Method for preparing hawthorn extract by combining high-voltage discharge with fermentation treatment or low-temperature plasma

Abstract

The invention relates to the technical field of tobacco flavor processing, in particular to a method for preparing hawthorn extract by combining high-voltage discharge with fermentation treatment or low-temperature plasma, which overcomes four major pain points of'thin aroma, thermosensitive vulnerability, long flow and high cost 'of the traditional hawthorn extract by one stroke. The aroma richness is remarkably improved, the extraction efficiency is remarkably improved, the resource utilization rate is remarkably improved, and the energy consumption and emission are remarkably reduced; the technology is in a normal-temperature short range, the equipment is universal and easy to amplify, the solvent is recycled and zero-waste, the residue can be used for preparing the fertilizer, the economic, environment-friendly and sensory benefits are taken into account, a reproducible, generalizable and sustainable green manufacturing normal form is provided for the cigarette and food natural perfume industry, and the method has wide industrial application prospects.

Description

Technical Field

[0001] This invention relates to the field of tobacco flavoring processing technology, and more specifically, to a method for preparing hawthorn extract using high-voltage discharge combined with fermentation or low-temperature plasma. Background Technology

[0002] Hawthorn (Crataegus pinnatifida Bunge) is the mature fruit of a deciduous tree belonging to the genus Crataegus in the family Rosaceae. Also known as mountain red or red fruit, it has been used in my country for over two thousand years as both food and medicine. Modern analysis shows that hawthorn pulp is rich in organic acids (citric acid, malic acid, etc.), flavonoids (quercetin, hyperoside, etc.), triterpenoids, vitamin C, pectin, sugars, and other active ingredients. It possesses physiological functions such as aiding digestion, promoting qi circulation, dispersing blood stasis, and reducing lipids. It is also an important raw material in the food industry for preparing hawthorn cakes, hawthorn leather, and beverages.

[0003] In the tobacco industry, hawthorn extract, as a traditional flavoring agent, can neutralize the alkalinity of cigarette smoke, mask impurities, reduce irritation, and impart a sweet fruity aroma and mellow taste to cigarettes. It has been widely used by domestic cigarette manufacturers. However, existing preparation technologies have the following main drawbacks:

[0004] 1. Traditional hot reflux or Soxhlet extraction: The process is simple and the equipment is inexpensive, but prolonged high temperature can easily cause heat-sensitive aroma components (such as low-boiling-point aldehydes, ketones, and esters) to volatilize or degrade, resulting in a thin aroma, heavy off-odors, high solvent consumption, and long extraction cycle.

[0005] 2. New technologies such as molecular distillation and supercritical extraction: Although they can improve the yield of aroma substances, the equipment is expensive and the operating cost is high, making it difficult to promote on a large scale.

[0006] 3. Single biological or physical methods: such as simple enzymatic hydrolysis or simple mechanical crushing, have limited effect on the dense structure of hawthorn pectin, cellulose and other components, resulting in insufficient release of aroma precursors and a lack of aroma richness in the product.

[0007] In recent years, high-voltage discharge has been proven to be a green and efficient extraction technology: it forms a "stream-electric breakdown" plasma channel in water, which instantaneously generates shock waves, cavitation bubbles and a large number of active particles such as OH and O, which destroy plant cell walls, promote the dissolution of intracellular effective components, and can be carried out at room temperature or low temperature, significantly reducing the loss of heat-sensitive substances.

[0008] On the other hand, low-temperature plasma can generate high-energy electrons and active oxygen / nitrogen species under normal pressure, which can etch and oxidize the surface of materials, increase the specific surface area, and break down macromolecular pectin and polysaccharides into low-molecular-weight aroma precursors.

[0009] In addition, microbial fermentation utilizes active yeasts (Saccharomyces cerevisiae, Yeast for aroma) to convert sugars, pectins, proteins, etc. in hawthorn into aroma substances such as alcohols, esters, and lactones under mild conditions, further enriching the aroma and reducing residual off-flavors.

[0010] However, the three technologies mentioned above (high-voltage discharge, low-temperature plasma, and fermentation) are currently used independently, and there are no reports of their synergistic integration for the preparation of hawthorn extract. How to use high-voltage discharge as the core, combined with low-temperature plasma cell disruption and fermentation for aroma enhancement, to construct a synergistic "physical-chemical-biological" process to achieve efficient release, targeted transformation, and quality improvement of hawthorn aroma remains a pressing technical challenge for the industry. Summary of the Invention

[0011] The purpose of this invention is to overcome the shortcomings of existing hawthorn extract preparation processes, such as easy volatility of aroma components, low extraction efficiency, and limited aroma range, and to provide a new method for the synergistic enhanced extraction of hawthorn extract using "high-voltage discharge-low-temperature plasma-fermentation" and its applications. This method can be completed under normal / low-temperature conditions and features a short cycle time, low solvent consumption, high aroma retention rate, and strong product applicability.

[0012] To achieve the above objectives, the present invention provides the following technical solution: a method for preparing hawthorn extract using high-voltage discharge combined with fermentation or low-temperature plasma, comprising the following steps:

[0013] S01. Dry the hawthorn at 80℃ for 12 hours, then pulverize it and pass it through a 60-mesh sieve to obtain hawthorn powder;

[0014] S02. Hawthorn powder is subjected to low-temperature plasma treatment to obtain pretreated powder;

[0015] S03. Add distilled water to the pretreated powder and perform high-voltage discharge treatment on the pretreated powder to obtain the discharge treatment solution.

[0016] S04. Add anhydrous ethanol to the discharge treatment solution and perform hot reflux to obtain reflux solution;

[0017] S05. Concentrate the reflux liquid under reduced pressure to obtain hawthorn extract.

[0018] A further technical solution of this application: the mass of distilled water added in step S03 is 4 to 5 times the mass of hawthorn powder; the high-voltage discharge treatment time is 5 to 40 minutes, and the voltage is 15 to 25 kV;

[0019] In step S04, the ratio of anhydrous ethanol added to liquid is 1:8 to 12, the volume concentration of ethanol in the anhydrous ethanol is 60% to 80%, and the reflux time is 30 to 120 minutes.

[0020] In step S05, the temperature for vacuum concentration is 40 to 60°C, and the vacuum degree for vacuum concentration is 0.09 MPa.

[0021] The final relative density of the hawthorn extract was 1.35 to 1.45 g / cm³. 3 .

[0022] A method for preparing hawthorn extract using high-voltage discharge and fermentation synergistically includes the following steps:

[0023] S11. After drying the hawthorn at 80℃ for 12 hours, pulverize it and pass it through a 60-mesh sieve to obtain hawthorn powder;

[0024] S12. Add 4 times the weight of distilled water to the hawthorn powder, and add mixed enzyme solution to adjust the pH value. Carry out enzymatic hydrolysis at 50℃ to obtain the enzymatic hydrolysate.

[0025] S13. Pump the enzyme hydrolysate into the high-voltage discharge treatment chamber for high-voltage discharge treatment, and filter to obtain the discharge treatment solution.

[0026] S14. Sterilize the discharge treatment solution at 121℃ for 30 min, then cool it to 40℃, inoculate it with 2% active yeast, and ferment for 5 to 25 days to obtain the fermentation broth.

[0027] S15. Add 3 times the volume of 95% ethanol to the fermentation broth, let it stand at 4°C for 24 hours, filter, and concentrate under reduced pressure at 55°C and a vacuum of 0.09 MPa to obtain hawthorn extract.

[0028] A further technical solution of this application: the high-voltage discharge adopts a needle-shaped electrode and a plate-shaped electrode structure, with an electrode spacing of 2 to 6 mm.

[0029] Hawthorn extract is used in cigarette flavoring to increase the aroma concentration, sweetness, and reduce irritation of cigarettes.

[0030] A further technical solution of this application: the processing time of the low-temperature plasma treatment in step S02 is 1 to 5 minutes.

[0031] A further technical solution of this application: the flow rate of the enzymatic hydrolysate pumped into the high-voltage discharge treatment chamber in step S13 is 8 to 12 mL / min;

[0032] In step S13, the voltage of the high-voltage discharge treatment is 9kV, and the treatment time is 20 to 40 minutes.

[0033] A further technical solution of this application: the mixed enzyme solution in step S12 is a mixture of pectinase and saccharifying enzyme in a mass ratio of 4 to 6: 1 to 2, wherein the pectinase activity is 40,000 U / g and the saccharifying enzyme activity is 20,000 U / g.

[0034] The amount of the mixed enzyme solution added is 1 to 3% of the mass of hawthorn powder;

[0035] The pH value is adjusted within the range of 4.5 to 5.5, and the enzymatic hydrolysis time is 2 to 4 hours.

[0036] A further technical solution of this application: the flow rate of the enzymatic hydrolysate pumped into the high-voltage discharge treatment chamber in step S13 is 8 to 12 mL / min;

[0037] In step S13, the voltage of the high-voltage discharge treatment is 9kV, and the treatment time is 20 to 40 minutes.

[0038] Compared with the prior art, the technical solution provided by this invention has the following advantages:

[0039] This invention uses high-voltage discharge as a hub, deeply coupling the instantaneous cell-wall breaking effect of low-temperature plasma with the directional transformation capability of microbial fermentation. It solves the four major pain points of traditional hawthorn extract: "weak aroma, heat sensitivity and susceptibility to damage, lengthy process, and high cost." It achieves significant advantages of "three highs and one low": significantly improved aroma richness, significantly improved extraction efficiency, significantly improved resource utilization, and significantly reduced energy consumption and emissions. The process is carried out at room temperature with a short range, the equipment is universal and easy to scale up, the solvent is recycled with zero waste, and the residue can be used to make fertilizer. It takes into account economic, environmental, and sensory benefits, and provides a replicable, scalable, and sustainable green manufacturing paradigm for the tobacco and food natural flavoring industries, with broad prospects for industrial application. Attached Figure Description

[0040] Figure 1 The total ion chromatogram of hawthorn extract obtained by hot reflux is shown below.

[0041] Figure 2 The total ion current chromatogram of hawthorn extract in Example 5 of this invention;

[0042] Figure 3 This is the total ion chromatogram of the hot reflux hawthorn extract prepared by the method of preparing hawthorn extract by high voltage discharge and fermentation in this invention;

[0043] Figure 4 This is the total ion chromatogram of hawthorn extract in Example 8 of the present invention. Detailed Implementation

[0044] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. The present invention will be further described below with reference to the embodiments.

[0045] Example 1

[0046] The method for preparing hawthorn extract using high-voltage discharge combined with low-temperature plasma and fermentation treatment provided by this invention includes the following steps:

[0047] S01. Dry the hawthorn at 80℃ for 12 hours, then pulverize it and pass it through a 60-mesh sieve to obtain hawthorn powder;

[0048] S02. Hawthorn powder is subjected to low-temperature plasma treatment to obtain pretreated powder;

[0049] S03. Add distilled water to the pretreated powder and perform high-voltage discharge treatment on the pretreated powder to obtain the discharge treatment solution.

[0050] S04. Add anhydrous ethanol to the discharge treatment solution and perform hot reflux to obtain reflux solution;

[0051] S05. Concentrate the reflux liquid under reduced pressure to obtain hawthorn extract.

[0052] Furthermore, the high-voltage discharge employs a needle-shaped electrode and a plate-shaped electrode structure with an electrode spacing of 5 mm.

[0053] Furthermore, the processing time for the low-temperature plasma treatment in step S02 is 1 minute.

[0054] Furthermore, in step S03, the mass of distilled water added is 4 times the mass of hawthorn powder; the high-voltage discharge treatment time is 20 minutes, and the voltage is 15kV.

[0055] In step S04, the ratio of anhydrous ethanol added to liquid is 1:8, the volume concentration of ethanol in the anhydrous ethanol is 60%, and the reflux time is 60 min.

[0056] In step S05, the temperature for vacuum concentration is 50°C, and the vacuum degree for vacuum concentration is 0.09 MPa.

[0057] The final relative density of the hawthorn extract was 1.38 g / cm³. 3 .

[0058] Example 2

[0059] The method for preparing hawthorn extract using high-voltage discharge combined with low-temperature plasma and fermentation treatment provided by this invention includes the following steps:

[0060] S01. Dry the hawthorn at 80℃ for 12 hours, then pulverize it and pass it through a 60-mesh sieve to obtain hawthorn powder;

[0061] S02. Hawthorn powder is subjected to low-temperature plasma treatment to obtain pretreated powder;

[0062] S03. Add distilled water to the pretreated powder and perform high-voltage discharge treatment on the pretreated powder to obtain the discharge treatment solution.

[0063] S04. Add anhydrous ethanol to the discharge treatment solution and perform hot reflux to obtain reflux solution;

[0064] S05. Concentrate the reflux liquid under reduced pressure to obtain hawthorn extract.

[0065] Furthermore, the high-voltage discharge employs a needle-shaped electrode and a plate-shaped electrode structure with an electrode spacing of 5 mm.

[0066] Furthermore, the processing time for the low-temperature plasma treatment in step S02 is 2 minutes.

[0067] Furthermore, in step S03, the mass of distilled water added is 5 times the mass of hawthorn powder; the high-voltage discharge treatment time is 25 minutes, and the voltage is 17.5 kV;

[0068] In step S04, the ratio of anhydrous ethanol to liquid is 1:9, the volume concentration of ethanol in the anhydrous ethanol is 75%, and the reflux time is 60 min.

[0069] In step S05, the temperature for vacuum concentration is 50°C, and the vacuum degree for vacuum concentration is 0.09 MPa.

[0070] The final relative density of the hawthorn extract was 1.37 g / cm³. 3 .

[0071] Example 3

[0072] The method for preparing hawthorn extract using high-voltage discharge combined with low-temperature plasma and fermentation treatment provided by this invention includes the following steps:

[0073] S01. Dry the hawthorn at 80℃ for 12 hours, then pulverize it and pass it through a 60-mesh sieve to obtain hawthorn powder;

[0074] S02. Hawthorn powder is subjected to low-temperature plasma treatment to obtain pretreated powder;

[0075] S03. Add distilled water to the pretreated powder and perform high-voltage discharge treatment on the pretreated powder to obtain the discharge treatment solution.

[0076] S04. Add anhydrous ethanol to the discharge treatment solution and perform hot reflux to obtain reflux solution;

[0077] S05. Concentrate the reflux liquid under reduced pressure to obtain hawthorn extract.

[0078] Furthermore, the high-voltage discharge employs a needle-shaped electrode and a plate-shaped electrode structure with an electrode spacing of 5 mm.

[0079] Furthermore, the processing time for the low-temperature plasma treatment in step S02 is 3 minutes.

[0080] Furthermore, in step S03, the mass of distilled water added is 4 times the mass of hawthorn powder; the high-voltage discharge treatment time is 30 minutes, and the voltage is 20kV;

[0081] In step S04, the ratio of anhydrous ethanol to liquid is 1:9, the volume concentration of ethanol in the anhydrous ethanol is 80%, and the reflux time is 60 min.

[0082] In step S05, the temperature for vacuum concentration is 55°C, and the vacuum degree for vacuum concentration is 0.09 MPa.

[0083] The final relative density of the hawthorn extract was 1.41 g / cm³. 3 .

[0084] Example 4

[0085] The method for preparing hawthorn extract using high-voltage discharge combined with low-temperature plasma and fermentation treatment provided by this invention includes the following steps:

[0086] S01. Dry the hawthorn at 80℃ for 12 hours, then pulverize it and pass it through a 60-mesh sieve to obtain hawthorn powder;

[0087] S02. Hawthorn powder is subjected to low-temperature plasma treatment to obtain pretreated powder;

[0088] S03. Add distilled water to the pretreated powder and perform high-voltage discharge treatment on the pretreated powder to obtain the discharge treatment solution.

[0089] S04. Add anhydrous ethanol to the discharge treatment solution and perform hot reflux to obtain reflux solution;

[0090] S05. Concentrate the reflux liquid under reduced pressure to obtain hawthorn extract.

[0091] Furthermore, the high-voltage discharge employs a needle-shaped electrode and a plate-shaped electrode structure with an electrode spacing of 5 mm.

[0092] Furthermore, the processing time for the low-temperature plasma treatment in step S02 is 4 minutes.

[0093] Furthermore, in step S03, the mass of distilled water added is 5 times the mass of hawthorn powder; the high-voltage discharge treatment time is 35 minutes, and the voltage is 22.5 kV;

[0094] In step S04, the ratio of anhydrous ethanol to liquid is 1:10, the volume concentration of ethanol in the anhydrous ethanol is 60%, and the reflux time is 120 min.

[0095] In step S05, the temperature for vacuum concentration is 55°C, and the vacuum degree for vacuum concentration is 0.09 MPa.

[0096] The final relative density of the hawthorn extract was 1.36 g / cm³. 3 .

[0097] Example 5

[0098] The method for preparing hawthorn extract using high-voltage discharge combined with low-temperature plasma and fermentation treatment provided by this invention includes the following steps:

[0099] S01. Dry the hawthorn at 80℃ for 12 hours, then pulverize it and pass it through a 60-mesh sieve to obtain hawthorn powder;

[0100] S02. Hawthorn powder is subjected to low-temperature plasma treatment to obtain pretreated powder;

[0101] S03. Add distilled water to the pretreated powder and perform high-voltage discharge treatment on the pretreated powder to obtain the discharge treatment solution.

[0102] S04. Add anhydrous ethanol to the discharge treatment solution and perform hot reflux to obtain reflux solution;

[0103] S05. Concentrate the reflux liquid under reduced pressure to obtain hawthorn extract.

[0104] Furthermore, the high-voltage discharge employs a needle-shaped electrode and a plate-shaped electrode structure with an electrode spacing of 5 mm.

[0105] Furthermore, the processing time for the low-temperature plasma treatment in step S02 is 5 minutes.

[0106] Furthermore, in step S03, the mass of distilled water added is 4 times the mass of hawthorn powder; the high-voltage discharge treatment time is 40 minutes, and the voltage is 25kV.

[0107] In step S04, the ratio of anhydrous ethanol to liquid is 1:8, the volume concentration of ethanol in the anhydrous ethanol is 80%, and the reflux time is 90 min.

[0108] In step S05, the temperature for vacuum concentration is 55°C, and the vacuum degree for vacuum concentration is 0.09 MPa.

[0109] The final relative density of the hawthorn extract was 1.43 g / cm³. 3 .

[0110] The hawthorn extract described in Examples 1 to 5 was added to the test tobacco of the Jin Sheng (Tengwangge) series of cigarettes to produce cigarettes. The cigarettes were then evaluated by five provincial-level taste testers using the usual evaluation methods in the cigarette industry. Each indicator was scored out of 10, with higher satisfaction scores receiving higher marks. The average score given by the five provincial-level taste testers was calculated. Hawthorn extract prepared by spraying the same mass of ethanol and using the hot reflux method was used as controls 1 and 2. The evaluation results are shown in Table 1.

[0111] Table 1. Evaluation Results

[0112] Serial Number experimental group Style and taste Comfort features flue gas characteristics Aroma characteristics 1 Blank control 1 6.2 6.1 6.5 7.2 2 Hot reflux hawthorn extract 7.5 6.3 7.4 7.8 3 Example 1 8.8 9.1 8.6 8.6 4 Example 2 8.9 8.4 9.1 8.8 5 Example 3 8.7 8.8 9.1 8.9 6 Example 4 8.8 8.9 8.9 8.7 7 Example 5 9.3 9.1 9.4 9.1

[0113] The best-performing flavoring effect was achieved in Example 5, which was analyzed by gas chromatography-mass spectrometry. The hawthorn extract obtained after high-voltage discharge-assisted ionic liquid treatment showed a higher content of heat-sensitive flavor compounds in its volatile aroma components compared to the hawthorn extract obtained by the hot reflux method. The types of aldehydes, ketones, and esters also increased. Table 2 shows the GC-MS analysis of the hawthorn extract obtained by the hot reflux method. The total ion chromatogram of the hot reflux hawthorn extract is shown below. Figure 1 As shown, the X-axis represents retention time in minutes, and the Y-axis represents abundance.

[0114] Table 2 GC-MS analysis of hot reflux hawthorn extract

[0115]

[0116]

[0117] The GC-MS analysis of the hawthorn extract prepared using the method of Example 5 is shown in Table 3. The results of the gas chromatography-mass spectrometry analysis of Example 5 are as follows: Figure 2 As shown, the X-axis represents retention time in minutes, and the Y-axis represents abundance.

[0118] Table 3. GC-MS analysis of hawthorn extract in Example 5

[0119]

[0120]

[0121] Example 6

[0122] The method for preparing hawthorn extract using high-voltage discharge and fermentation synergistically provided by this invention includes the following steps:

[0123] S11. After drying the hawthorn at 80℃ for 12 hours, pulverize it and pass it through a 60-mesh sieve to obtain hawthorn powder;

[0124] S12. Add 4 times the weight of distilled water to the hawthorn powder, and add mixed enzyme solution to adjust the pH value. Carry out enzymatic hydrolysis at 50℃ to obtain the enzymatic hydrolysate.

[0125] S13. Pump the enzyme hydrolysate into the high-voltage discharge treatment chamber for high-voltage discharge treatment, and filter to obtain the discharge treatment solution.

[0126] S14. Sterilize the discharge treatment solution at 121℃ for 30 min, cool it to 40℃, inoculate it with 2% active yeast, and ferment for 5 days to obtain the fermentation broth.

[0127] S15. Add 3 times the volume of 95% ethanol to the fermentation broth, let it stand at 4°C for 24 hours, filter, and concentrate under reduced pressure at 55°C and a vacuum of 0.09 MPa to obtain hawthorn extract.

[0128] Furthermore, the high-voltage discharge employs a needle-shaped electrode and a plate-shaped electrode structure with an electrode spacing of 2 mm.

[0129] Furthermore, the mixed enzyme solution in step S12 is a mixture of pectinase and saccharifying enzyme in a mass ratio of 4:1, wherein the pectinase activity is 40,000 U / g and the saccharifying enzyme activity is 20,000 U / g.

[0130] The amount of the mixed enzyme solution added is 1% of the mass of hawthorn powder;

[0131] The pH value is adjusted within a range of 4.5, and the enzymatic hydrolysis time is 2 hours.

[0132] Furthermore, in step S13, the flow rate of the enzymatic hydrolysate pumped into the high-voltage discharge treatment chamber is 8 mL / min.

[0133] In step S13, the voltage of the high-voltage discharge treatment is 9kV, and the treatment time is 20min.

[0134] Example 7

[0135] The method for preparing hawthorn extract using high-voltage discharge and fermentation synergistically provided by this invention includes the following steps:

[0136] S11. After drying the hawthorn at 80℃ for 12 hours, pulverize it and pass it through a 60-mesh sieve to obtain hawthorn powder;

[0137] S12. Add 4 times the weight of distilled water to the hawthorn powder, and add mixed enzyme solution to adjust the pH value. Carry out enzymatic hydrolysis at 50℃ to obtain the enzymatic hydrolysate.

[0138] S13. Pump the enzyme hydrolysate into the high-voltage discharge treatment chamber for high-voltage discharge treatment, and filter to obtain the discharge treatment solution.

[0139] S14. Sterilize the discharge treatment solution at 121℃ for 30 min, then cool it to 40℃, inoculate it with 2% active yeast, and ferment for 10 days to obtain the fermentation broth.

[0140] S15. Add 3 times the volume of 95% ethanol to the fermentation broth, let it stand at 4°C for 24 hours, filter, and concentrate under reduced pressure at 55°C and a vacuum of 0.09 MPa to obtain hawthorn extract.

[0141] Furthermore, the high-voltage discharge employs a needle-shaped electrode and a plate-shaped electrode structure with an electrode spacing of 3 mm.

[0142] Furthermore, the mixed enzyme solution in step S12 is a mixture of pectinase and saccharifying enzyme in a mass ratio of 5:1, wherein the pectinase activity is 40,000 U / g and the saccharifying enzyme activity is 20,000 U / g.

[0143] The amount of the mixed enzyme solution added is 2% of the mass of hawthorn powder;

[0144] The pH value is adjusted within a range of 5, and the enzymatic hydrolysis time is 2.5 hours.

[0145] Furthermore, in step S13, the flow rate of the enzymatic hydrolysate pumped into the high-voltage discharge treatment chamber is 9 mL / min.

[0146] In step S13, the voltage of the high-voltage discharge treatment is 9kV, and the treatment time is 25min.

[0147] Example 8

[0148] The method for preparing hawthorn extract using high-voltage discharge and fermentation synergistically provided by this invention includes the following steps:

[0149] S11. After drying the hawthorn at 80℃ for 12 hours, pulverize it and pass it through a 60-mesh sieve to obtain hawthorn powder;

[0150] S12. Add 4 times the weight of distilled water to the hawthorn powder, and add mixed enzyme solution to adjust the pH value. Carry out enzymatic hydrolysis at 50℃ to obtain the enzymatic hydrolysate.

[0151] S13. Pump the enzyme hydrolysate into the high-voltage discharge treatment chamber for high-voltage discharge treatment, and filter to obtain the discharge treatment solution.

[0152] S14. Sterilize the discharge treatment solution at 121℃ for 30 min, then cool it to 40℃, inoculate it with 2% active yeast, and ferment for 15 days to obtain the fermentation broth.

[0153] S15. Add 3 times the volume of 95% ethanol to the fermentation broth, let it stand at 4°C for 24 hours, filter, and concentrate under reduced pressure at 55°C and a vacuum of 0.09 MPa to obtain hawthorn extract.

[0154] Furthermore, the high-voltage discharge employs a needle-shaped electrode and a plate-shaped electrode structure with an electrode spacing of 4 mm.

[0155] Furthermore, the mixed enzyme solution in step S12 is a mixture of pectinase and saccharifying enzyme in a mass ratio of 3:1, wherein the pectinase activity is 40,000 U / g and the saccharifying enzyme activity is 20,000 U / g.

[0156] The amount of the mixed enzyme solution added is 3% of the mass of hawthorn powder;

[0157] The pH value is adjusted within a range of 5.5, and the enzymatic hydrolysis time is 3 hours.

[0158] Furthermore, in step S13, the flow rate of the enzymatic hydrolysate pumped into the high-voltage discharge treatment chamber is 10 mL / min.

[0159] In step S13, the voltage of the high-voltage discharge treatment is 9kV, and the treatment time is 30min.

[0160] Example 9

[0161] The method for preparing hawthorn extract using high-voltage discharge and fermentation synergistically provided by this invention includes the following steps:

[0162] S11. After drying the hawthorn at 80℃ for 12 hours, pulverize it and pass it through a 60-mesh sieve to obtain hawthorn powder;

[0163] S12. Add 4 times the weight of distilled water to the hawthorn powder, and add mixed enzyme solution to adjust the pH value. Carry out enzymatic hydrolysis at 50℃ to obtain the enzymatic hydrolysate.

[0164] S13. Pump the enzyme hydrolysate into the high-voltage discharge treatment chamber for high-voltage discharge treatment, and filter to obtain the discharge treatment solution.

[0165] S14. Sterilize the discharge treatment solution at 121℃ for 30 min, then cool it to 40℃, inoculate it with 2% active yeast, and ferment for 20 days to obtain the fermentation broth.

[0166] S15. Add 3 times the volume of 95% ethanol to the fermentation broth, let it stand at 4°C for 24 hours, filter, and concentrate under reduced pressure at 55°C and a vacuum of 0.09 MPa to obtain hawthorn extract.

[0167] Furthermore, the high-voltage discharge employs a needle-shaped electrode and a plate-shaped electrode structure with an electrode spacing of 5 mm.

[0168] Furthermore, the mixed enzyme solution in step S12 is a mixture of pectinase and saccharifying enzyme in a mass ratio of 5:2, wherein the pectinase activity is 40,000 U / g and the saccharifying enzyme activity is 20,000 U / g.

[0169] The amount of the mixed enzyme solution added is 3% of the mass of hawthorn powder;

[0170] The pH value is adjusted within a range of 4.5, and the enzymatic hydrolysis time is 3.5 hours.

[0171] Furthermore, in step S13, the flow rate of the enzymatic hydrolysate pumped into the high-voltage discharge treatment chamber is 11 mL / min.

[0172] In step S13, the voltage of the high-voltage discharge treatment is 9kV, and the treatment time is 35min.

[0173] Example 10

[0174] The method for preparing hawthorn extract using high-voltage discharge and fermentation synergistically provided by this invention includes the following steps:

[0175] S11. After drying the hawthorn at 80℃ for 12 hours, pulverize it and pass it through a 60-mesh sieve to obtain hawthorn powder;

[0176] S12. Add 4 times the weight of distilled water to the hawthorn powder, and add mixed enzyme solution to adjust the pH value. Carry out enzymatic hydrolysis at 50℃ to obtain the enzymatic hydrolysate.

[0177] S13. Pump the enzyme hydrolysate into the high-voltage discharge treatment chamber for high-voltage discharge treatment, and filter to obtain the discharge treatment solution.

[0178] S14. Sterilize the discharge treatment solution at 121℃ for 30 min, then cool it to 40℃, inoculate it with 2% active yeast, and ferment for 25 days to obtain the fermentation broth.

[0179] S15. Add 3 times the volume of 95% ethanol to the fermentation broth, let it stand at 4°C for 24 hours, filter, and concentrate under reduced pressure at 55°C and a vacuum of 0.09 MPa to obtain hawthorn extract.

[0180] Furthermore, the high-voltage discharge employs a needle-shaped electrode and a plate-shaped electrode structure with an electrode spacing of 6 mm.

[0181] Furthermore, the mixed enzyme solution in step S12 is a mixture of pectinase and saccharifying enzyme in a mass ratio of 6:1, wherein the pectinase activity is 40,000 U / g and the saccharifying enzyme activity is 20,000 U / g.

[0182] The amount of the mixed enzyme solution added is 2% of the mass of hawthorn powder;

[0183] The pH value is adjusted within a range of 5, and the enzymatic hydrolysis time is 4 hours.

[0184] Furthermore, in step S13, the flow rate of the enzymatic hydrolysate pumped into the high-voltage discharge treatment chamber is 12 mL / min.

[0185] In step S13, the voltage of the high-voltage discharge treatment is 9kV, and the treatment time is 40min.

[0186] The hawthorn extract described in Examples 6-10 was added to the test tobacco of the Jin Sheng (Tengwangge) series of cigarettes to produce cigarettes. The cigarettes were then evaluated by five provincial-level taste testers using the usual evaluation methods in the cigarette industry. Each indicator was scored out of 10, with higher satisfaction scores receiving higher marks. The average score given by the five provincial-level taste testers was calculated. Hawthorn extract prepared by spraying the same mass of ethanol and using the hot reflux method was used as controls 1 and 2. The evaluation results are shown in Table 4.

[0187] Table 4 Evaluation Results

[0188]

[0189]

[0190] The best-performing flavoring effect was achieved in Example 8, which was analyzed by gas chromatography-mass spectrometry. The hawthorn extract obtained after high-voltage discharge-assisted ionic liquid treatment showed a higher content of heat-sensitive flavor compounds in its volatile aroma components compared to the hawthorn extract obtained by the hot reflux method. The types of aldehydes, ketones, and esters also increased. The GC-MS analysis of the hawthorn extract obtained by the hot reflux method is shown in Table 5. The total ion chromatogram of the hot reflux hawthorn extract is shown below. Figure 3 As shown, the X-axis represents retention time in minutes, and the Y-axis represents abundance.

[0191] Table 5 GC-MS analysis of hot reflux hawthorn extract

[0192]

[0193] The GC-MS analysis of the hawthorn extract prepared using the method of Example 8 is shown in Table 6. The results of the gas chromatography-mass spectrometry analysis of Example 8 are as follows: Figure 4 As shown, the X-axis represents retention time in minutes, and the Y-axis represents abundance.

[0194] Table 6. GC-MS analysis of hawthorn extract in Example 8.

[0195]

[0196] The present invention and its embodiments have been described above illustratively. This description is not restrictive, and the figures shown are only one embodiment of the present invention; the actual structure is not limited thereto. Therefore, if those skilled in the art are inspired by this description and design similar structures and embodiments without departing from the spirit of the present invention, such designs should fall within the protection scope of the present invention.

[0197] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A method for preparing hawthorn extract using high-voltage discharge combined with low-temperature plasma and fermentation treatment, characterized in that, The steps are as follows: S01. Dry the hawthorn at 80℃ for 12 hours, then pulverize it and pass it through a 60-mesh sieve to obtain hawthorn powder; S02. Hawthorn powder is subjected to low-temperature plasma treatment to obtain pretreated powder; S03. Add distilled water to the pretreated powder and perform high-voltage discharge treatment on the pretreated powder to obtain the discharge treatment solution. S04. Add anhydrous ethanol to the discharge treatment solution and perform hot reflux to obtain reflux solution; S05. Concentrate the reflux liquid under reduced pressure to obtain hawthorn extract.

2. A method for preparing hawthorn extract using high-voltage discharge and fermentation synergistically, characterized in that, Includes the following steps: S11. After drying the hawthorn at 80℃ for 12 hours, pulverize it and pass it through a 60-mesh sieve to obtain hawthorn powder; S12. Add 4 times the weight of distilled water to the hawthorn powder, and add mixed enzyme solution to adjust the pH value. Carry out enzymatic hydrolysis at 50℃ to obtain the enzymatic hydrolysate. S13. Pump the enzyme hydrolysate into the high-voltage discharge treatment chamber for high-voltage discharge treatment, and filter to obtain the discharge treatment solution. S14. Sterilize the discharge treatment solution at 121℃ for 30 minutes, then cool it to 40℃, inoculate it with 2% active yeast, and ferment for 5 to 25 days to obtain the fermentation broth. S15. Add 3 times the volume of 95% ethanol to the fermentation broth, let it stand at 4℃ for 24 hours, filter it, and concentrate it under reduced pressure at 55℃ and a vacuum of 0.09 MPa to obtain hawthorn extract.

3. The method for preparing hawthorn extract according to claim 1 or 2, characterized in that, The high-voltage discharge employs needle-shaped and plate-shaped electrode structures with an electrode spacing of 2 to 6 mm.

4. The use of hawthorn extract in cigarette flavoring, characterized by: The hawthorn extract is prepared by the method described in claim 1 or 2 and is used to improve the aroma concentration and sweetness of cigarettes while reducing their irritation.

5. The method for preparing hawthorn extract using high-voltage discharge combined with low-temperature plasma and fermentation treatment according to claim 1, characterized in that, The processing time for the low-temperature plasma treatment in step S02 is 1 to 5 minutes.

6. The method for preparing hawthorn extract using high-voltage discharge combined with low-temperature plasma and fermentation treatment according to claim 1, characterized in that, In step S03, the mass of distilled water added is 4 to 5 times the mass of hawthorn powder; the high-voltage discharge treatment time is 5 to 40 minutes, and the voltage is 15 to 25 kV. In step S04, the ratio of anhydrous ethanol added to liquid is 1:8 to 12, the volume concentration of ethanol in the anhydrous ethanol is 60% to 80%, and the reflux time is 30 to 120 minutes. In step S05, the temperature for vacuum concentration is 40 to 60°C, and the vacuum degree for vacuum concentration is 0.09 MPa. The final relative density of the hawthorn extract is 1.35 to 1.45 g / cm³.

7. The method for preparing hawthorn extract using high-voltage discharge and fermentation synergistically according to claim 2, characterized in that, The mixed enzyme solution in step S12 is a mixture of pectinase and saccharifying enzyme in a mass ratio of 4 to 6:1 to 2, wherein the pectinase activity is 40,000 U / g and the saccharifying enzyme activity is 20,000 U / g. The amount of the mixed enzyme solution added is 1 to 3% of the mass of hawthorn powder; The pH value is adjusted within the range of 4.5 to 5.5, and the enzymatic hydrolysis time is 2 to 4 hours.

8. The method for preparing hawthorn extract using high-voltage discharge and fermentation synergistically according to claim 2, characterized in that, In step S13, the flow rate of the enzymatic hydrolysate pumped into the high-voltage discharge treatment chamber is 8 to 12 mL / min. In step S13, the voltage of the high-voltage discharge treatment is 9kV, and the treatment time is 20 to 40 minutes.

Images