Method for preparing tobacco Maillard reaction flavor by using Nanguo pear residue enzymatic hydrolysate as raw material

Abstract

The invention belongs to the technical field of spices, and provides a method for preparing a Maillard reaction spice for cigarettes by taking Nanguo pear residue enzymatic hydrolysate as a raw material. The Maillard reaction flavor for the cigarettes is prepared by the following steps: performing enzymolysis on Nanguo pear pomace through pectinase to obtain enzymatic hydrolysate, adding amino acid, and reacting to obtain the Maillard reaction flavor. The method specifically comprises the following steps: mixing Nanguo pear residues with water according to a certain solid-to-liquid ratio, adjusting the pH value, adding 1-2% of pectinase, putting the mixture into a constant-temperature incubator for enzymolysis, and performing suction filtration on a solid-liquid mixture after enzymolysis to obtain pear residue enzymatic hydrolysate; finally, amino acid is added for reaction, and the Maillard reaction flavor for the cigarettes is obtained. The prepared Maillard reactant not only has the roasted sweet aroma of the amino acid Maillard reactant, but also has the specific fruity aroma of Nanguo pears, is well harmonized with the tobacco aroma, can increase the thick smoke concentration and improve the aroma quality, can greatly reduce the offensive odor and irritation of smoke, increases the sweet feeling, and has a good application prospect. The cigarette is endowed with specific style characteristics.

Description

Technical Field

[0001] The present invention relates to a method for preparing a tobacco flavor using fermentation technology, specifically a method for preparing a Maillard reaction flavor for tobacco using the enzymolysis solution of Nanguo pear pomace, belonging to the technical field of flavors. Background Art

[0002] Nanguo pear is a special local fruit in the southern Liaoning region of Liaoning Province, China. The main producing areas are Anshan City and Haicheng City. It is known as the "king of pears" and is a rare and precious pear variety. The fruit of Nanguo pear is relatively large, generally pear-shaped or round, with a smooth peel, yellow or golden yellow. The pulp is white or yellow, with a delicate texture and sufficient juice. There are no protrusions on the peel, and it feels smooth when touched. The pulp of Nanguo pear is delicate, with sufficient juice and a sweet taste. Nanguo pear contains rich trace elements, including zinc, iron, potassium, calcium, etc., as well as crude protein, crude fiber, crude fat, lysine, soluble sugar, etc., and the contents are all higher than those of other fruits. When Nanguo pear is ripe, its pulp will naturally ferment and emit a strong wine fragrance. This is a unique feature of Nanguo pear and has not been found in other fruits.

[0003] The Nanguo pear pomace not only retains the unique aroma components of Nanguo pear but also contains a large amount of soluble polysaccharides and pectin. If it is discarded as waste and deteriorates rapidly in a short time, it will ultimately cause environmental pollution and waste of resources.

[0004] Using pectinase to further enzymolyze Nanguo pear pomace, pectinase acts on pectin molecules in various ways to change its structure and properties. Pectinase converts the large pectin molecules in Nanguo pear into a large number of small molecule substances such as soluble sugars and galacturonic acid, and due to its enzymolysis, it destroys the cell structure and releases more aroma components in the Nanguo pear pulp cells.

[0005] Most of the preparations of Maillard reactants for tobacco mainly involve a series of complex reactions of raw materials such as sugars and amino acids at room temperature or when heated. These reactions ultimately produce brown or even brownish-black macromolecular substances, and Maillard reaction is used to generate compounds with specific flavors, and these compounds can be used to improve the aroma and taste of tobacco products. However, such reaction raw materials are likely to result in the aroma style characteristics of the reactants not being obvious enough, the richness and harmony of the tobacco aroma being slightly insufficient, and bringing a certain degree of irritation and dryness, and the effect in cigarette flavoring is relatively single and not prominent enough. Instead, using the self-sugar source after enzymolysis of Nanguo pear pomace as the raw material and adding a certain amount of amino acids to obtain the Maillard reactant. Summary of the Invention

[0006] The present invention overcomes the deficiencies existing in the above-mentioned preparation technology and provides a method for preparing Maillard reactants for tobacco use from the enzymatic hydrolysate of Nanguo pear pomace. This method is a new way for the optimized utilization of Nanguo pear pomace resources and provides greater economic value for the comprehensive utilization of Nanguo pears. The reactants prepared from the enzymatic hydrolysate of Nanguo pear pomace have obvious aroma characteristics. In addition to the roasted sweet aroma, they also have the unique fruity aroma of Nanguo pears, and are well coordinated with the tobacco aroma. They can increase the thickness and fullness of the smoke concentration, improve the quality of the aroma, greatly reduce the miscellaneous odor and irritation of the smoke, increase the sweet and mellow feeling, and endow the cigarette with unique style characteristics.

[0007] The technical solution provided by the present invention: The method for preparing Maillard reaction spices for tobacco use from the enzymatic hydrolysate of Nanguo pear pomace includes the following steps:

[0008] 1) Pretreatment: Dry and crush the Nanguo pear pomace, mix it with water, and adjust the pH to acidic.

[0009] 2) Enzymatic hydrolysis: Add pectinase to the mixed solution obtained in step 1) for enzymatic hydrolysis.

[0010] 3) Preparation of Maillard reactants: After filtering the enzymatic hydrolysate by suction, add amino acids and adjust the pH value, and carry out a thermal reflux reaction to obtain Maillard reaction spices from the enzymatic hydrolysate of Nanguo pear pomace.

[0011] In the above method for preparing Maillard reaction spices for tobacco use from the enzymatic hydrolysate of Nanguo pear pomace, in step 1), the material-liquid ratio of Nanguo pear pomace to water is 1:(10 - 15).

[0012] In the above method for preparing Maillard reaction spices for tobacco use from the enzymatic hydrolysate of Nanguo pear pomace, in step 1), the adjustment of pH to acidic is carried out by using glacial acetic acid or citric acid to adjust the pH to 4.0 - 5.0 and stirring evenly.

[0013] In the above method for preparing Maillard reaction spices for tobacco use from the enzymatic hydrolysate of Nanguo pear pomace, in step 2), the pectinase is pectinase E038, the addition amount is 0.5% - 1% of the weight of Nanguo pear pomace, and the enzyme activity is 15000u / g.

[0014] In the above method for preparing Maillard reaction spices for tobacco use from the enzymatic hydrolysate of Nanguo pear pomace, in step 2), the enzymatic hydrolysis temperature is 45 - 55°C, the rotation speed is 100 - 150rpm, and the enzymatic hydrolysis time is 20 - 24 hours.

[0015] In the above method for preparing Maillard reaction spices for tobacco use from the enzymatic hydrolysate of Nanguo pear pomace, in step 3), the amino acids are phenylalanine, alanine or proline, and the addition amount of amino acids is 0 - 3% of the weight of the enzymatic hydrolysate of Nanguo pear pomace.

[0016] In the above method for preparing a Maillard reaction flavor for cigarettes using the enzymatic hydrolysate of Nanguo pear pomace, in step 3), the pH value is adjusted to 2 - 11 with potassium hydroxide or sodium hydroxide.

[0017] In the above method for preparing a Maillard reaction flavor for cigarettes using the enzymatic hydrolysate of Nanguo pear pomace, in step 3), the reflux temperature of the thermal reflux reaction is 40 - 130 °C, and the reflux reaction is carried out for 1 - 7 hours.

[0018] Application of the Maillard reaction flavor of the enzymatic hydrolysate of Nanguo pear pomace obtained by the above method in cigarettes.

[0019] In the above application, the addition ratio of the Maillard reaction flavor of the enzymatic hydrolysate of Nanguo pear pomace in cigarettes is 0.01% - 0.05%.

[0020] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0021] The present invention provides a new method for preparing Maillard reactants using the enzymatic hydrolysate of Nanguo pear pomace. By enzymatically hydrolyzing and recycling the endogenous sugars and aroma components in Nanguo pear pomace and carrying out Maillard reaction with exogenous amino acids, the waste resources of Nanguo pear pomace are utilized. The prepared Maillard reactants have obvious Nanguo pear aroma characteristics, with caramel-like sweet and baking aromas. When used in cigarettes, they have good harmony with the cigarette aroma, can increase the smoke concentration, improve the aroma quality, enhance the taste, and make the aftertaste comfortable. Detailed implementation manners

[0022] Example 1

[0023] Weigh 10 grams of Nanguo pear pomace, mix the Nanguo pear pomace raw material with water at a material-liquid ratio of 1:10, adjust the pH to 4.8 with 1 mol / L glacial acetic acid and stir evenly. Transfer the pretreated fruit residue mixture to a conical flask, add pectinase accounting for 1% of the weight of the Nanguo pear pomace, place it in a constant temperature incubator, with an enzymatic hydrolysis temperature of 50 °C, a rotation speed of 100 - 150 rpm, and an enzymatic hydrolysis time of 24 hours. After enzymatic hydrolysis, filter the enzymatic hydrolysate by suction, collect the filtrate to obtain the Nanguo pear extract, add 2.7 grams of phenylalanine based on the weight of the enzymatic hydrolysate of Nanguo pear pomace and adjust the pH to 8 with potassium hydroxide to obtain the enzymatic hydrolysis reaction solution of Nanguo pear pomace. Carry out thermal reflux on the enzymatic hydrolysis reaction solution of Nanguo pear pomace, with a reflux temperature of 120 °C and a reflux reaction for 2.5 hours. After the reaction ends, immediately stop heating, and collect the material liquid, which is the Maillard reaction flavor of the enzymatic hydrolysate of Nanguo pear pomace prepared.

[0024] The molar ratio of the added amino acid mass to the total sugar content of Nanguo pear pomace is 1:1.

[0025] Example 2

[0026] Weigh 10 grams of Nanguo pear pomace. Mix the Nanguo pear pomace raw material with water at a solid-liquid ratio of 1:10. Adjust the pH to 4.8 with 1 mol / L glacial acetic acid and stir evenly. Transfer the pretreated pomace mixture to a conical flask, add pectinase accounting for 1% of the weight of the Nanguo pear pomace, place it in a constant temperature incubator, with the enzymolysis temperature at 50 °C, the rotation speed at 100 - 150 rpm, and the enzymolysis time for 24 hours. After enzymolysis, filter the enzymolysis solution by suction, collect the filtrate to obtain the Nanguo pear extract, add 2.16 grams of alanine based on the weight of the Nanguo pear pomace enzymolysis solution and adjust the pH to 8 with potassium hydroxide to obtain the Nanguo pear pomace enzymolysis reaction solution. Conduct a thermal reflux on the Nanguo pear pomace enzymolysis reaction solution, with the reflux temperature at 120 °C and the reflux reaction for 2.5 hours. After the reaction ends, immediately stop heating, and collect the liquid material, which is the prepared Maillard reaction flavor of phenylalanine from the Nanguo pear pomace enzymolysis solution.

[0027] The molar ratio of the added amino acid mass to the total sugar content of the Nanguo pear pomace is 1:1.

[0028] Example 3

[0029] Weigh 10 grams of Nanguo pear pomace. Mix the Nanguo pear pomace raw material with water at a solid-liquid ratio of 1:10. Adjust the pH to 4.8 with 1 mol / L glacial acetic acid and stir evenly. Transfer the pretreated pomace mixture to a conical flask, add pectinase accounting for 1% of the weight of the Nanguo pear pomace, place it in a constant temperature incubator, with the enzymolysis temperature at 50 °C, the rotation speed at 100 - 150 rpm, and the enzymolysis time for 24 hours. After enzymolysis, filter the enzymolysis solution by suction, collect the filtrate to obtain the Nanguo pear extract, add 1.5 grams of proline based on the weight of the Nanguo pear pomace enzymolysis solution and adjust the pH to 8.5 with potassium hydroxide to obtain the Nanguo pear pomace enzymolysis reaction solution. Conduct a thermal reflux on the Nanguo pear pomace enzymolysis reaction solution, with the reflux temperature at 120 °C and the reflux reaction for 2 hours. After the reaction ends, immediately stop heating, and collect the liquid material, which is the prepared Maillard reaction flavor of proline from the Nanguo pear pomace enzymolysis solution.

[0030] The molar ratio of the added amino acid mass to the total sugar content of the Nanguo pear pomace is 1:1.

[0031] Detection of total sugar and reducing sugar in the Maillard reaction flavor of the Nanguo pear pomace enzymolysis solution in Example 4

[0032] Perform the detection of total sugar and reducing sugar on the Nanguo pear extract obtained in Example 1 and the Nanguo pear extract without adding pectinase.

[0033] Test method:

[0034] I. Determination methods for total sugar and reducing sugar: Refer to the industry standard YC / T 159 - 2002, and use the continuous flow method to analyze and quantitatively detect total sugar and reducing sugar. The determination method is as follows:

[0035] (1) Draw the annotation curve: Weigh 10.0 g of D-glucose into a beaker, accurate to 0.0001 g. Dissolve it with 5% acetic acid solution and transfer it into a 1 L volumetric flask. Dilute it to the mark with 5% acetic acid solution to obtain the glucose standard stock solution.

[0036] Prepare glucose standard solutions with concentrations of 0.3, 0.6, 1.2, 1.8, 2.4, and 3.0 (mg / mL).

[0037] (2) Sample determination: Dilute the sample to be measured by an appropriate multiple and then perform the same operations as in the above steps for determination. The calculation formula is as follows:

[0038] Calculation of water-soluble sugar

[0039] The content of water-soluble sugar calculated on a dry basis, calculated as glucose, is obtained from Equation (1):

[0040]

[0041] In the formula:

[0042] c—the instrumental observed value of the total (reducing) sugar in the sample solution, unit: milligram per milliliter (mg / mL); V—the volume of the extraction solution, unit: milliliter (mL); m—the mass of the test sample, unit: milligram (mg); W—the moisture content of the test sample.

[0043] Table 1 Reducing sugar and total sugar contents of the extraction solution of Nanguo pears with 1% pectinase added and without enzyme added (blank)

[0044]

[0045] It can be seen from Table 1 that after enzymatic hydrolysis with 1% pectinase solution, pectin and polysaccharides will be decomposed, releasing more sugars, resulting in a significant increase in the amount of reducing sugar and total sugar in the enzymatic hydrolysis solution. The addition of pectinase is beneficial to the improvement of the flavor of the spice in the subsequent work.

[0046] Example 5 Analysis of the aroma of the Maillard reaction spice prepared from the enzymatic hydrolysis solution of Nanguo pear pomace

[0047] Analyze the Maillard reaction spice prepared from the enzymatic hydrolysis solution of Nanguo pear pomace by HS-SPME-GCMS method

[0048] Weigh 1 g of the reaction flavor in Example 1 into a 20 mL headspace vial and inject it directly without dilution.

[0049] Instrument: Use the Gerstel MPS multi-functional pretreatment platform and Agilent gas chromatograph-mass spectrometer

[0050] 1. HS-SPME conditions:

[0051] Solid-phase microextraction head: Supelco 50 / 30μm, shaking speed: 250 r / min; DVB / CAR / PDMS; desorption time: 5 min;

[0052] Extraction temperature: 80 °C;

[0053] Extraction head aging temperature: 270 °C;

[0054] Preheating and equilibration time: 5 min;

[0055] Extraction head aging time: 20 min;

[0056] Extraction time: 30 min;

[0057] Extraction head aging purge gas: nitrogen;

[0058] GC / MS conditions

[0059] 2. Chromatographic conditions:

[0060] Chromatographic column: DB-5MS (60 m × 0.25 mm i.d. × 0.25 μm d.f.)

[0061] Injector: temperature 250 °C, split ratio 15:1, injection volume 1 μL

[0062] Column flow rate: helium, constant flow mode, 1 mL / min

[0063] Programmed temperature rise:

[0064] Transfer line temperature: 280 °C

[0065] 3. Mass spectrometry conditions:

[0066] Ion source (EI) temperature: 230 °C; ionization voltage: 70 eV; solvent delay: 4.8 min; scan range: 33 - 400.

[0067] Table 2 Analysis of Aroma Components of Maillard Reaction Products of Phenylalanine in Nanguo Pear Enzymolysis Solution

[0068]

[0069]

[0070] Example 6 Aroma Analysis of Maillard Reaction Flavors for Cigarette Use Prepared from Nanguo Pear Pomace Enzymolysis Solution

[0071] According to the method described in Example 5, weigh 1 g of the reaction essence in Example 2 into a 20 mL headspace vial and inject it directly without dilution.

[0072] Table 3 Analysis of Aroma Components of Maillard Reaction Products of Alanine in Nanguo Pear Enzymolysis Solution

[0073]

[0074]

[0075] Example 7 Aroma Analysis of Maillard Reaction Flavor for Cigarette Prepared from Enzymatic Hydrolysate of Nanguo Pear Pomace

[0076] Weigh 1 g of the reaction flavor in Example 3 into a 20 mL headspace vial according to the method described in Example 5, and inject the sample directly without dilution.

[0077] Table 4 Aroma Component Analysis of Proline Maillard Reaction Products from Enzymatic Hydrolysate of Nanguo Pear

[0078]

[0079]

[0080] Example 8 Sensory Evaluation Results of Maillard Reaction Flavors from Nanguo Pear Pomace

[0081] Sensory evaluation was carried out on three Maillard reaction flavors prepared from enzymatic hydrolysates of Nanguo pear pomace. The results are shown in Table 5. The scores of the three Maillard reaction flavors are all better than those of the blank cigarette, indicating that the addition of the three reaction flavors has a positive improvement on the sensory results of the cigarette. Moreover, each reaction flavor not only has the characteristic aroma of Nanguo pear, but also has the characteristics of Maillard reaction products, which can combine the aromas. When smoking, the overall performance is better and there will be no aroma stratification. At the same time, it also has the effects of enhancing aroma, improving the smoke, enriching the smoke aroma, increasing the richness of the smoke and removing the off-odors, weakening the scorched roasting feeling of the smoke, and retaining the fruit aroma to a greater extent.

[0082] When using different exogenous amino acids, according to the structural characteristics and optimal reaction conditions of different amino acids, the Maillard reaction products prepared have different effects and flavor characteristics, as shown in Table 5.

[0083] The Maillard reaction product prepared with phenylalanine as the exogenous amino acid was added to the blank cigarette for smoking evaluation. In addition to the obvious characteristic fruit aroma of Nanguo pear, it was found that this product could significantly increase the smoke concentration, make the smoke soft and delicate, cover up the off-odors, and significantly improve the tobacco quality.

[0084] The Maillard reaction product prepared with proline as the exogenous amino acid was added to the blank cigarette for smoking evaluation. The obtained product showed strong fruit aroma and caramel-like sweet aroma. When this product was added to the blank cigarette for smoking evaluation, it was found that this product could significantly improve the taste, with a comfortable aftertaste and mild smoke.

[0085] The Maillard reaction product prepared with alanine as the exogenous amino acid was added to the blank cigarette for sensory evaluation. The product exhibited a rich burnt-sweet roasted fragrance. When this product was added to the blank cigarette for sensory evaluation, it was found that the product could significantly enhance the roasted-sweet fragrance of the cigarette, make the smoke more volatilized, giving a very brisk feeling, and significantly improve the quality of the cigarette.

[0086] Table 5 Sensory evaluation results of Maillard reaction flavor from enzymatic hydrolysate of Nanguo pear pomace

[0087]

[0088] Note: 0.5 point is the scoring unit.

Claims

1. A method for preparing Maillard reaction flavoring for tobacco using Nanguo pear residue enzymatic hydrolyzate as raw material, characterized in that: The steps include: 1) Pretreatment: drying and crushing the pear residue, mixing it with water, and adjusting the pH to acidic; 2) Enzymatic hydrolysis: adding pectinase to the mixed solution obtained in step 1) for enzymatic hydrolysis; 3) Preparation of Maillard reaction product: After the enzymatic hydrolyzate is filtered, amino acids are added and the pH value is adjusted, and a heat reflux reaction is performed to obtain the Nanguo pear residue enzymatic hydrolyzate Maillard reaction flavor.

2. The method for preparing Maillard reaction flavoring for tobacco using Nanguo pear residue enzymatic hydrolyzate as raw material according to claim 1, characterized in that: In step 1), the material-liquid ratio of Nanguo pear residue to water is 1:10-15.

3. The method for preparing Maillard reaction flavoring for tobacco using Nanguo pear residue enzymatic hydrolyzate as raw material according to claim 1, characterized in that: In step 1), the pH is adjusted to acidic by using glacial acetic acid or citric acid to adjust the pH to 4.0-5.0 and stirring evenly.

4. The method for preparing Maillard reaction flavoring for tobacco using Nanguo pear residue enzymatic hydrolyzate as raw material according to claim 1, characterized in that: In step 2), the pectinase is pectinase E038, the added amount is 0.5%-1% of the weight of Nanguo pear residue, and the enzyme activity is 15000u / g.

5. The method for preparing Maillard reaction flavoring for tobacco using Nanguo pear residue enzymatic hydrolyzate as raw material according to claim 1, characterized in that: In step 2), the enzymolysis temperature is 45-55° C., the rotation speed is 100-150 rpm, and the enzymolysis time is 20-24 hours.

6. The method for preparing Maillard reaction flavoring for tobacco using Nanguo pear residue enzymatic hydrolyzate as raw material according to claim 1, characterized in that: In step 3), the amino acid is phenylalanine, alanine or proline, and the amount of the amino acid added is 0-3% by weight of the Nanguo pear residue enzymatic hydrolyzate.

7. The method for preparing Maillard reaction flavoring for tobacco using Nanguo pear residue enzymatic hydrolyzate as raw material according to claim 1, characterized in that: In step 3), the pH value is adjusted to 2-11 using potassium hydroxide or sodium hydroxide.

8. The method for preparing Maillard reaction flavoring for tobacco using Nanguo pear residue enzymatic hydrolyzate as raw material according to claim 1, characterized in that: In step 3), the reflux temperature of the thermal reflux reaction is 40-130° C., and the reflux reaction is performed for 1-7 hours.

9. Use of the Maillard reaction flavoring of Nanguo pear residue enzymatic hydrolyzate according to the method of any one of claims 1 to 8 in cigarettes.

10. The use according to claim 9, characterized in that: The Maillard reaction flavoring of Nanguo pear residue enzymatic hydrolyzate is added in a proportion of 0.01-0.05% in cigarettes.

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