Method for preparing Maillard reactant of mint polysaccharide by utilizing microwaves and application of Maillard reactant
The preparation of peppermint polysaccharide Maillard reactants through microwave heating technology solves the problem of reducing the aroma of cigarettes, improves the aroma richness and taste comfort, and enhances the sensory quality of cigarettes.
Patent Information
- Application Number
- CN202411628379.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-14
- Publication Date
- 2024-12-24
AI Technical Summary
While cigarettes reduce the amount of tar, the aroma and concentration are greatly reduced, affecting the comfort and satisfaction of smoking. Traditional heating methods lead to the loss and destruction of heat-sensitive or volatile aroma substances.
The mint polysaccharide Maillard reactant is prepared by microwave heating technology. By optimizing extraction and reaction conditions, it improves the aroma richness and taste comfort, retains aroma substances, and enhances antioxidant activity.
It shortens the reaction time, enriches the aroma, covers up miscellaneous air, increases the sweetness of smoke, reduces the dryness and irritation of the mouth, and improves the sensory quality of the cigarette.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of tobacco flavors, and particularly relates to a method for preparing mint polysaccharide Maillard reactants by utilizing microwaves and an application thereof. Background Art
[0002] With the rise of the global tobacco control wave and the increasing attention of cigarette consumers to their own health, reducing tar in cigarettes has become a consensus in the tobacco industry around the world. However, while the tar content of cigarettes is reduced, the aroma volume and concentration of cigarettes are greatly reduced, which directly affects the comfort and satisfaction of smoking cigarettes. Adding flavors to cigarettes can enhance the flavor of cigarettes, increase smoke concentration, improve the taste, remove impurities, and reduce irritation. At the same time, flavors can give characteristic aromas and highlight the personalized style of cigarette products.
[0003] The Maillard reaction, also known as the non-enzymatic browning reaction, is a polymerization and condensation reaction between carbonyl compounds (such as reducing sugars) and amino compounds (such as amino acids, amines, polypeptides, etc.) at room temperature or when heated, producing a series of substances with special aromas, which are widely used in food baking, meat processing, flavor production and other fields. Since the Maillard reaction products contain a large number of aromatic substances, and most of them are coordinated with the aroma of tobacco, they can effectively improve the sensory quality of cigarettes, cover up the miscellaneous smell, and increase the flavor of cigarettes, thus becoming a good type of tobacco flavoring.
[0004] Mint, a perennial herbaceous plant of the Lamiaceae family, has both edible and medicinal functions and can be used as a flavoring agent, spice, and wine pairing. Mint water extract has a relatively significant antioxidant activity and has a relatively high scavenging effect on oxidative free radicals. Mint polysaccharides contain a variety of sugars such as glucose, galactose, mannose, and glucuronic acid. Choosing it as the source of carbonyl compounds for the Maillard reaction can enrich the aroma type and give cigarettes a unique aroma.
[0005] Traditional heating methods have disadvantages such as slow heating, uneven heating, and open reaction, which can easily cause the loss and destruction of heat-sensitive or volatile aroma substances. Microwave heating, as a new type of efficient, energy-saving, and environmentally friendly heating method, heats quickly and evenly; has strong penetration ability and fast penetration speed; is selective, has good absorption of polar substances, and cannot absorb non-polar substances, which can better preserve the quality and flavor of the raw materials. In addition, the early reaction degree of the Maillard reaction under microwave heating is higher, the mid-term product composition is different, the aroma substances are richer, and the antioxidant and other physiological activities of the late compounds are significantly enhanced. Summary of the invention
[0006] The object of the present invention is to provide a method for preparing a mint polysaccharide Maillard reactant using microwaves and its application. The reactant prepared by the method has a greatly shortened preparation time, a richer and fuller aroma, a comfortable taste, and a good application effect in cigarettes. The natural extract is rich in various sugars, and different aroma substances can be produced through the Maillard complex reaction under microwaves, thereby promoting the comprehensive development and efficient utilization of various natural extracts to solve the problems existing in the above-mentioned background technology.
[0007] To achieve the above objectives, this application is implemented through the following technical solutions:
[0008] A method for preparing mint polysaccharide Maillard reactant using microwaves, comprising the following steps:
[0009] S1. Extraction of peppermint polysaccharides:
[0010] The dried mint raw material is weighed, crushed and sieved. After the first round of extraction, a set amount of solvent is used for soaking, and then the precipitate is collected for a set time and a set number of extractions. The second round of extraction adopts L9 orthogonal experimental design, with extraction temperature, extraction time and solid-liquid ratio as the three factors for investigation and extraction for a set number of times, and mint polysaccharides are obtained after post-treatment. In this application, the mint polysaccharide yield is used as the screening index, and the optimal process conditions for mint polysaccharide extraction are determined according to the orthogonal test intuitive analysis and variance analysis results (Table 1 and Table 2).
[0011] S2. Microwave preparation of Maillard products of mint polysaccharides:
[0012] The mint polysaccharide prepared in step S1 is mixed with amino acids in a solvent according to a set molar ratio, the pH of the system is adjusted, microwave heating is used at a set temperature, the reaction is performed for a set time, and a mint polysaccharide Maillard reaction product is obtained after post-treatment.
[0013] Furthermore, in step S1, the set amount of solvent in the first round of extraction is 95% ethanol by volume, which is 5-10 times the volume of the mint powder; the heating reflux time is 30-60 minutes each time, and the set number of times is 2-4 times.
[0014] Furthermore, in step S1, in the second round of extraction, the extraction temperature is 60-100°C, the extraction time is 0.5-2.5h, the solid-liquid ratio refers to the ratio of precipitate to water is 1:5-1:25; the number of extractions is 2-4 times.
[0015] Furthermore, the solid-liquid ratio was 1:25, and the extraction was performed twice at 100°C, each time for 1 h.
[0016] Furthermore, in step S1, the post-treatment in the first round of extraction refers to taking the precipitate after filtration to evaporate the ethanol; the post-treatment in the second round of extraction refers to filtering and combining the extracts, concentrating under reduced pressure, adding 4 times the amount of anhydrous ethanol, and then standing for 24 hours, filtering, washing with anhydrous ethanol, and vacuum drying at 60°C.
[0017] Furthermore, in step S2, the amino acids are one or more combinations of glycine, alanine, cysteine, proline, lysine, serine, arginine, aspartic acid, glutamic acid, phenylalanine, histidine, and threonine.
[0018] Furthermore, in step S2, the molar ratio is 1:3-3:1, the solvent is water or methanol, the pH is 6.0-9.0, the set temperature is 130-150°C, and the reaction time is 10-30 min.
[0019] Furthermore, in the microwave preparation of the mint polysaccharide Maillard product, the post-treatment is cooling to room temperature, filtering, discarding insoluble matter, and taking the upper liquid.
[0020] An application, the mint polysaccharide Maillard reaction product prepared by any one of the above methods is used as a tobacco flavoring.
[0021] Furthermore, the mint polysaccharide Maillard reactant is added at 0.0001%-2% by weight of the tobacco.
[0022] Furthermore, the tobacco is sprayed or injected in the form of adding surface aroma, adding flavor or adding flake aroma.
[0023] In the present application, tobacco includes cigarettes, new tobacco, cigars, and pipe tobacco. The sensory quality of tobacco with added flavors is evaluated, and the evaluation results are shown in Table 3.
[0024] The beneficial effects of the present invention are:
[0025] The present invention studies the extraction process of mint polysaccharide, and shows that the factors affecting the yield of mint polysaccharide are extraction temperature>solid-liquid ratio>extraction time. It is determined that the optimal extraction process is to add 25 times of water, extract twice at 100°C, and extract for 1 hour each time. Under this condition, the yield of mint polysaccharide is (8.85±0.57)%. The mint polysaccharide Maillard reactant prepared by the present invention has the effects of enriching aroma, covering impurities, increasing the characteristic aroma of mint, increasing the sweetness of smoke, reducing oral dryness and irritation, etc. when acting on cigarettes. DETAILED DESCRIPTION
[0026] The technical solution of the present invention is described in detail below through examples. The following examples are merely exemplary and can only be used to explain and illustrate the technical solution of the present invention, but cannot be construed as limiting the technical solution of the present invention.
[0027] Preparation Example 1
[0028] Weigh the dried mint raw material and grind it through a 30-mesh sieve to obtain mint powder. Use 95% by volume ethanol and a volume ratio of mint powder to ethanol of 1:10, then heat and reflux at 60°C for extraction. Each extraction time is 60 minutes, and the extraction is repeated 3 times. Then, the precipitate is separated by suction filtration and the ethanol is evaporated. The precipitate is extracted twice, and 25 times the amount of water is used to extract at 100°C for 1 hour each time. The filtrate obtained is combined with the filtrate of the first extraction and concentrated under reduced pressure. Then, 4 times the amount of anhydrous ethanol is added and allowed to stand for 24 hours, then filtered, washed with anhydrous ethanol, and vacuum dried at 60°C to obtain mint polysaccharide P1.
[0029] Preparation Example 2
[0030] Weigh the dried mint raw material and grind it through a 30-mesh sieve to obtain mint powder. Use 95% by volume ethanol and a volume ratio of mint powder to ethanol of 1:5, then heat and reflux at 60°C for extraction. Each extraction time is 60 minutes, and the extraction is repeated 3 times. Then, the precipitate is separated by filtration and the ethanol is evaporated. The precipitate is extracted twice, using 20 times the amount of water to extract twice at 100°C for 1 hour each time. The filtrate obtained is combined with the filtrate of the first extraction and concentrated under reduced pressure. Then, 4 times the amount of anhydrous ethanol is added and allowed to stand for 24 hours, then filtered, washed with anhydrous ethanol, and vacuum dried at 60°C to obtain mint polysaccharide P2.
[0031] Preparation Example 3
[0032] Weigh the dried mint raw material and grind it through a 50-mesh sieve to obtain mint powder. Use 95% by volume ethanol and a volume ratio of mint powder to ethanol of 1:8, then heat and reflux at 60°C for extraction. Each extraction time is 60 minutes, and the extraction is repeated 3 times. Then, the precipitate is separated by filtration and the ethanol is evaporated. The precipitate is extracted twice, using 10 times the amount of water to extract twice at 100°C for 1 hour each time. The filtrate obtained is combined with the filtrate of the first extraction and concentrated under reduced pressure. Then, 4 times the amount of anhydrous ethanol is added and allowed to stand for 24 hours, then filtered, washed with anhydrous ethanol, and vacuum dried at 60°C to obtain mint polysaccharide P3.
[0033] Preparation Example 4
[0034] Weigh the dried mint raw material and grind it through a 20-mesh sieve to obtain mint powder. Use 95% by volume ethanol and a volume ratio of mint powder to ethanol of 1:10, then heat and reflux at 60°C for extraction. Each extraction time is 60 minutes, and the extraction is repeated 3 times. Then, the precipitate is separated by suction filtration and the ethanol is evaporated. The precipitate is extracted twice, and 18 times the amount of water is used to extract it at 100°C twice, each time for 1 hour. The filtrate obtained is combined with the filtrate of the first extraction and concentrated under reduced pressure. Then, 4 times the amount of anhydrous ethanol is added and allowed to stand for 24 hours, then filtered, washed with anhydrous ethanol, and vacuum dried at 60°C to obtain mint polysaccharide P4.
[0035] After testing the mint polysaccharides prepared in Preparation Examples 1 to 4, it was found that the compositions of the mint polysaccharides in each Preparation Example were the same, and the only difference was the yield. Therefore, in the following examples, those skilled in the art can select the mint polysaccharide produced by any Preparation Example as needed. For this reason, in the following examples, it is not clearly stated which Preparation Example is used to prepare the mint polysaccharide in each Example.
[0036] Example 1
[0037] Accurately weigh 30g of mint polysaccharide extract and 16.5g of phenylalanine, add 150mL of methanol and water mixed solution (v / v=1:1), wait for complete dissolution, adjust pH to 9.0 with NaOH aqueous solution, and heat the reaction at 130℃ for 10min. After the reaction, quickly cool the reaction product to room temperature, filter, discard the insoluble matter, and take the upper liquid to obtain the mint Maillard reaction product. The mint Maillard product is added to the tobacco, and accounts for 40ppm of the weight of the tobacco.
[0038] Example 2
[0039] Accurately weigh 30g of mint polysaccharide extract, 8.3g of phenylalanine and 3.8g of glycine, add 150mL of a mixed solution of methanol and water (v / v=1:1), and wait until it is completely dissolved. Use a NaOH aqueous solution to adjust the pH to 9.0, and microwave heating at 140°C for 20 minutes. After the reaction is completed, the reaction product is quickly cooled to room temperature, filtered, and the insoluble matter is discarded. The upper liquid is taken to obtain the mint Maillard reaction product. The obtained mint Maillard product is added to the tobacco, and accounts for 60ppm of the weight of the tobacco.
[0040] Example 3
[0041] Accurately weigh 30g of mint polysaccharide extract, 8.3g of phenylalanine and 3.8g of glycine, add 150mL of a mixed solution of methanol and water (v / v=1:1), and wait until it is completely dissolved. Use dilute hydrochloric acid to adjust the pH to 6.0, and microwave heating at 150°C for 20 minutes. After the reaction is completed, the reaction product is quickly cooled to room temperature, filtered, and the insoluble matter is discarded. The upper liquid is taken to obtain the mint Maillard reaction product. The obtained mint Maillard product is added to the tobacco, and accounts for 80ppm of the weight of the tobacco.
[0042] Example 4
[0043] Accurately weigh 30g of mint polysaccharide extract, 5.8g of proline and 3.8g of glycine, add 150mL of methanol and water mixed solution (v / v=1:1), and wait until it is completely dissolved. Use dilute hydrochloric acid and NaOH aqueous solution to adjust the pH to 7.5, and microwave heating at 140℃ for 30min. After the reaction is completed, the reaction product is quickly cooled to room temperature, filtered, and the insoluble matter is discarded. The upper liquid is taken to obtain the mint Maillard reaction product. The obtained mint Maillard product is added to the tobacco, and accounts for 100ppm of the weight of the tobacco.
[0044] Table 1. Orthogonal test results
[0045]
[0046] Table 2. ANOVA table
[0047]
[0048] Table 3. Results of the inhalation efficacy test
[0049]
[0050] According to the inhalation effect test, the mint Maillard product prepared by microwave provided by the present invention can significantly enrich the aroma, cover up the impurities, increase the characteristic aroma of mint, increase the sweetness of smoke, reduce the dryness and irritation of the mouth, and have the following effects.
[0051] Although the invention has been described herein with reference to illustrative embodiments thereof, it should be understood that numerous other modifications and implementations can be devised by those skilled in the art that will fall within the scope and spirit of the principles disclosed herein.
Claims
1. A method for preparing mint polysaccharide Maillard reactants using microwaves, characterized in that: Use the following steps: S1. Extraction of peppermint polysaccharides: Weigh the dried mint raw material, crush and sieve it, soak it in a set amount of solvent, heat it under reflux and extract it for a set time and a set number of times in the first round of extraction, collect the precipitate for the second round of extraction, the second round of extraction adopts L9 orthogonal experimental design, with extraction temperature, extraction time and material-liquid ratio as the three factors to be investigated, and extract it for a set number of times, and then obtain mint polysaccharide after post-treatment; S2. Microwave preparation of Maillard products of mint polysaccharides: The mint polysaccharide prepared in step S1 is mixed with amino acids in a solvent according to a set molar ratio, the pH of the system is adjusted, microwave heating is used at a set temperature, the reaction is performed for a set time, and a mint polysaccharide Maillard reaction product is obtained after post-treatment.
2. The method for preparing mint polysaccharide Maillard reactants using microwaves according to claim 1, characterized in that: In step S1, the set amount of solvent in the first round of extraction is 95% ethanol by volume, which is 5-10 times the volume of the mint powder; the heating reflux time is 30-60 minutes each time, and the set number of times is 2-4 times.
3. The method for preparing mint polysaccharide Maillard reactant using microwave according to claim 1, characterized in that: In step S1, in the second round of extraction, the extraction temperature is 60-100°C, the extraction time is 0.5-2.5h, the solid-liquid ratio refers to the ratio of precipitate to water is 1:5-1:25; the number of extractions is 2-4 times.
4. The method for preparing mint polysaccharide Maillard reactants using microwaves according to claim 3, characterized in that: The solid-liquid ratio was 1:25, and the extraction was performed twice at 100°C, each time for 1 hour.
5. The method for preparing mint polysaccharide Maillard reactant using microwave according to claim 1, characterized in that: In step S1, the post-treatment in the first round of extraction refers to taking the precipitate after filtration to evaporate the ethanol; the post-treatment in the second round of extraction refers to filtering and combining the extracts, concentrating under reduced pressure, adding 4 times the amount of anhydrous ethanol, and standing for 24 hours, filtration, washing with anhydrous ethanol, and vacuum drying at 60°C.
6. The method for preparing mint polysaccharide Maillard reactant using microwave according to claim 1, characterized in that: In step S2, the amino acids are one or more combinations of glycine, alanine, cysteine, proline, lysine, serine, arginine, aspartic acid, glutamic acid, phenylalanine, histidine, and threonine.
7. The method for preparing mint polysaccharide Maillard reactant using microwave according to claim 1, characterized in that: In step S2, the molar ratio is 1:3-3:1, the solvent is water or methanol, the pH is 6.0-9.0, the set temperature is 130-150°C, and the reaction time is 10-30min.
8. An application, characterized in that: The mint polysaccharide Maillard reaction product prepared according to any one of claims 1 to 7 is used as a tobacco flavoring.
9. The use according to claim 8, characterized in that: The mint polysaccharide Maillard reactant is added at 0.0001%-2% of the weight of the tobacco.
10. The use according to claim 9, characterized in that: Spray or inject it into tobacco by adding surface flavor, flavoring or flake flavoring.