Method for preparing fig extract using ozone and pulsed light

Abstract

The present invention belongs to the technical field of tobacco flavorings, specifically relating to a method for preparing fig extract using ozone and pulsed light, and its application in cigarettes. This method utilizes pulsed light and ozone treatment to improve the extraction process of fig extract, thereby increasing the yield and quality of the extract and reducing the volatilization of heat-sensitive flavor components. The extracted fig extract has the advantages of increasing the aroma concentration of cigarettes, enhancing the sweetness of cigarettes, reducing cigarette irritation, and improving cigarette comfort.

Description

Technical Field

[0001] The invention belongs to the technical field of tobacco flavorings, and particularly relates to a method for preparing fig extract by utilizing ozone and pulsed light. The invention also relates to application of the tobacco flavoring in cigarettes. Background Art

[0002] The fig, also known as the "Wenxian Guo" (Chinese fig) or "Yingri Guo" (Chinese fig), is a deciduous shrub or small tree in the Moraceae family. Its thin, soft skin and tender, sweet flesh are rich in carbohydrates, protein, crude fiber, polyphenols, and flavonoids. Considered both a medicinal and edible plant, it is not only edible but also highly valued for its stomach-tonifying, intestinal-clearing, swelling-reducing, and detoxifying properties. It is primarily used to treat symptoms such as loss of appetite, sore throat, and cough with phlegm.

[0003] In the field of tobacco production technology, figs are primarily used to prepare extracts for cigarette flavoring. Fig extract is one of the earliest traditional flavoring ingredients used in cigarettes, possessing characteristic aromas such as sweet, fruity, and tobacco. It is a key spice used in tobacco flavorings to create both sweet and creamy notes. While traditional plant extract preparation methods are simple, easy to operate, and inexpensive, they suffer from long reaction cycles, high solvent consumption, ineffective enrichment of flavoring components, and low quality. Newer technologies, such as molecular distillation and supercritical fluid extraction, have limited investment, high operating costs, and low yields, resulting in low returns. Summary of the Invention

[0004] Based on the above reasons, the purpose of the present invention is to provide a method for preparing fig extract with high extraction efficiency, low impurity content and low organic solvent usage. The extract prepared by the method contains a high level of aroma-causing substances and can significantly improve the aroma concentration and sweetness of cigarettes.

[0005] The purpose of the present invention is achieved through the following technical solutions:

[0006] A first aspect of the present invention provides a method for preparing fig extract using ozone and pulsed light, comprising the following steps:

[0007] (1) Drying commercially available dried figs;

[0008] (2) Grinding the dried figs into powder in time, and passing through a 60-mesh sieve to obtain fig powder;

[0009] (3) Pulsed light treatment of fig powder;

[0010] (4) adding 3 to 4 times the mass of distilled water to the pulsed light treated fig powder, and then adding 1 to 3% of the mass of the mixed enzyme solution to the fig powder, adjusting the pH to 4.5 to 5.5 with acid, stirring evenly, and performing enzymolysis at 50° C. for 2 to 4 hours to obtain a fig enzymatic hydrolyzate;

[0011] (5) ozone treatment of the fig enzymatic hydrolysate;

[0012] (6) adding anhydrous ethanol to the ozone-treated fig hydrolysate, refluxing for 30 to 120 minutes, and filtering to obtain an extract;

[0013] (7) Concentrate the extract to a relative density of 1.35-1.45 g / cm 3 of the extract.

[0014] Furthermore, the drying in step (1) refers to drying at 70-80° C. for 10-15 hours.

[0015] Furthermore, the pulse light treatment conditions in step (3) are: pulse light intensity 2 to 8 J / m 2 , voltage is 1~4kV, pulse energy is 2~5J, pulse frequency is 1~8 times / s, and pulse light treatment time is 5~30min.

[0016] Furthermore, the mixed enzyme solution in step (4) is prepared by mixing pectinase and saccharifying enzyme in a mass ratio of 4-6:1-2, wherein the pectinase activity is 30,000-40,000 U / g, and the saccharifying enzyme activity is 10,000-20,000 U / g, both of which are food grade.

[0017] Furthermore, the acid in step (4) is 1 mol / L citric acid solution or 1 mol / L sodium citrate solution.

[0018] Furthermore, in step (5), ozone treatment is performed by uniformly introducing ozone for 10 to 40 minutes, with an ozone flow rate of 20 to 200 L / h.

[0019] Furthermore, the amount of anhydrous ethanol added in step (6) is: added until the material-liquid ratio is 1:8-12 and the ethanol concentration is 60%-80%.

[0020] Furthermore, the concentration in step (7) is carried out by using a rotary evaporator under reduced pressure, with a temperature of 45 to 60° C. and a rotation speed of 45 to 65 rpm.

[0021] The second aspect of the present invention provides the use of the fig extract prepared by the method in cigarettes.

[0022] Furthermore, the application method is: diluting the prepared fig extract with water or alcohol solution and then adding the diluted extract to shredded tobacco to prepare cigarettes.

[0023] The present invention achieves the following technical effects.

[0024] This patent innovatively combines ozone and pulsed light treatment for the extraction of fig extract, establishing a preparation method with high extraction efficiency, low impurities, short reaction cycle, and low use of organic solvents. This method can prepare fig extract with high aroma-causing substances, which has the advantages of increasing aroma concentration, increasing the sweetness of cigarettes, reducing cigarette irritation, and improving comfort when used in cigarettes. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 The figure is the total ion current chromatogram of the heat reflux fig extract of the present invention.

[0026] Figure 2 This is the total ion current chromatogram of the fig extract of Example 4 of the present invention. DETAILED DESCRIPTION

[0027] In order to more clearly understand the above-mentioned objects, features and advantages of the present invention, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments. It should be noted that the embodiments of the present invention and the features therein can be combined with each other without conflict.

[0028] In the following description, many specific details are set forth to facilitate a full understanding of the present invention. However, the present invention may also be implemented in other ways different from those described herein. Therefore, the scope of protection of the present invention is not limited to the specific embodiments disclosed below.

[0029] Example 1

[0030] (1) Commercially available dried figs were dried at 80°C for 12 h to promote the Maillard reaction of proteins and sugars in the figs at high temperature.

[0031] (2) The dried figs were promptly crushed into powder and passed through a 60-mesh sieve to obtain fig powder.

[0032] (3) The fig powder in (2) was treated with pulsed light. The reaction conditions were: pulsed light intensity 4 J / m 2 , voltage is 2kV, pulse energy is 3J, pulse frequency is 4 times / s, and pulse light treatment time is 10min.

[0033] (4) Take 200 g of fig powder, add distilled water 3 times the weight of fig powder, then add 2% of the weight of fig mixed enzyme solution, adjust the pH to 4.5 with 1 mol / L sodium citrate solution, stir evenly, and enzymolyze at 50°C for 3 h to obtain fig enzymatic hydrolyzate.

[0034] The mixed enzyme solution is prepared by mixing 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, both of which are food grade.

[0035] (5) Ozone was introduced into the enzymatic hydrolysate in (4) at a constant rate of 50 L / h for 25 min.

[0036] (6) Anhydrous ethanol was added to the ozone-treated enzymatic hydrolysate to make the final material-liquid ratio 1:8 and the ethanol concentration 80%, and then the mixture was refluxed for 60 minutes and filtered to obtain an extract.

[0037] (7) The extract of (6) was placed on a rotary evaporator and concentrated under reduced pressure to a relative density of 1.45 g / cm 3 The extract temperature is 45-60℃ and the rotation speed is 65rpm.

[0038] Example 2

[0039] (1) Commercially available dried figs were dried at 80°C for 12 h to promote the Maillard reaction of proteins and sugars in the figs at high temperature.

[0040] (2) The dried figs were promptly crushed into powder and passed through a 60-mesh sieve to obtain fig powder.

[0041] (3) The fig powder in (2) was treated with pulsed light. The reaction conditions were: pulsed light intensity 5 J / m 2 , voltage is 1kV, pulse energy is 2J, pulse frequency is 3 times / s, and pulse light treatment time is 5min.

[0042] (4) Take 200 g of fig powder, add distilled water 4 times the mass of fig powder, then add 1% of the mass of fig mixed enzyme solution, adjust the pH to 5.5 with 1 mol / L citric acid solution, stir evenly, and enzymolyze at 50°C for 4 h to obtain fig enzymatic hydrolyzate.

[0043] The mixed enzyme solution is prepared by mixing pectinase and saccharifying enzyme in a mass ratio of 4:2, wherein the pectinase activity is 30,000 U / g and the saccharifying enzyme activity is 10,000 U / g, both of which are food grade.

[0044] (5) Ozone was introduced into the enzymatic hydrolysate in (4) at a constant rate of 20 to 200 L / h for 15 min.

[0045] (6) Anhydrous ethanol was added to the ozone-treated enzymatic hydrolysate to make the final material-liquid ratio 1:10 and the ethanol concentration 80%, and then the mixture was refluxed for 50 minutes and filtered to obtain an extract.

[0046] (7) The extract of (6) was placed on a rotary evaporator and concentrated under reduced pressure to a relative density of 1.35 g / cm 3 The extract was stirred at a temperature of 50°C and a rotation speed of 50 rpm.

[0047] Example 3

[0048] (1) Commercially available dried figs were dried at 80°C for 12 h to promote the Maillard reaction of proteins and sugars in the figs at high temperature.

[0049] (2) The dried figs were promptly crushed into powder and passed through a 60-mesh sieve to obtain fig powder.

[0050] (3) The fig powder in (2) was treated with pulsed light. The reaction conditions were: pulsed light intensity 6 J / m 2 , voltage is 3kV, pulse energy is 3J, pulse frequency is 6 times / s, and pulse light treatment time is 25min.

[0051] (4) Take 200 g of fig powder, add distilled water 3 times the mass of fig powder, then add 1% of the mass of fig mixed enzyme solution, adjust the pH to 4.5 with 1 mol / L sodium citrate solution, stir evenly, and enzymolyze at 50°C for 2 h to obtain fig enzymatic hydrolyzate.

[0052] The mixed enzyme solution is prepared by mixing 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 10,000 U / g, both of which are food grade.

[0053] (5) Ozone was introduced into the enzymatic hydrolysate in (4) at a constant rate of 100 L / h for 15 min.

[0054] (6) Anhydrous ethanol was added to the ozone-treated enzymatic hydrolysate to make the final material-liquid ratio 1:12 and the ethanol concentration 70%, and then the mixture was refluxed for 70 minutes and filtered to obtain an extract.

[0055] (7) The extract of (6) was placed on a rotary evaporator and concentrated under reduced pressure to a relative density of 1.38 g / cm 3 The extract was stirred at a temperature of 55°C and a rotation speed of 50 rpm.

[0056] Example 4

[0057] (1) Commercially available dried figs were dried at 80°C for 12 h to promote the Maillard reaction of proteins and sugars in the figs at high temperature.

[0058] (2) The dried figs were promptly crushed into powder and passed through a 60-mesh sieve to obtain fig powder.

[0059] (3) The fig powder in (2) was treated with pulsed light. The reaction conditions were: pulsed light intensity 7 J / m 2 , voltage is 3kV, pulse energy is 2J, pulse frequency is 1 time / s, and pulse light treatment time is 30min.

[0060] (4) Take 200 g of fig powder, add distilled water 4 times the weight of fig powder, then add 3% of the weight of fig mixed enzyme solution, adjust the pH to 5.0 with 1 mol / L citric acid solution, stir evenly, and enzymolyze at 50°C for 4 h to obtain fig enzymatic hydrolyzate.

[0061] The mixed enzyme solution is prepared by mixing 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 10,000 U / g, both of which are food grade.

[0062] (5) Ozone was introduced into the enzymatic hydrolysate in (4) at a constant rate of 25 L / h for 25 min.

[0063] (6) Anhydrous ethanol was added to the ozone-treated enzymatic hydrolysate to make the final material-liquid ratio 1:8 and the ethanol concentration 60%, and then refluxed for 45 minutes and filtered to obtain an extract.

[0064] (7) The extract of (6) was placed on a rotary evaporator and concentrated under reduced pressure to a relative density of 1.42 g / cm 3 The extract was stirred at 60°C and the rotation speed was 65 rpm.

[0065] Example 5

[0066] (1) Commercially available dried figs were dried at 80°C for 12 h to promote the Maillard reaction of proteins and sugars in the figs at high temperature.

[0067] (2) The dried figs were promptly crushed into powder and passed through a 60-mesh sieve to obtain fig powder.

[0068] (3) The fig powder in (2) was treated with pulsed light. The reaction conditions were: pulsed light intensity 6 J / m 2 , voltage is 4kV, pulse energy is 5J, pulse frequency is 1 to 8 times / s, and pulse light treatment time is 30min.

[0069] (4) Take 200 g of fig powder, add distilled water 4 times the weight of fig powder, then add 2% of the weight of fig mixed enzyme solution, adjust the pH to 5.5 with 1 mol / L citric acid solution, stir evenly, and enzymolyze at 50°C for 4 h to obtain fig enzymatic hydrolyzate.

[0070] The mixed enzyme solution is prepared by mixing 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 10,000 U / g, and both are food grade.

[0071] (5) Ozone was introduced into the enzymatic hydrolysate in (4) at a constant rate of 100 L / h for 40 min.

[0072] (6) Anhydrous ethanol was added to the ozone-treated enzymatic hydrolysate to make the final material-liquid ratio 1:12 and the ethanol concentration 70%, and then the mixture was refluxed for 120 minutes and filtered to obtain an extract.

[0073] (7) The extract of (6) was placed on a rotary evaporator and concentrated under reduced pressure to a relative density of 1.43 g / cm 3 The extract was stirred at 60°C and the rotation speed was 65 rpm.

[0074] Comparative Example 1

[0075] (1) Commercially available dried figs were dried at 80°C for 12 h to promote the Maillard reaction of proteins and sugars in the figs at high temperature.

[0076] (2) The dried figs were promptly crushed into powder and passed through a 60-mesh sieve to obtain fig powder.

[0077] (3) Take 200 g of fig powder, add distilled water 4 times the mass of fig powder, then add 3% of the mass of fig mixed enzyme solution, adjust the pH to 5.0 with 1 mol / L citric acid solution, stir evenly, and enzymolyze at 50°C for 4 h to obtain fig enzymatic hydrolyzate.

[0078] The mixed enzyme solution is prepared by mixing 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 10,000 U / g, both of which are food grade.

[0079] (4) Ozone was introduced into the enzymatic hydrolysate in (3) at a constant rate of 25 L / h for 25 min.

[0080] (5) Anhydrous ethanol was added to the ozone-treated enzymatic hydrolysate to make the final material-liquid ratio 1:8 and the ethanol concentration 60%, and then the mixture was refluxed for 45 minutes and filtered to obtain an extract.

[0081] (6) The extract was treated with pulsed light. The reaction conditions were: pulsed light intensity 7 J / m 2 , voltage is 3kV, pulse energy is 2J, pulse frequency is 1 time / s, and pulse light treatment time is 30min.

[0082] (7) The extract of (6) was placed on a rotary evaporator and concentrated under reduced pressure to a relative density of 1.42 g / cm 3 The extract was stirred at 60°C and the rotation speed was 65 rpm.

[0083] Comparative Example 2

[0084] (1) Commercially available dried figs were dried at 80°C for 12 h to promote the Maillard reaction of proteins and sugars in the figs at high temperature.

[0085] (2) The dried figs were promptly crushed into powder and passed through a 60-mesh sieve to obtain fig powder.

[0086] (3) Take 200 g of fig powder, add distilled water 4 times the mass of fig powder, then add 3% of the mass of fig mixed enzyme solution, adjust the pH to 5.0 with 1 mol / L citric acid solution, stir evenly, and enzymolyze at 50°C for 4 h to obtain fig enzymatic hydrolyzate.

[0087] The mixed enzyme solution is prepared by mixing 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 10,000 U / g, both of which are food grade.

[0088] (4) The fig enzymatic hydrolysate was treated with pulsed light. The reaction conditions were: pulsed light intensity 7 J / m 2 , voltage is 3kV, pulse energy is 2J, pulse frequency is 1 time / s, and pulse light treatment time is 30min.

[0089] (5) Ozone was introduced into the pulsed light treated fig enzymatic hydrolysate at a constant speed for 25 min, with an ozone flow rate of 25 L / h.

[0090] (6) Anhydrous ethanol was added to the ozone-treated enzymatic hydrolysate to make the final material-liquid ratio 1:8 and the ethanol concentration 60%, and then refluxed for 45 minutes and filtered to obtain an extract.

[0091] (7) The extract of (6) was placed on a rotary evaporator and concentrated under reduced pressure to a relative density of 1.42 g / cm 3 The extract was stirred at 60°C and the rotation speed was 65 rpm.

[0092] The fig extracts described in Examples 1 to 5 and Comparative Examples 1 to 2 were added to the test tobacco of the Jinsheng (Tengwang Pavilion) series cigarettes to prepare cigarettes. Cigarettes were evaluated by five provincial-level smoking assessors according to the common evaluation method YC / T497-2014_Chinese-style cigarette sensory evaluation method in the cigarette industry. Each indicator was scored out of 10 points. The higher the satisfaction, the higher the score. The average score of the five provincial-level smoking assessors was calculated. A blank control 1 was prepared by spraying the same mass of ethanol, and a tobacco extract prepared by the hot reflux method was used as a control 2. The hot reflux method was specifically as follows: the fig powder treated in the same manner as in the example was placed in a reflux device, 1:10 ethanol was added, and the extract was obtained for 120 minutes to obtain an extract. The extract was placed on a rotary concentrator and concentrated under reduced pressure to a relative density of 1.42 g / cm 3 The extract was evaluated in Table 1.

[0093] Gas chromatography-mass spectrometry analysis was performed on Example 4, which had the best flavoring effect. The content of heat-sensitive flavor substances (such as 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyran-4-one and 5-hydroxymethylfurfural) in the volatile flavor components of the fig extract obtained after ozone treatment was higher than that of the fig extract obtained by the hot reflux method. The types of substances such as aldehydes, ketones, and esters (such as 5-methyl-2-furfural, perillone, vanillin, ethyl oleate, and ethyl linoleate) also increased.

[0094] Table 1 Evaluation results

[0095]

[0096]

[0097] Table 2 GC-MS analysis of hot reflux fig extract

[0098]

[0099]

[0100] Table 3 GC-MS analysis of Fig extract of Example 4

[0101]

[0102]

[0103]

Claims

1. A method for preparing fig extract using ozone and pulsed light, characterized in that: The following steps are involved: (1) Dry commercially available dried figs; (2) Grind the dried figs into powder in time, and pass through a 60-mesh sieve to obtain fig powder; (3) Pulsed light treatment of fig powder; (4) Add 3-4 times the mass of distilled water to the pulsed light treated fig powder, then add 1-3% of the mass of the mixed enzyme solution to the mixture, adjust the pH to 4.5-5.5 with acid, stir evenly, and perform enzymolysis at 50°C for 2-4 hours to obtain a fig enzymatic hydrolysate. (5) ozone treatment of fig enzymatic hydrolysate; (6) Add anhydrous ethanol to the ozone-treated fig hydrolysate, reflux for 30-120 min, and filter to obtain an extract; (7) Concentrate the extract to a relative density of 1.35~1.45g / cm 3 of the extract, The mixed enzyme solution in step (4) is prepared by mixing pectinase and saccharifying enzyme in a mass ratio of 4-6:1-2, wherein the pectinase activity is 30,000-40,000 U / g, and the saccharifying enzyme activity is 10,000-20,000 U / g, both of which are food grade.

2. The method for preparing fig extract using ozone and pulsed light according to claim 1, characterized in that: The drying in step (1) refers to drying at 70-80°C for 10-15 hours.

3. The method for preparing fig extract using ozone and pulsed light according to claim 1, characterized in that: The pulse light treatment conditions in step (3) are: pulse light intensity 2~8J / m 2 , voltage is 1~4 kV, pulse energy is 2~5 J, pulse frequency is 1~8 times / s, and pulse light treatment time is 5~30 min.

4. The method for preparing fig extract using ozone and pulsed light according to claim 1, wherein: The acid in step (4) is 1 mol / L citric acid solution or 1 mol / L sodium citrate solution.

5. The method for preparing fig extract using ozone and pulsed light according to claim 1, characterized in that: In step (5), ozone treatment is performed by uniformly introducing ozone for 10 to 40 minutes, with an ozone flow rate of 20 to 200 L / h.

6. The method for preparing fig extract using ozone and pulsed light according to claim 1, characterized in that: The amount of anhydrous ethanol added in step (6) is: added until the material-liquid ratio is 1:8~12 and the ethanol concentration is 60%~80%.

7. The method for preparing the fig extract according to claim 1, wherein: The concentration in step (7) is carried out by using a rotary evaporator under reduced pressure at a temperature of 45-60° C. and a rotation speed of 45-65 rpm.

8. Use of the fig extract prepared by the method according to any one of claims 1 to 7 in cigarettes.

9. The use according to claim 8, characterized in that The application method comprises the following steps: diluting the prepared fig extract with water or alcohol solution and then adding the diluted extract into shredded tobacco to prepare cigarettes.

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