Improved preparation method of fig extract

Abstract

The present invention belongs to the technical field of tobacco flavorings, specifically relating to an improved preparation method for fig extract and its use in cigarettes. This method utilizes various techniques, including ionizing radiation, pulsed light, and ozone, 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 present invention belongs to the technical field of tobacco flavorings, and mainly relates to an improved preparation method of fig extract. The present invention also relates to the application of the tobacco flavoring in cigarettes. Background Art

[0002] The fig is a deciduous shrub or small tree in the genus Ficus in the Moraceae family, also known as the "Wenxianguo" (Chinese fig) or "Yingriguo" (Chinese fig). Figs actually have flowers, but the inflorescence is cryptic, hidden within the fruit. The fruit we eat is primarily the fig flower. Figs have a thin, soft skin, a tender flesh, a sweet taste, and rich nutrition. They are considered both a medicinal and edible plant. Not only is it edible, it also has high medicinal value, boasting stomach-tonifying, intestinal-clearing, swelling-reducing, and detoxifying properties. They are 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 mainly used to prepare extracts for cigarette flavoring. Fig extract is one of the traditional fragrance raw materials used in cigarettes earlier. It has characteristic aromas such as sweet, fruity, and tobacco. It is an important spice used to mix sweet and creamy aromas in tobacco flavors. The traditional method of extracting extracts is to use organic solvents to soak the organ tissues of spice plants (such as flowers, branches, leaves, bark, roots, fruits, etc.), and then obtain a viscous extract with a rich aroma after filtering, evaporation, and other operations. Because the composition of the extract is relatively complex, it also contains a certain amount of impurities, such as plant waxes and pigments. Moreover, although the traditional method is simple to operate, it uses a large amount of organic solvents, is time-consuming, and has a low extraction rate. Summary of the Invention

[0004] This patent addresses the problems of the existing fig extract extraction process, such as long reaction cycle, high solvent consumption, and low aroma components. It provides an efficient method for preparing fig extract. The method innovatively combines ozone, ionizing radiation and pulsed light for extracting the extract, which is beneficial to improving the yield and quality of the extract and reducing the volatilization of heat-sensitive aroma components.

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

[0006] A first aspect of the present invention provides an improved method for preparing fig extract, comprising the following steps:

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

[0008] (2) treating dried figs with ionizing radiation;

[0009] (3) promptly crushing the dried figs treated with ionizing radiation into powder, and passing the powder through a 60-mesh sieve to obtain fig powder;

[0010] (4) Pulsed light treatment of fig powder;

[0011] (5) Take fig powder, add distilled water 3 to 4 times the mass of fig powder, then add 1 to 3% of the mass of fig mixed enzyme solution, adjust the pH to 4.5 to 5.5 with acid, stir evenly, and perform enzymolysis at 50°C for 2 to 4 hours to obtain fig enzymatic hydrolyzate;

[0012] (6) introducing ozone into the fig enzymatic hydrolysate;

[0013] (7) adding anhydrous ethanol to the ozone-treated enzymatic hydrolyzate, refluxing for 30 to 120 minutes, and filtering to obtain an extract;

[0014] (8) Concentrate the extract to a relative density of 1.35-1.45 g / cm 3 of the extract.

[0015] Furthermore, the drying in step (1) refers to drying at 70-80° C. for 10-15 hours.

[0016] Furthermore, the ionizing radiation in step (2) has a radiation dose of 1.0 to 5.0 Gy, a radiation rate of 0.5 to 3.0 Gy / min, and a radiation time of 20 to 60 seconds.

[0017] Furthermore, the intensity of the pulsed light in step (4) is 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.

[0018] Furthermore, the mixed enzyme solution in step (5) 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.

[0019] Furthermore, the acid in step (5) is 1 mol / L citric acid solution or 1 mol / L sodium citrate solution.

[0020] Furthermore, the ozone treatment in step (6) is performed by uniformly introducing ozone for 10 to 40 minutes, with an ozone flow rate of 20 to 200 L / h.

[0021] Furthermore, the amount of anhydrous ethanol added in step (7) is such that the material-liquid ratio is 1:8-12 and the ethanol concentration is 60%-80%.

[0022] Furthermore, the concentration in step (8) 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.

[0023] The second aspect of the present invention provides the use of the fig extract prepared by the method in cigarettes.

[0024] Furthermore, the application is: diluting the prepared fig extract with water or alcohol solution and then adding the diluted extract to shredded tobacco to prepare cigarettes.

[0025] This patent innovatively combines ozone, ionizing radiation, and pulsed light treatment for the extraction of fig extract, establishing an improved preparation method with high extraction efficiency, short reaction cycle, low impurities, and minimal organic solvent usage. This method is capable of producing a fig extract rich in aroma-producing substances. The extracted fig extract, when used in cigarettes, can enhance aroma concentration, sweetness, and comfort, while reducing cigarette irritation. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 Total ion current chromatogram of the hot reflux fig extract according to the embodiment of the present invention.

[0027] Figure 2 Total ion current chromatogram of fig extract in Example 4 of the present invention DETAILED DESCRIPTION

[0028] 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.

[0029] 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.

[0030] Example 1

[0031] (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.

[0032] (2) The dried figs in (1) were subjected to ionizing radiation treatment under the following reaction conditions: radiation dose of 4.0 Gy, radiation rate of 2.0 Gy / min, and radiation time of 30 s.

[0033] (3) The dried figs treated with ionizing radiation are promptly crushed into powder, and passed through a 60-mesh sieve to obtain fig powder.

[0034] (4) The fig powder in (3) 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 15min.

[0035] (5) 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.

[0036] 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 10,000 U / g, both of which are food grade.

[0037] (6) Ozone was introduced into the enzymatic hydrolysate in (5) at a constant rate of 80 L / h for 20 min.

[0038] (7) 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 refluxed for 60 minutes and filtered to obtain an extract.

[0039] (8) The extract of (7) was placed on a rotary evaporator and concentrated under reduced pressure to a relative density of 1.37 g / cm 3 The extract was stirred at a temperature of 50°C and a rotation speed of 50 rpm.

[0040] Example 2

[0041] (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.

[0042] (2) The dried figs in (1) were subjected to ionizing radiation treatment under the following reaction conditions: radiation dose of 3.0 Gy, radiation rate of 1.5 Gy / min, and radiation time of 25 s.

[0043] (3) The dried figs treated with ionizing radiation are promptly crushed into powder, and passed through a 60-mesh sieve to obtain fig powder.

[0044] (4) The fig powder in (3) was treated with pulsed light. The reaction conditions were: pulsed light intensity 5 J / m 2 , voltage is 3kV, pulse energy is 3J, pulse frequency is 4 times / s, and pulse light treatment time is 20min.

[0045] (5) 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 citric acid solution, stir evenly, and enzymolyze at 50 ° C for 3 h to obtain fig enzymatic hydrolyzate.

[0046] 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 10,000 U / g, both of which are food grade.

[0047] (6) Ozone was introduced into the enzymatic hydrolysate in (5) at a constant rate of 80 L / h for 20 min.

[0048] (7) 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.

[0049] (8) The extract of (7) was placed on a rotary evaporator and concentrated under reduced pressure to a relative density of 1.37 g / cm 3 The extract was stirred at a temperature of 50°C and a rotation speed of 50 rpm.

[0050] Example 3

[0051] (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.

[0052] (2) The dried figs in (1) were subjected to ionizing radiation treatment under the following reaction conditions: radiation dose of 3.0 Gy, radiation rate of 2.0 Gy / min, and radiation time of 30 s.

[0053] (3) The dried figs treated with ionizing radiation are promptly crushed into powder, and passed through a 60-mesh sieve to obtain fig powder.

[0054] (4) The fig powder in (3) was treated with pulsed light. The reaction conditions were: pulsed light intensity 5 J / m 2 , voltage is 3kV, pulse energy is 3J, pulse frequency is 5 times / s, and pulse light treatment time is 10min.

[0055] (5) 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 4.5 with 1 mol / L sodium citrate solution, stir evenly, and enzymolyze at 50 ° C for 3 h to obtain fig enzymatic hydrolyzate.

[0056] 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.

[0057] (6) Ozone was introduced into the enzymatic hydrolysate in (5) at a constant rate of 60 L / h for 15 min.

[0058] (7) Anhydrous ethanol was added to the ozone-treated enzymatic hydrolysate to make the final material-liquid ratio 1:10 and the ethanol concentration 75%, and then refluxed for 60 minutes and filtered to obtain an extract.

[0059] (8) The extract of (7) was placed on a rotary evaporator and concentrated under reduced pressure to a relative density of 1.37 g / cm 3 The extract was stirred at a temperature of 50°C and a rotation speed of 50 rpm.

[0060] Example 4

[0061] (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.

[0062] (2) The dried figs in (1) were subjected to ionizing radiation treatment under the following reaction conditions: radiation dose of 3.5 Gy, radiation rate of 1.5 Gy / min, and radiation time of 45 s.

[0063] (3) The dried figs treated with ionizing radiation are promptly crushed into powder, and passed through a 60-mesh sieve to obtain fig powder.

[0064] (4) The fig powder in (3) was treated with pulsed light. The reaction conditions were: pulsed light intensity 3 J / m 2 , voltage is 3kV, pulse energy is 3J, pulse frequency is 2 times / s, and pulse light treatment time is 20min.

[0065] (5) 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.

[0066] 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.

[0067] (6) Ozone was introduced into the enzymatic hydrolysate in (5) at a constant rate of 40 L / h for 15 min.

[0068] (7) Anhydrous ethanol was added to the ozone-treated enzymatic hydrolysate to make the final material-liquid ratio 1:9 and the ethanol concentration 70%, and then the mixture was refluxed for 60 minutes and filtered to obtain an extract.

[0069] (8) The extract of (7) was placed on a rotary evaporator and concentrated under reduced pressure to a relative density of 1.37 g / cm 3 The extract was stirred at a temperature of 50°C and a rotation speed of 50 rpm.

[0070] Example 5

[0071] (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.

[0072] (2) The dried figs in (1) were subjected to ionizing radiation treatment under the following reaction conditions: radiation dose of 5.0 Gy, radiation rate of 3.0 Gy / min, and radiation time of 40 s.

[0073] (3) The dried figs treated with ionizing radiation are promptly crushed into powder, and passed through a 60-mesh sieve to obtain fig powder.

[0074] (4) The fig powder in (3) was treated with pulsed light. The reaction conditions were: pulsed light intensity 5 J / m 2 , voltage is 2kV, pulse energy is 3J, pulse frequency is 4 times / s, and pulse light treatment time is 25min.

[0075] (5) 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.

[0076] The mixed enzyme solution is prepared by mixing pectinase and saccharifying enzyme in a mass ratio of 6:2, 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.

[0077] (6) Ozone was introduced into the enzymatic hydrolysate in (5) at a constant rate of 55 L / h for 30 min.

[0078] (7) Anhydrous ethanol was added to the ozone-treated enzymatic hydrolysate to make the final material-liquid ratio 1:8 and the ethanol concentration 75%, and then the mixture was refluxed for 60 minutes and filtered to obtain an extract.

[0079] (8) The extract of (7) was placed on a rotary evaporator and concentrated under reduced pressure to a relative density of 1.37 g / cm 3 The extract was stirred at a temperature of 50°C and a rotation speed of 50 rpm.

[0080] Comparative Example 1

[0081] (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.

[0082] (2) The dried figs in (1) were treated with pulsed light. The reaction conditions were: pulsed light intensity 5 J / m 2, voltage is 2kV, pulse energy is 3J, pulse frequency is 4 times / s, and pulse light treatment time is 25min.

[0083] (3) The dried figs treated with pulsed light were promptly crushed into powder and passed through a 60-mesh sieve to obtain fig powder.

[0084] (4) The fig powder was treated with ionizing radiation under the following conditions: radiation dose of 5.0 Gy, radiation rate of 3.0 Gy / min, and radiation time of 40 s.

[0085] (5) Take 200 g of ionizing irradiated fig powder, add distilled water 3 times the weight of the fig powder, then add 2% of the weight of the mixed enzyme solution, adjust the pH to 4.5 with 1 mol / L sodium citrate solution, stir evenly, and perform enzymolysis at 50°C for 3 h to obtain a fig enzymatic hydrolyzate.

[0086] The mixed enzyme solution is prepared by mixing pectinase and saccharifying enzyme in a mass ratio of 6:2, 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.

[0087] (6) Ozone was introduced into the enzymatic hydrolysate in (5) at a constant rate of 55 L / h for 30 min.

[0088] (7) Anhydrous ethanol was added to the ozone-treated enzymatic hydrolysate to make the final material-liquid ratio 1:8 and the ethanol concentration 75%, and then the mixture was refluxed for 60 minutes and filtered to obtain an extract.

[0089] (8) The extract of (7) was placed on a rotary evaporator and concentrated under reduced pressure to a relative density of 1.37 g / cm 3 The extract was stirred at a temperature of 50°C and a rotation speed of 50 rpm.

[0090] Comparative Example 2

[0091] (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.

[0092] (2) The dried figs in (1) were subjected to ionizing radiation treatment under the following reaction conditions: radiation dose of 5.0 Gy, radiation rate of 3.0 Gy / min, and radiation time of 40 s.

[0093] (3) The dried figs treated with ionizing radiation are promptly crushed into powder, and passed through a 60-mesh sieve to obtain fig powder.

[0094] (4) The fig powder in (3) was treated with pulsed light. The reaction conditions were: pulsed light intensity 5 J / m 2, voltage is 2kV, pulse energy is 3J, pulse frequency is 4 times / s, and pulse light treatment time is 25min.

[0095] (5) 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.

[0096] The mixed enzyme solution is prepared by mixing pectinase and saccharifying enzyme in a mass ratio of 6:2, 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.

[0097] (6) Anhydrous ethanol was added to the fig hydrolysate to make the final material-liquid ratio 1:8 and the ethanol concentration 75%, and then the mixture was refluxed for 60 minutes and filtered to obtain an extract.

[0098] (7) The extract was then introduced into ozone at a constant rate for 30 min, with an ozone flow rate of 55 L / h.

[0099] (8) The extract of (7) was placed on a rotary evaporator and concentrated under reduced pressure to an extract with a relative density of 1.37 g / cm3 at a temperature of 50°C and a rotation speed of 50 rpm.

[0100] 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 the control 2. The hot reflux method is 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.

[0101] Gas chromatography-mass spectrometry analysis was performed on Example 5, which had the best flavoring effect. The content of heat-sensitive flavor substances (2,3-dihydro-3,5-dihydroxy-6-methyl-4(H)-pyran-4-one, 5-hydroxymethylfurfural, and ethyl palmitate) 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 aldehydes, ketones, esters, and other substances (furfural, phenylacetaldehyde, 5-decanone, 2-methylbutyl propionate, etc.) also increased.

[0102] Table 1 Evaluation results

[0103]

[0104] Table 2 GC-MS analysis of hot reflux fig extract

[0105]

[0106]

[0107] Table 3 GC-MS analysis of Fig extract of Example 5

[0108]

[0109]

[0110]

Claims

1. An improved preparation method of fig extract, characterized in that: The following steps are involved: (1) Dry commercially available dried figs; (2) Treatment of dried figs with ionizing radiation; (3) Grinding the dried figs treated with ionizing radiation into powder in a timely manner, and passing through a 60-mesh sieve to obtain fig powder; (4) Pulsed light treatment of fig powder; (5) Take fig powder, add 3-4 times the mass of distilled water to the powder, then add 1-3% of the mass of the mixed enzyme solution to the powder, 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. (6) Adding ozone to the fig enzymatic hydrolysate; (7) Add anhydrous ethanol to the ozone-treated enzymatic hydrolysate, reflux for 30-120 min, and filter to obtain an extract; (8) Concentrate the extract to a relative density of 1.35~1.45g / cm 3 of the extract, The mixed enzyme solution in step (5) 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 improved preparation method of fig extract 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 improved preparation method of fig extract according to claim 1, characterized in that: The ionizing radiation in step (2) has a radiation dose of 1.0 to 5.0 Gy, a radiation rate of 0.5 to 3.0 Gy / min, and a radiation time of 20 to 60 seconds.

4. The improved preparation method of fig extract according to claim 1, characterized in that: The intensity of the pulsed light in step (4) is 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.

5. The improved preparation method of fig extract according to claim 1, characterized in that: The acid in step (5) is 1 mol / L citric acid solution or 1 mol / L sodium citrate solution.

6. The improved preparation method of fig extract according to claim 1, characterized in that: The ozone treatment in step (6) is to introduce ozone at a constant speed for 10 to 40 minutes, with an ozone flow rate of 20 to 200 L / h.

7. The improved preparation method of fig extract according to claim 1, characterized in that: The amount of anhydrous ethanol added in step (7) is such that the material-liquid ratio is 1:8-12 and the ethanol concentration is 60%-80%.

8. The improved preparation method of fig extract according to claim 1, characterized in that: The concentration in step (8) 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.

9. Use of the fig extract prepared by the method according to any one of claims 1 to 7 in cigarettes, the use comprising: diluting the prepared fig extract with water or an alcohol solution and then adding the diluted extract to shredded tobacco to prepare the cigarettes.

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