-liquid ratio, reflux extraction, filter out the fenugreek powder after cooling, heat and evaporate the filtrate, collect the extract, and obtain the fenugreek ethanol extract.

[0021] Cold soaking extraction method: Take a certain mass of fenugreek seeds, crush them, and use 50 times the amount of water to cold soak and extract at 10°C for 3 times, each time for 1 hour, centrifuge for 10 minutes, collect the supernatant and concentrate it to obtain fenugreek extract.

[0022] In some embodiments, in the step a, the enzymatic hydrolysis step can use biological enzymes for enzymatic hydrolysis. In some embodiments, preferably, in the step a, the biological enzyme can be a mixture of amylase, pectinase and galactomannanase. In some embodiments, more preferably, the mass ratio of the amylase, pectinase and galactomannanase can be (0.5-3): (0.5-3): (0.5-3). In some embodiments, the mass ratio of the amylase, pectinase and galactomannanase can be (0.75-2.75): (0.75-2.75): (0.75-2.75). In some embodiments, the mass ratio of the amylase, pectinase and galactomannanase can be (1-2.5): (1-2.5): (1-2.5). In some embodiments, the mass ratio of the amylase, pectinase and galactomannanase can be (1.25-2.25): (1.25-2.25): (1.25-2.25). In some embodiments, the mass ratio of the amylase, pectinase and galactomannanase can be (1.5-2): (1.5-2): (1.5-2). In some embodiments, the mass ratio of the amylase, pectinase and galactomannanase can be (1.75-2): (1.75-2): (1.75-2). In some embodiments, further preferably, the mass ratio of the amylase, pectinase and galactomannanase can be 1:1:1.

[0023] In some embodiments, in the step a, the mass ratio of the fenugreek extract to the biological enzyme may be (80-120): (0.5-3). In some embodiments, in the step a, the mass ratio of the fenugreek extract to the biological enzyme may be (85-115): (0.75-2.75). In some embodiments, in the step a, the mass ratio of the fenugreek extract to the biological enzyme may be (90-110): (1-2.5). In some embodiments, in the step a, the mass ratio of the fenugreek extract to the biological enzyme may be (95-105): (1.25-2.25). In some embodiments, in the step a, the mass ratio of the fenugreek extract to the biological enzyme may be (100-105): (1.5-2). In some embodiments, in the step a, the mass ratio of the fenugreek extract to the biological enzyme may be (100-105): (1.75-2). In some embodiments, preferably, in the step a, the mass ratio of the fenugreek extract to the biological enzyme may be 100:1.5.

[0024] In some embodiments, in step a, before enzymolysis, the fenugreek extract is diluted with distilled water and sterilized by high pressure. In some embodiments, preferably, the mass volume ratio of the fenugreek extract to distilled water can be 10% to 30% (g / mL). For example, the mass volume ratio of the fenugreek extract to distilled water can be 10%, 12%, 14%, 16%, 18%, 20%, 22%, 24%, 26%, 28% or 30% (g / mL). It also includes any range characterized by a combination of the above end values, which will not be repeated here. In some embodiments, more preferably, the mass volume ratio of the fenugreek extract to distilled water can be 20% (g / mL).

[0025] In some embodiments, in the step a, after enzymolysis, the mixture of fenugreek extract, distilled water and biological enzyme is heated at 80-100°C for 15-45 minutes, and then cooled to 25-45°C. In some embodiments, in the step a, after enzymolysis, the mixture of fenugreek extract, distilled water and biological enzyme is heated at 82.5-97.5°C for 17.5-42.5 minutes, and then cooled to 27.5-42.5°C. In some embodiments, in the step a, after enzymolysis, the mixture of fenugreek extract, distilled water and biological enzyme is heated at 85-95°C for 20-40 minutes, and then cooled to 30-40°C. In some embodiments, in the step a, after enzymolysis, the mixture of fenugreek extract, distilled water and biological enzyme is heated at 87.5-92.5°C for 22.5-37.5 minutes, and then cooled to 32.5-37.5°C. In some embodiments, in the step a, after enzymolysis, the mixture of fenugreek extract, distilled water and biological enzyme is heated at 90-92.5°C for 25-35 minutes, and then cooled to 35-37.5°C. In some embodiments, in the step a, after enzymolysis, the mixture of fenugreek extract, distilled water and biological enzyme is heated at 90-92.5°C for 27.5-32.5 minutes, and then cooled to 35-37.5°C. In some embodiments, in the step a, after enzymolysis, the mixture of fenugreek extract, distilled water and biological enzyme can be heated at 90-92.5°C for 30-32.5 minutes, and then cooled to 35-37.5°C.

[0026] In some embodiments, preferably, after enzymolysis, the mixture of fenugreek extract, distilled water and biological enzyme can be heated at 100°C for 35 minutes and then cooled to 35°C.

[0027] In some embodiments, the enzymatic hydrolysis conditions may be 40-60° C. for 4-6 hours. For example, the enzymatic hydrolysis conditions may be 40, 42, 44, 46, 48, 50, 52, 54, 56, 58 or 60° C. Any range characterized by a combination of the above end values ​​is also included, which will not be repeated here.

[0028] For example, the enzymolysis time can be 4, 4.25, 4.5, 4.75, 5, 5.25, 5.5, 5.75 or 6 hours. Any range characterized by a combination of the above end values ​​is also included, which will not be repeated here.

[0029] In some embodiments, preferably, the enzymatic hydrolysis conditions may be 50° C. for 5 hours.

[0030] In some embodiments, in step b, before the Maillard reaction, the fenugreek extract hydrolysate can be mixed with the diluent. In some embodiments, preferably, the mass ratio of the fenugreek extract hydrolysate to the diluent can be (8-12): (3-7). In some embodiments, the mass ratio of the fenugreek extract hydrolysate to the diluent can be (9-11): (4-6). In some embodiments, the mass ratio of the fenugreek extract hydrolysate to the diluent can be (10-11): (5-6). In some embodiments, more preferably, the mass ratio of the fenugreek extract hydrolysate to the diluent can be 2:1.

[0031] In some embodiments, in the step b, the mass ratio of the fenugreek extract hydrolysate to the amino acid can be: (16-24): (0.1-2). In some embodiments, in the step b, the mass ratio of the fenugreek extract hydrolysate to the amino acid can be: (17-23): (0.25-1.75). In some embodiments, in the step b, the mass ratio of the fenugreek extract hydrolysate to the amino acid can be: (18-22): (0.5-1.5). In some embodiments, in the step b, the mass ratio of the fenugreek extract hydrolysate to the amino acid can be: (19-21): (0.75-1.25). In some embodiments, in the step b, the mass ratio of the fenugreek extract hydrolysate to the amino acid can be: (20-21): (1-1.25). In some embodiments, preferably, the mass ratio of the fenugreek extract hydrolysate to the amino acid can be 20:1.

[0032] In some embodiments, in step b, the amino acids may include phenylalanine, threonine, leucine and tryptophan. In some embodiments, preferably, the mass ratio of phenylalanine, threonine, leucine and tryptophan may be (0.6-3): (0.2-1): (0.1-0.5): (0.1-0.5). In some embodiments, the mass ratio of phenylalanine, threonine, leucine and tryptophan may be (1-2.5): (0.4-0.8): (0.2-0.4): (0.2-0.4). In some embodiments, the mass ratio of phenylalanine, threonine, leucine and tryptophan may be (1.5-2): (0.6-0.8): (0.3-0.4): (0.3-0.4). In some embodiments, more preferably, the mass ratio of phenylalanine, threonine, leucine and tryptophan may be 3:1:0.5:0.5.

[0033] In some embodiments, in step b, a catalyst is added before the Maillard reaction. In some embodiments, preferably, the catalyst may be acetic acid. In some embodiments, more preferably, 1 to 5 mL of acetic acid may be added to every 100 g of fenugreek extract hydrolysate. In some embodiments, 2 to 4 mL of acetic acid may be added to every 100 g of fenugreek extract hydrolysate. In some embodiments, 3 to 4 mL of acetic acid may be added to every 100 g of fenugreek extract hydrolysate. In some embodiments, further preferably, 3 mL of acetic acid may be added to every 100 g of fenugreek extract hydrolysate.

[0034] In some embodiments, in step b, the Maillard reaction may be carried out under reflux at 80-100°C for 4-7 hours. In some embodiments, in step b, the Maillard reaction may be carried out under reflux at 85-95°C for 5-6 hours. In some embodiments, in step b, the Maillard reaction may be carried out under reflux at 90-95°C for 5-6 hours. In some embodiments, preferably, the Maillard reaction may be carried out under reflux at 90°C for 5 hours.

[0035] In some embodiments, the diluent may be a mixture of water and anhydrous ethanol. In some embodiments, preferably, the mass ratio of water to anhydrous ethanol may be (1-3): (2-5). In some embodiments, preferably, the mass ratio of water to anhydrous ethanol may be (2-3): (3-4). In some embodiments, more preferably, the mass ratio of water to anhydrous ethanol may be 2:3.

[0036] In some embodiments, in step c, the Maillard reaction product can be cooled to room temperature before filtering.

[0037] In some embodiments, in the step c, the conditions for distilling off the solvent under reduced pressure may be 30-50°C and 40-60Pa. In some embodiments, in the step c, the conditions for distilling off the solvent under reduced pressure may be 32.5-47.5°C and 42.5-57.5Pa. In some embodiments, in the step c, the conditions for distilling off the solvent under reduced pressure may be 35-45°C and 45-55Pa. In some embodiments, in the step c, the conditions for distilling off the solvent under reduced pressure may be 37.5-42.5°C and 47.5-52.5Pa. In some embodiments, in the step c, preferably, the conditions for distilling off the solvent under reduced pressure may be 40°C and 50Pa.

[0038] In some embodiments, the propylene glycol solution may be an aqueous solution of propylene glycol. In some embodiments, preferably, the concentration of the propylene glycol solution may be 20 to 40%. In some embodiments, the concentration of the propylene glycol solution may be 22 to 38%. In some embodiments, the concentration of the propylene glycol solution may be 24 to 36%. In some embodiments, the concentration of the propylene glycol solution may be 26 to 34%. In some embodiments, the concentration of the propylene glycol solution may be 28 to 32%. In some embodiments, more preferably, the concentration of the propylene glycol solution may be 30%.

[0039] The present application also provides a fragrance prepared by the above preparation method.

[0040] The present application also provides the use of the above-mentioned flavor in tobacco products.

[0041] In some embodiments, the tobacco product may include at least one of cigarettes, cigars, shredded tobacco, re-cured tobacco leaves, or tobacco leaves.

[0042] The experimental methods in the following examples are conventional methods unless otherwise specified. The experimental materials used in the following examples are purchased from conventional biochemical reagent companies unless otherwise specified. The quantitative tests in the following examples are repeated three times, and the results are averaged.

[0043] The fenugreek extract used in each embodiment of the present invention was purchased from Xinzheng Jinye Spice Co., Ltd. (JY-1808), and other reagents and raw materials were purchased from conventional markets. Unless otherwise specified, the methods used are conventional methods in the art.

[0044] Example 1

[0045] 100g of fenugreek extract was mixed with distilled water at a ratio of 1:5 (w / v), and the mixture was sterilized in an autoclave to completely inactivate the enzyme activity. Then 1.5g of enzyme (a mixture of amylase, pectinase and galactomannanase (1:1:1)) was added for enzymolysis for 5h at a temperature of 50°C. After the hydrolysis, it was heated at 100°C for 30min to inactivate all enzymes, and then cooled to 35°C to obtain a fenugreek extract hydrolyzate for later use.

[0046] Take 100g of fenugreek extract hydrolyzate, add 20g of water, 30g of anhydrous ethanol, 0.6g of phenylalanine, 0.2g of threonine, 0.1g of leucine and 0.1g of tryptophan, stir and mix evenly, add 3ml of acetic acid (analytical grade) as a catalyst, and reflux for 5h at 90°C. After the reaction is completed, cool to room temperature, filter to remove solid insolubles, evaporate the solvent under reduced pressure at 40°C and 50Pa, and dilute with 30% propylene glycol aqueous solution to obtain the fenugreek extract Maillard reaction flavor.

[0047] The contents of various Maillard reaction intermediates in the prepared Maillard reaction flavors were detected. The results are shown in Table 1.

[0048] Example 2

[0049] 100g of fenugreek extract was mixed with distilled water at a ratio of 1:5 (w / v), and the mixture was sterilized in an autoclave to completely inactivate the enzyme activity. Then 1.5g of enzyme (a mixture of amylase, pectinase and galactomannanase (1:1:1)) was added for enzymolysis for 5h at a temperature of 50°C. After the hydrolysis, it was heated at 100°C for 30min to inactivate all enzymes, and then cooled to 35°C to obtain a fenugreek extract hydrolyzate for later use.

[0050] Take 100g of fenugreek extract hydrolyzate, add 20g of water, 30g of anhydrous ethanol, 3g of phenylalanine, 1g of threonine, 0.5g of leucine and 0.5g of tryptophan, stir and mix evenly, add 3ml of acetic acid (analytical grade) as a catalyst, and reflux for 5h at 90°C. After the reaction is completed, cool to room temperature, filter to remove solid insolubles, evaporate the solvent under reduced pressure at 40°C and 50Pa, and dilute with 30% propylene glycol aqueous solution to obtain fenugreek extract Maillard reaction flavor.

[0051] The contents of various Maillard reaction intermediates in the prepared Maillard reaction flavors were detected. The results are shown in Table 1.

[0052] Example 3

[0053] 100g of fenugreek extract was mixed with distilled water at a ratio of 1:5 (w / v), and the mixture was sterilized in an autoclave to completely inactivate the enzyme activity. Then 1.5g of enzyme (a mixture of amylase, pectinase and galactomannanase (1:1:1)) was added for enzymolysis for 5h at a temperature of 50°C. After the hydrolysis, it was heated at 100°C for 30min to inactivate all enzymes, and then cooled to 35°C to obtain a fenugreek extract hydrolyzate for later use.

[0054] Take 100g of fenugreek extract hydrolyzate, add 20g of water, 30g of anhydrous ethanol, 1.8g of phenylalanine, 0.6g of threonine, 0.3g of leucine and 0.3g of tryptophan, stir and mix evenly, add 1ml of acetic acid (analytical grade) as a catalyst, and reflux for 5h at 90°C. After the reaction is completed, cool to room temperature, filter to remove solid insolubles, evaporate the solvent under reduced pressure at 40°C and 50Pa, and dilute with 30% propylene glycol aqueous solution to obtain fenugreek extract Maillard reaction flavor.

[0055] The contents of various Maillard reaction intermediates in the prepared Maillard reaction flavors were detected. The results are shown in Table 1.

[0056] Example 4

[0057] 100g of fenugreek extract was mixed with distilled water at a ratio of 1:5 (w / v), and the mixture was sterilized in an autoclave to completely inactivate the enzyme activity. Then 1.5g of enzyme (a mixture of amylase, pectinase and galactomannanase (1:1:1)) was added for enzymolysis for 5h at a temperature of 50°C. After the hydrolysis, it was heated at 100°C for 30min to inactivate all enzymes, and then cooled to 35°C to obtain a fenugreek extract hydrolyzate for later use.

[0058] Take 100g of fenugreek extract hydrolyzate, add 20g of water, 30g of anhydrous ethanol, 1.8g of phenylalanine, 0.6g of threonine, 0.3g of leucine and 0.3g of tryptophan, stir and mix evenly, add 5ml of acetic acid (analytical grade) as a catalyst, and reflux for 6h at 90°C. After the reaction is completed, cool to room temperature, filter to remove solid insolubles, evaporate the solvent under reduced pressure at 40°C and 50Pa, and dilute with 30% propylene glycol aqueous solution to obtain fenugreek extract Maillard reaction fragrance.

[0059] The contents of various Maillard reaction intermediates in the prepared Maillard reaction flavors were detected. The results are shown in Table 1.

[0060] Example 5

[0061] 100g of fenugreek extract was mixed with distilled water at a ratio of 1:5 (w / v), and the mixture was sterilized in an autoclave to completely inactivate the enzyme activity. Then 1.5g of enzyme (a mixture of amylase, pectinase and galactomannanase (1:1:1)) was added for enzymolysis for 5h at a temperature of 50°C. After the hydrolysis, it was heated at 100°C for 30min to inactivate all enzymes, and then cooled to 35°C to obtain a fenugreek extract hydrolyzate for later use.

[0062] Take 100g of fenugreek extract hydrolyzate, add 20g of water, 30g of anhydrous ethanol, 1.8g of phenylalanine, 0.6g of threonine, 0.3g of leucine and 0.3g of tryptophan, stir and mix evenly, add 3ml of acetic acid (analytical grade) as a catalyst, and reflux for 5h at 100°C. After the reaction is completed, cool to room temperature, filter to remove solid insolubles, evaporate the solvent under reduced pressure at 40°C and 50Pa, and dilute with 30% propylene glycol aqueous solution to obtain fenugreek extract Maillard reaction fragrance.

[0063] The contents of various Maillard reaction intermediates in the prepared Maillard reaction flavors were detected. The results are shown in Table 1.

[0064] Example 6

[0065] 100g of fenugreek extract was mixed with distilled water at a ratio of 1:5 (w / v), and the mixture was sterilized in an autoclave to completely inactivate the enzyme activity. Then 1.5g of enzyme (a mixture of amylase, pectinase and galactomannanase (1:1:1)) was added for enzymolysis for 5h at a temperature of 50°C. After the hydrolysis, it was heated at 100°C for 30min to inactivate all enzymes, and then cooled to 35°C to obtain a fenugreek extract hydrolyzate for later use.

[0066] Take 100g of fenugreek extract hydrolyzate, add 30g of water, 20g of anhydrous ethanol, 1.8g of phenylalanine, 0.6g of threonine, 0.3g of leucine and 0.3g of tryptophan, stir and mix evenly, add 3ml of acetic acid (analytical grade) as a catalyst, and reflux for 5h at 90°C. After the reaction is completed, cool to room temperature, filter to remove solid insolubles, and then evaporate the solvent under reduced pressure at 40°C and 50Pa, and dilute with 30% propylene glycol aqueous solution to obtain fenugreek extract Maillard reaction fragrance.

[0067] The contents of various Maillard reaction intermediates in the prepared Maillard reaction flavors were detected. The results are shown in Table 1.

[0068] Comparative Example 1

[0069] 100g of fenugreek extract was mixed with distilled water at a ratio of 1:5 (w / v), and the mixture was sterilized in an autoclave to completely inactivate the biological enzyme activity. Then 1.5g of biological enzyme (a mixture of amylase, pectinase and galactomannanase (1:1:1)) was added for enzymolysis at 50°C for 5 hours, and then heated at 100°C for 30 minutes to inactivate all enzymes, and then cooled to 35°C to obtain a fenugreek extract enzymolysis solution for standby use.

[0070] Take 100g of fenugreek extract hydrolyzate, add 20g of water, 30g of anhydrous ethanol, 1.8g of phenylalanine, 0.6g of threonine, 0.3g of leucine and 0.3g of tryptophan, stir and mix evenly, add 3ml of acetic acid (analytical grade) as a catalyst, and reflux for 5h at 90°C. After the reaction is completed, cool to room temperature, filter to remove solid insolubles, and then evaporate the solvent under reduced pressure at 40°C and 50Pa, and dilute with 30% propylene glycol aqueous solution to obtain fenugreek extract Maillard reaction fragrance.

[0071] The contents of various Maillard reaction intermediates in the prepared Maillard reaction flavors were detected. The results are shown in Table 1.

[0072] Comparative Example 2

[0073] 100g of fenugreek extract was mixed with distilled water at a ratio of 1:5 (w / v), and the mixture was sterilized in an autoclave to completely inactivate the biological enzyme activity. Then 1.5g of biological enzyme (a mixture of amylase, pectinase and galactomannanase (1:1:1)) was added for enzymolysis at 50°C for 5h, and then heated at 100°C for 30min to inactivate all enzymes, and then cooled to 35°C to obtain a fenugreek extract enzymolysis solution for standby use.

[0074] Take 100g of fenugreek extract hydrolyzate, add 20g of water, 30g of anhydrous ethanol, 1.8g of phenylalanine and 0.6g of threonine, stir and mix evenly, add 3ml of acetic acid (analytical grade) as a catalyst, and reflux for 5h at 90°C. After the reaction is completed, cool to room temperature, filter to remove solid insolubles, evaporate the solvent under reduced pressure at 40°C and 50Pa, and dilute with 30% propylene glycol aqueous solution to obtain fenugreek extract Maillard reaction fragrance.

[0075] The contents of various Maillard reaction intermediates in the prepared Maillard reaction flavors were detected. The results are shown in Table 1.

[0076] Simultaneous analysis of multiple Maillard reaction intermediates by HPLC-MS / MS

[0077] (1) Extraction of Maillard reaction intermediates

[0078] Accurately weigh 2g of Fenugreek extract Maillard reaction spices, place in a stoppered conical flask, add 70% methanol solution, solid-liquid ratio 1:30 (m / v, g / mL), ultrasonically extract at 100W power for 20min, filter and wash 3 times, combine the filtrate and washing liquid, concentrate to dryness at 30°C using a rotary evaporator under reduced pressure, make the volume to 50mL with 70% methanol solution, then add 30mL of n-hexane to extract five times, remove weak polar impurities such as pigments, retain the methanol-water phase, and obtain the Maillard reaction intermediate extract. Pass through a 0.45μm organic filter membrane for HPLC-MS / MS analysis

[0079] (2) Selection of HPLC-MS / MS conditions

[0080] Chromatographic conditions: Chromatographic column: Thermo Hypersil Gold 100 2.1 (mm), Particle SZ (μm) 1.9; Mobile phase: methanol: water (0.1% formic acid) = 50:50 (V:V); Flow rate: 200 μL / min; Column temperature: 20°C; Injection mode: automatic injection; Injection volume: 2 μL; Nitrogen pressure: 0.6 MPa.

[0081] Mass spectrometry conditions: ion source: electrospray ion source (ESI), positive ionization mode scanning; scanning mode: SRM; capillary temperature: 350°C; ion source spray voltage: 5 kV; helium pressure: 0.25 MPa (sheath gas: 35 Arb, auxiliary gas: 10 Arb); normalized collision energy: 30%; isolation width: 2 m / z.

[0082] Table 1 Maillard reaction intermediate content of different fenugreek extracts and spices

[0083]

[0084] As can be seen from Table 1, the total content of intermediates produced in the Maillard reaction of fenugreek extract exceeds 50 mg / g. By adjusting the type and content of amino acids, the type and content of Maillard reaction intermediates in fenugreek extract can be effectively increased, thereby preparing a fenugreek extract Maillard reaction flavor with a prominent roasted sweet aroma. Among them, the total content of intermediates in the fenugreek extract Maillard reaction flavor in Example 2 is the highest, reaching 60.49 mg / g.

[0085] Sensory evaluation of fenugreek extract Maillard reaction flavor:

[0086] Using Evergrande brand reference cigarettes as a carrier, fenugreek extract Maillard reaction flavor (HLM) was added to the cigarettes, with the added amount being 1 / 10,000, 1.5 / 10,000, 2 / 10,000, 2.5 / 10,000, and 3 / 10,000 of the weight of the tobacco, and placed (humidity 60% ± 2%, temperature 25 ± 1°C) for 48 hours, and evaluated using the emotional indication value scale method. The appropriate amount of fenugreek extract Maillard reaction flavor was determined to be 2.5 / 10,000. According to this amount, fenugreek extract (HL) was added to cigarettes and compared with fenugreek extract Maillard reaction flavor. The results are as follows: Figure 1 shown.

[0087] from Figure 1 It can be seen that both fenugreek extract and fenugreek extract Maillard reaction spices have special herbal aromas, with significant roasted sweet, creamy and sweet aromas, and also have a certain effect on enhancing the roasted and floral aromas, accompanied by weak fruity and fresh aromas; at the same time, in addition to permeability, it has a good effect on the aroma characteristics and smoke characteristics of Evergrande brand cigarettes. Compared with fenugreek extract, the roasted sweet and sweet aromas of fenugreek extract Maillard reaction spices are more prominent, and the roasted sweet aroma is increased by 0.50 points. It can significantly improve the aroma quality of cigarettes, increase the amount of aroma, reduce impurities, reduce irritation, reduce residues, and further increase the delicate and soft degree of smoke. The overall effect is significantly better than fenugreek extract.

[0088] The basic concepts have been described above. Obviously, for those skilled in the art, the above detailed disclosure is only for example and does not constitute a limitation of this specification. Although not explicitly stated here, those skilled in the art may make various modifications, improvements and corrections to this specification. Such modifications, improvements and corrections are suggested in this specification, so such modifications, improvements and corrections still belong to the spirit and scope of the exemplary embodiments of this specification.

[0089] At the same time, this specification uses specific words to describe the embodiments of this specification. For example, "one embodiment", "an embodiment", and / or "some embodiments" refer to a certain feature, structure or characteristic related to at least one embodiment of this specification. Therefore, it should be emphasized and noted that "one embodiment" or "an embodiment" or "an alternative embodiment" mentioned twice or more in different positions in this specification does not necessarily refer to the same embodiment. In addition, certain features, structures or characteristics in one or more embodiments of this specification can be appropriately combined.

[0090] In some embodiments, numbers describing the number of components and attributes are used. It should be understood that such numbers used in the description of the embodiments are modified by the modifiers "about", "approximately" or "substantially" in some examples. Unless otherwise specified, "about", "approximately" or "substantially" indicate that the numbers are allowed to vary by ±20%. Accordingly, in some embodiments, the numerical parameters used in the specification and claims are approximate values, which may change according to the required features of individual embodiments. In some embodiments, the numerical parameters should take into account the specified significant digits and adopt the general method of retaining digits. Although the numerical domains and parameters used to confirm the breadth of their range in some embodiments of this specification are approximate values, in specific embodiments, the setting of such numerical values ​​is as accurate as possible within the feasible range.

[0091] Finally, it should be understood that the embodiments described in this specification are only used to illustrate the principles of the embodiments of this specification. Other variations may also fall within the scope of this specification. Therefore, as an example and not a limitation, alternative configurations of the embodiments of this specification may be considered consistent with the teachings of this specification. Accordingly, the embodiments of this specification are not limited to the embodiments explicitly introduced and described in this specification.

Claims

1. A method for preparing a spice, characterized in that: The following steps are involved: a. enzymolyze the fenugreek extract to obtain a fenugreek extract enzymolyzate; b. subjecting the fenugreek extract hydrolyzate to a Maillard reaction with amino acids to obtain a Maillard reaction product; c. Filter the Maillard reaction product, collect the filtrate, evaporate the solvent under reduced pressure, and dissolve it in propylene glycol solution to obtain the fragrance.

2. The preparation method according to claim 1, characterized in that The step a includes the following features: The enzymatic hydrolysis step uses biological enzymes for enzymatic hydrolysis. Preferably, the biological enzyme is a mixture of amylase, pectinase and galactomannanase. More preferably, the mass ratio of the amylase, pectinase and galactomannanase is (0.5-3): (0.5-3): (0.5-3). Further preferably, the mass ratio of the amylase, pectinase and galactomannanase is 1:1:

1. And / or, the mass ratio of the fenugreek extract to the biological enzyme is (80-120):(0.5-3), preferably, the mass ratio of the fenugreek extract to the biological enzyme is 100:1.5; and / or, before enzymolysis, diluting the fenugreek extract with distilled water and sterilizing by high pressure, preferably, the mass volume ratio of the fenugreek extract to the distilled water is 10% to 30% (g / mL), more preferably, the mass volume ratio of the fenugreek extract to the distilled water is 20% (g / mL); And / or, after enzymolysis, the mixture of fenugreek extract, distilled water and biological enzyme is heated at 80-100° C. for 15-45 min, and then cooled to 25-45° C. Preferably, after enzymolysis, the mixture of fenugreek extract, distilled water and biological enzyme is heated at 100° C. for 35 min, and then cooled to 35° C.

3. The preparation method according to claim 1, characterized in that: The enzymatic hydrolysis conditions are 40-60° C. for 4-6 hours, preferably, the enzymatic hydrolysis conditions are 50° C. for 5 hours.

4. The preparation method according to claim 1, characterized in that: The step b includes the following features: Before the Maillard reaction, the fenugreek extract hydrolyzate is mixed with a diluent. Preferably, the mass ratio of the fenugreek extract hydrolyzate to the diluent is (8-12):(3-7), and more preferably, the mass ratio of the fenugreek extract hydrolyzate to the diluent is 2:

1. And / or, the mass ratio of the fenugreek extract hydrolysate to the amino acid is: (16-24): (0.1-2), preferably, the mass ratio of the fenugreek extract hydrolysate to the amino acid is 20:1; And / or, the amino acids include phenylalanine, threonine, leucine and tryptophan, preferably, the mass ratio of phenylalanine, threonine, leucine and tryptophan is (0.6-3): (0.2-1): (0.1-0.5): (0.1-0.5), More preferably, the mass ratio of phenylalanine, threonine, leucine and tryptophan is 3:1:0.5:0.5; And / or, before the Maillard reaction, a catalyst is further added, preferably, the catalyst is acetic acid, more preferably, 1 to 5 mL of acetic acid is added to every 100 g of fenugreek extract hydrolyzate, and further preferably, 3 mL of acetic acid is added to every 100 g of fenugreek extract hydrolyzate; And / or, the Maillard reaction is carried out under conditions of 80-100° C. reflux reaction for 4-7 hours. Preferably, the Maillard reaction is carried out under conditions of 90° C. reflux reaction for 5 hours.

5. The preparation method according to claim 4, characterized in that: The diluent is a mixture of water and anhydrous ethanol. Preferably, the mass ratio of water to anhydrous ethanol is (1-3):(2-5), and more preferably, the mass ratio of water to anhydrous ethanol is 2:

3.

6. The preparation method according to claim 1, characterized in that: The step c includes the following features: Before filtering, the Maillard reaction product was cooled to room temperature; And / or, the conditions for distilling off the solvent under reduced pressure are 30-50°C and 40-60Pa. Preferably, the conditions for distilling off the solvent under reduced pressure are 40°C and 50Pa.

7. The preparation method according to claim 1, characterized in that: The propylene glycol solution is an aqueous solution of propylene glycol. Preferably, the concentration of the propylene glycol solution is 20-40%, and more preferably, the concentration of the propylene glycol solution is 30%.

8. The fragrance prepared by the preparation method according to any one of claims 1 to 7.

9. Use of the flavor according to claim 8 in tobacco products.

10. The use according to claim 9, characterized in that The tobacco product comprises at least one of cigarettes, cigars, shredded tobacco, redried tobacco leaves or tobacco leaves.

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