A method for the preparation of a fig extract using ionizing radiation

Abstract

The present application relates to a method for preparing fig extract by ionizing radiation, which innovatively uses ionizing radiation for extracting fig extract, is beneficial to improving the yield and quality of the extract, and reducing the volatilization of heat-sensitive flavor components. The present application establishes a method for preparing fig extract with high extraction efficiency, low impurities, short reaction period and less use of organic solvents, which can prepare fig extract with high aroma-producing substances, and when added to cigarettes, has the advantages of increasing aroma concentration, improving sweet and smooth feeling, reducing cigarette irritation, and improving comfort.

Description

Technical Field

[0001] This invention belongs to the field of tobacco flavoring technology, and particularly relates to a method for preparing fig extract using ionizing radiation. This invention also relates to the application of the tobacco flavoring in cigarettes. Background Technology

[0002] Traditional methods for preparing plant extracts include water extraction and alcohol extraction. Although these methods are simple, easy to operate, and inexpensive, they involve long reaction cycles, high solvent consumption, and the aroma components cannot be effectively enriched, resulting in low quality. Newer technologies, such as molecular distillation and supercritical fluid extraction, require smaller investments, have higher operating costs, lower yields, and lower efficiency.

[0003] The fig is a deciduous shrub or small tree belonging to the genus Ficus in the family Moraceae. It is also known as the fig, the sun-reflecting fruit, etc. The fig has a thin, soft skin, tender and sweet flesh, and is rich in nutrients. It is considered a plant with both edible and medicinal value, possessing not only edible properties but also high medicinal value. It is believed to have stomach-strengthening, intestinal-cleansing, swelling-reducing, and detoxifying effects, and is mainly used for symptoms such as loss of appetite, sore throat, and cough with phlegm.

[0004] In the field of tobacco production technology, figs are mainly used to prepare extracts for flavoring cigarettes. Fig extract is one of the earliest traditional flavoring raw materials used in cigarettes, possessing characteristic aromas such as sweetness, fruitiness, and tobacco. It is an important flavoring agent used to blend sweet and savory notes in tobacco flavorings. Summary of the Invention

[0005] This invention addresses the problems of long reaction cycles, high solvent consumption, and low aroma components in existing fig extract extraction processes. It provides a highly efficient method for preparing fig extract, which innovatively uses ionizing radiation for fig extract extraction, thereby improving the yield and quality of the extract and reducing the volatilization of heat-sensitive aroma components.

[0006] The objective of this invention is achieved through the following technical solution:

[0007] The first aspect of this invention provides a method for preparing fig extract using ionizing radiation, comprising the following steps:

[0008] (1) Dry commercially available dried figs;

[0009] (2) The dried figs are promptly crushed into powder and passed through a 60-mesh sieve to obtain fig powder;

[0010] (3) Take fig powder, add 3 to 4 times the weight of fig powder in distilled water, then add 1 to 3% of the weight of fig in mixed enzyme solution, adjust the pH to 4.5 to 5.5 with acid, stir evenly, and enzymatically hydrolyze at 50°C for 2 to 4 hours to obtain fig enzymatic hydrolysate.

[0011] (4) Add anhydrous ethanol to the fig enzymatic hydrolysate to obtain a mixture;

[0012] (5) The mixture is subjected to ionizing radiation treatment and filtered to obtain the extract;

[0013] (6) Concentrate the extract to a relative density of 1.35–1.45 g / cm³. 3 Extract of .

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

[0015] Furthermore, the mixed enzyme solution in step (3) is composed of 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.

[0016] Furthermore, the acid in step (3) is a 1 mol / L citric acid solution or a 1 mol / L sodium citrate solution.

[0017] Further, the amount of anhydrous ethanol added in step (4) is such that the material-to-liquid ratio is 1:8 to 12 and the ethanol concentration is 60% to 80%.

[0018] Furthermore, in step (5), the radiation dose is 1.0–5.0 Gy, the radiation rate is 0.5–3.0 Gy / min, and the radiation time is 20–60 s.

[0019] Furthermore, the concentration described in step (6) is carried out under reduced pressure on a rotary evaporator at a temperature of 45–60°C and a rotation speed of 45–65 rpm.

[0020] A second aspect of the present invention provides the application of the fig extract prepared by the method in cigarettes.

[0021] Furthermore, the application method is as follows: the prepared fig extract is diluted with water or alcohol solution and then added to tobacco to make cigarettes.

[0022] The present invention achieves the following technical effects:

[0023] This invention innovatively utilizes ionizing radiation for the extraction of fig extract, which improves the yield and quality of the extract and reduces the volatilization of heat-sensitive aroma components. This invention establishes a method for preparing fig extract with high extraction efficiency, short reaction cycle, low impurities, and low solvent consumption. This method can prepare fig extract with high aroma content. When applied to cigarettes, it can significantly increase the aroma concentration, enhance the sweetness and smoothness of cigarettes, reduce irritation, and improve comfort. Attached Figure Description

[0024] Figure 1 Total ion chromatogram of hot reflux fig extract according to an embodiment of the present invention.

[0025] Figure 2 Example 5 of the present invention: Total ion current chromatogram of fig extract subjected to ionizing radiation. Detailed Implementation

[0026] To better understand the above-mentioned objectives, features, and advantages of the present invention, the present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments. It should be noted that, unless otherwise specified, the embodiments of the present invention and the features thereof can be combined with each other.

[0027] Many specific details are set forth in the following description in order to provide a full understanding of the invention. However, the invention may also be practiced in other ways different from those described herein, and therefore the scope of protection of the invention is not limited to the specific embodiments disclosed below.

[0028] Example 1

[0029] (1) Dry commercially available dried figs at 80℃ for 12 hours to promote the Maillard reaction of proteins and sugars in figs at high temperature.

[0030] (2) The dried figs are promptly crushed into powder and passed through a 60-mesh sieve to obtain fig powder.

[0031] (3) Take 200g of fig powder, add 3 times the weight of the fig powder in distilled water, then add 1% of the weight of the fig in mixed enzyme solution, adjust the pH to 4.5 with 1mol / L sodium citrate solution, stir evenly, and enzymatically hydrolyze at 50℃ for 2h to obtain fig enzymatic hydrolysate.

[0032] The mixed enzyme solution is composed 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, both of which are food grade.

[0033] (4) Add anhydrous ethanol to the fig enzymatic hydrolysate to make the final material-to-liquid ratio 1:8 and the ethanol concentration 80% to obtain a mixed solution.

[0034] (5) The mixture was subjected to ionizing radiation treatment under the following conditions: radiation dose of 1.0 Gy, radiation rate of 1.5 Gy / min, and radiation time of 60 s. The mixture was then filtered to obtain the extract.

[0035] (6) The extract was concentrated under reduced pressure in a rotary evaporator to a relative density of 1.35 g / cm³. 3 The extract was prepared at a temperature of 50°C and a rotation speed of 45 rpm.

[0036] Example 2

[0037] (1) Dry commercially available dried figs at 80℃ for 12 hours to promote the Maillard reaction of proteins and sugars in figs at high temperature.

[0038] (2) The dried figs are promptly crushed into powder and passed through a 60-mesh sieve to obtain fig powder.

[0039] (3) Take 200g of fig powder, add 4 times the weight of the fig powder in distilled water, then add 2% of the weight of the fig in mixed enzyme solution, adjust the pH to 5.0 with 1mol / L citric acid solution, stir evenly, and enzymatically hydrolyze at 50℃ for 3h to obtain fig enzymatic hydrolysate.

[0040] The mixed enzyme solution is composed 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, both of which are food grade.

[0041] (4) Add anhydrous ethanol to the fig enzymatic hydrolysate to make the final material-to-liquid ratio 1:10 and the ethanol concentration 75% to obtain a mixed solution.

[0042] (5) The mixture was subjected to ionizing radiation treatment under the following conditions: radiation dose of 2.5 Gy, radiation rate of 1.0 Gy / min, and radiation time of 30 s. The mixture was then filtered to obtain the extract.

[0043] (6) The extract was concentrated under reduced pressure in a rotary evaporator to a relative density of 1.37 g / cm³. 3 The extract was prepared at a temperature of 55°C and a rotation speed of 55 rpm.

[0044] Example 3

[0045] (1) Dry commercially available dried figs at 80℃ for 12 hours to promote the Maillard reaction of proteins and sugars in figs at high temperature.

[0046] (2) The dried figs are promptly crushed into powder and passed through a 60-mesh sieve to obtain fig powder.

[0047] (3) Take 200g of fig powder, add 4 times the weight of the fig powder in distilled water, then add 2% of the weight of the fig in mixed enzyme solution, adjust the pH to 5.5 with 1mol / L sodium citrate solution, stir evenly, and enzymatically hydrolyze at 50℃ for 3h to obtain fig enzymatic hydrolysate.

[0048] The mixed enzyme solution is composed 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, both of which are food grade.

[0049] (4) Add anhydrous ethanol to the fig enzymatic hydrolysate to make the final material-to-liquid ratio 1:9 and the ethanol concentration 70% to obtain a mixed solution.

[0050] (5) The mixture was subjected to ionizing radiation treatment under the following conditions: radiation dose of 3.0 Gy, radiation rate of 2.5 Gy / min, and radiation time of 40 s. The mixture was then filtered to obtain the extract.

[0051] (6) The extract was concentrated under reduced pressure using a rotary evaporator to a relative density of 1.41 g / cm³. 3 The extract was prepared at a temperature of 60°C and a rotation speed of 50 rpm.

[0052] Example 4

[0053] (1) Dry commercially available dried figs at 80℃ for 12 hours to promote the Maillard reaction of proteins and sugars in figs at high temperature.

[0054] (2) The dried figs are promptly crushed into powder and passed through a 60-mesh sieve to obtain fig powder.

[0055] (3) Take 200g of fig powder, add 4 times the weight of the fig powder in distilled water, then add 1% of the weight of the fig in mixed enzyme solution, adjust the pH to 5.0 with 1mol / L sodium citrate solution, stir evenly, and enzymatically hydrolyze at 50℃ for 3h to obtain fig enzymatic hydrolysate.

[0056] The mixed enzyme solution is composed of pectinase and saccharifying enzyme in a mass ratio of 8:1, 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.

[0057] (4) Add anhydrous ethanol to the fig enzymatic hydrolysate to make the final material-to-liquid ratio 1:8 and the ethanol concentration 75% to obtain a mixed solution.

[0058] (5) The mixture was subjected to ionizing radiation treatment under the following conditions: radiation dose of 3.0 Gy, radiation rate of 1.0 Gy / min, and radiation time of 25 s. The mixture was then filtered to obtain the extract.

[0059] (6) The extract was concentrated under reduced pressure in a rotary evaporator to a relative density of 1.39 g / cm³. 3 The extract was prepared at a temperature of 55°C and a rotation speed of 50 rpm.

[0060] Example 5

[0061] (1) Dry commercially available dried figs at 80℃ for 12 hours to promote the Maillard reaction of proteins and sugars in figs at high temperature.

[0062] (2) The dried figs are promptly crushed into powder and passed through a 60-mesh sieve to obtain fig powder.

[0063] (3) Take 200g of fig powder, add 3 times the weight of the fig powder in distilled water, then add 2% of the weight of the fig in mixed enzyme solution, adjust the pH to 5.0 with 1mol / L citric acid solution, stir evenly, and enzymatically hydrolyze at 50℃ for 2h to obtain fig enzymatic hydrolysate.

[0064] The mixed enzyme solution is composed 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, both of which are food grade.

[0065] (4) Add anhydrous ethanol to the fig enzymatic hydrolysate to make the final material-to-liquid ratio 1:10 and the ethanol concentration 80% to obtain a mixed solution.

[0066] (5) The mixture was subjected to ionizing radiation treatment under the following conditions: radiation dose of 3.5 Gy, radiation rate of 2.5 Gy / min, and radiation time of 45 s. The mixture was then filtered to obtain the extract.

[0067] (6) The extract was concentrated under reduced pressure using a rotary evaporator to a relative density of 1.43 g / cm³. 3 The extract was prepared at a temperature of 60°C and a rotation speed of 50 rpm.

[0068] Comparative Example 1

[0069] (1) Dry commercially available dried figs at 80℃ for 12 hours to promote the Maillard reaction of proteins and sugars in figs at high temperature.

[0070] (2) The dried figs are promptly crushed into powder and passed through a 60-mesh sieve to obtain fig powder.

[0071] (3) The fig powder was subjected to ionizing radiation treatment with a radiation dose of 3.5 Gy, a radiation rate of 2.5 Gy / min, and a radiation time of 45 s.

[0072] (4) Take 200g of ionized fig powder, add 3 times the weight of the fig powder in distilled water, then add 2% of the weight of the fig in mixed enzyme solution, adjust the pH to 5.0 with 1mol / L citric acid solution, stir evenly, and enzymatically hydrolyze at 50℃ for 2h to obtain fig enzymatic hydrolysate.

[0073] The mixed enzyme solution is composed 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, both of which are food grade.

[0074] (4) Add anhydrous ethanol to the fig enzymatic hydrolysate to make the final material-to-liquid ratio 1:10 and the ethanol concentration 80% to obtain a mixed solution.

[0075] (5) Filter the mixture to obtain the extract.

[0076] (6) The extract was concentrated under reduced pressure in a rotary evaporator to a relative density of 1.43 g / cm³. 3 The extract was prepared at a temperature of 60°C and a rotation speed of 50 rpm.

[0077] Comparative Example 2

[0078] (1) Dry commercially available dried figs at 80℃ for 12 hours to promote the Maillard reaction of proteins and sugars in figs at high temperature.

[0079] (2) The dried figs are promptly crushed into powder and passed through a 60-mesh sieve to obtain fig powder.

[0080] (3) Take 200g of fig powder, add 3 times the weight of the fig powder in distilled water, then add 2% of the weight of the fig in mixed enzyme solution, adjust the pH to 5.0 with 1mol / L citric acid solution, stir evenly, and enzymatically hydrolyze at 50℃ for 2h to obtain fig enzymatic hydrolysate.

[0081] The mixed enzyme solution is composed of pectinase and saccharifying enzyme in a 1:1 mass ratio, 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.

[0082] (4) Add anhydrous ethanol to the fig enzymatic hydrolysate to make the final material-to-liquid ratio 1:6 and the ethanol concentration 50% to obtain a mixed solution.

[0083] (5) The mixture was subjected to ionizing radiation treatment under the following conditions: radiation dose of 3.5 Gy, radiation rate of 2.5 Gy / min, and radiation time of 45 s. The mixture was then filtered to obtain the extract.

[0084] (6) The extract after ionizing radiation treatment was concentrated under reduced pressure in a rotary evaporator to a relative density of 1.43 g / cm³. 3 The extract was prepared at a temperature of 60°C and a rotation speed of 50 rpm.

[0085] The fig extracts described in Examples 1-5 and Comparative Examples 1-2 were added to the test tobacco of the Jin Sheng (Tengwang Pavilion) series of cigarettes to produce cigarettes. Cigarettes were then evaluated by five provincial-level cigarette tasters according to the common cigarette industry evaluation method YC / T497-2014_Sensory Evaluation Method for Chinese-style Cigarettes. Each indicator was scored out of 10, with higher satisfaction scores receiving higher marks. The average score given by the five provincial-level tasters 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 prepared as control (2). The hot reflux method involved placing fig powder treated in the same way as in the examples into a reflux evaporator, adding 1:10 ethanol, and refluxing for 120 minutes to obtain an extract. The extract was then concentrated under reduced pressure in a rotary evaporator to a relative density of 1.42 g / cm³. 3 The extract. The absorption results are shown in Table 1.

[0086] Gas chromatography-mass spectrometry analysis was performed on Example 5, which showed the best fragrance effect. The content of heat-sensitive fragrance substances (5-hydroxymethylfurfural, phytone, etc.) in the volatile fragrance components of the fig extract obtained after ionizing radiation treatment was higher than that of the fig extract obtained by hot reflux method. The types of aldehydes, ketones, esters, etc. (gemmaconone, curcumin, methyl linoleate, ethyl oleate, etc.) also increased.

[0087] Table 1. Evaluation Results

[0088]

[0089] Table 2 GC-MS analysis of hot-refluxed fig extract

[0090]

[0091]

[0092]

[0093] Table 3. GC-MS analysis of fig extract treated with ionizing radiation in Example 5.

[0094]

[0095]

[0096]

Claims

1. A method for preparing fig extract using ionizing radiation, characterized in that, Includes the following steps: (1) Dry commercially available dried figs; (2) The dried figs are promptly crushed into powder and passed through a 60-mesh sieve to obtain fig powder; (3) Take fig powder, add 3 times the weight of fig powder in distilled water, then add 2% of the weight of fig in mixed enzyme solution, adjust the pH to 5.0 with acid, stir evenly, and enzymatically hydrolyze at 50℃ for 2 hours to obtain fig enzymatic hydrolysate. (4) Add anhydrous ethanol to the fig enzymatic hydrolysate to obtain a mixture; (5) The mixture is subjected to ionizing radiation treatment and filtered to obtain the extract; (6) Concentrate the extract to a relative density of 1.43 g / cm³. 3 Extract; The drying mentioned in step (1) refers to drying at 80℃ for 12 hours; The mixed enzyme solution in step (3) is made 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 20,000 U / g, both of which are food grade; The acid mentioned in step (3) is a 1 mol / L citric acid solution; The amount of anhydrous ethanol added in step (4) is such that the material-to-liquid ratio is 1:10 and the ethanol concentration is 80%. Step (5) The radiation dose is 3.5 Gy, the radiation rate is 2.5 Gy / min, and the radiation time is 45 s; The concentration described in step (6) is carried out under reduced pressure on a rotary evaporator at a temperature of 60°C and a rotation speed of 50 rpm.

2. The application of the fig extract prepared by the method of claim 1 in cigarettes.

3. The application according to claim 2, characterized in that, The application method is as follows: the prepared fig extract is diluted with water or alcohol solution and then added to tobacco to make cigarettes.

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