Preparation process and application of fresh and sweet herb fragrance prominent Maillard reaction spice

Abstract

The invention belongs to the technical field of tobacco flavors, and particularly relates to a preparation process and application of a fresh and sweet herb flavor prominent Maillard reaction flavor. The preparation method comprises the following steps: carrying out heating reflux extraction on fragments of tobacco leaves produced in Yunnan and fragments of lysimachia foenum-graecum hance to obtain an extract, mixing the extract, distilled water and compound amino acid, heating to obtain a Maillard reaction spice extract, carrying out supercritical carbon dioxide extraction on the Maillard reaction spice extract, combining extracts of two separation kettles, adding ethanol for dissolving, and carrying out vacuum drying to obtain the Maillard reaction spice. And freezing and separating the upper-layer ethanol solution to obtain the tobacco flavor with prominent fresh and sweet herb fragrance. Compared with independent lysimachia foenum-graecum hance absolute oil, Yunnan tobacco absolute oil and the tobacco flavor prepared by blending the lysimachia foenum-graecum hance absolute oil and the Yunnan tobacco absolute oil, the tobacco flavor prepared by the invention can better improve the harmony, richness, aroma quality and taste of smoke, reduce irritation and reduce offensive odor.

Description

Technical Field

[0001] The invention belongs to the technical field of tobacco flavors, and particularly relates to a preparation process and application of a sweet herbal flavor with a prominent Maillard reaction. Background Art

[0002] Lysimachia foenum-graecum Hance, also known as vanilla, perilla, and paicao, is a perennial herb of the Primulaceae family. The whole plant contains coumarin-like aromatic oil, which can be used to extract spices and used in the tobacco field. It has a characteristic herbal aroma. Yunnan tobacco leaves are unique in the tobacco market for their mellow and soft flavor, rich aroma, delicate taste, sweet aftertaste, and stable combustion performance, and are deeply loved by consumers.

[0003] In the prior art, there is no report on the use of tobacco leaves and angelica as raw materials to prepare Maillard reaction flavors and apply them in cigarettes. In addition, the Maillard reaction flavor absolute oil prepared by the present invention can significantly improve the harmony, richness, aroma quality, and taste of smoke, reduce irritation, and reduce impurities compared to the single angelica absolute oil, Yunyan absolute oil, and the tobacco flavor obtained by blending the two. Summary of the invention

[0004] The object of the present invention is to provide a preparation process and application of a sweet herbal fragrance with a prominent Maillard reaction flavor, so as to solve the problems mentioned in the above background technology.

[0005] To achieve the above objectives, this application is implemented through the following technical solutions:

[0006] A preparation process of a sweet herbal fragrance with a prominent Maillard reaction flavor, comprising the following steps:

[0007] S1, weighing a set mass of tobacco leaf fragments produced in Yunnan, angelica officinalis fragments and a solvent, adding them together into a distillation flask, heating and refluxing for a set time, filtering, and concentrating under reduced pressure to obtain an extract;

[0008] S2, mixing distilled water, composite amino acid, catalyst and the extract of step S1, reacting at a set temperature for a set time, cooling to room temperature, filtering, and concentrating under reduced pressure to obtain a Maillard reaction spice extract;

[0009] S3, putting the Maillard reaction spice extract obtained in the step into an extraction kettle and performing supercritical carbon dioxide extraction;

[0010] S4. Combine the extracts obtained from separation kettles I and II in step S3, add 10 times the mass of 95% ethanol to dissolve, stir and heat in a water bath for 30 minutes, separate the system into two layers, cool the upper ethanol solution to room temperature, centrifuge at -5°C, and filter to obtain tobacco flavor with a sweet herbal aroma.

[0011] Furthermore, in step S1, the mass ratio of the Yunnan tobacco leaf fragments to the Angelica dahurica fragments is 1:1 or 2:1.

[0012] Furthermore, in step S1, the solvent is an ethanol aqueous solution with a mass percentage of 60-95%, the added amount is 8-10 times the mass of the tobacco leaf fragments and the angelica fragments, the heating temperature is 50-100°C, the extraction time is 2-6 h, and during reduced pressure concentration, the temperature is 40-60°C and the vacuum pressure is 50-100 Pa.

[0013] Furthermore, in step S2, the amount of distilled water added is 0.5-2 times the mass of the extract in step S1.

[0014] Furthermore, in step S2, the composite amino acid is composed of proline, threonine, tryptophan and leucine, with a mass ratio of 1:1:1:1, and the added amount is 6%-10% of the mass of the added distilled water, and the catalyst is at least one of organic acids such as citric acid, tartaric acid, malic acid and sorbic acid, and the added amount is 2%-6% of the added distilled water. The reaction temperature is 60-100°C, the reaction time is 6-12h, and when concentrated under reduced pressure, the temperature is 40-60°C and the vacuum pressure is 50-100Pa.

[0015] Furthermore, in step S3, the pressure of supercritical carbon dioxide extraction is 20-30MPa, the extraction temperature is 40-50°C, the carbon dioxide flow rate is 80 L / h, the pressure of separation kettle I is 6-8Mpa, the temperature is 50-60°C, the pressure of separation kettle II is 4-6Mpa, the temperature is 30-50°C, and the extraction time is 2-3 h.

[0016] Furthermore, in step S4, the water bath temperature is 80° C., and the timing is 30 min starting from the slightly boiling state.

[0017] An application, using any of the above-mentioned sweet herbal aroma and Maillard reaction spices in cigarettes.

[0018] Furthermore, the sweet herbal aroma Maillard reaction spices are added in an amount of 20-60 ppm in the cut tobacco.

[0019] The beneficial effects of the present invention are:

[0020] (1) The present invention uses tobacco leaf fragments produced in Yunnan and angelica officinalis fragments as raw materials, and develops a new process for natural fragrances with harmonious aroma through the combination of "solvent extraction + Maillard reaction + supercritical extraction + frozen alcohol precipitation". The process conditions are continuously optimized to obtain tobacco oil with distinct sensory characteristics and clear functional orientation.

[0021] (2) Organic acid is used to catalyze the Maillard reaction between amino acids and reducing sugars in the extract to generate nitrogen-containing heterocyclic compounds, cyclic enol one compounds, carbonyl compounds, Amadori compounds and Heyns compounds, thereby increasing the content of aroma compounds and aroma precursors.

[0022] (3) The catalyst used is also tobacco flavoring. After the Maillard reaction is completed, no treatment is required, which has the advantages of being green, environmentally friendly and easy to operate.

[0023] (4) Extraction with supercritical carbon dioxide better retains the characteristic aroma of Yunnan tobacco and angelica sinensis, with high extraction efficiency and no solvent residue.

[0024] (5) Through cryo-alcohol precipitation, the wax components in the supercritical extraction extract can be removed, and the aroma components, tobacco sterols and other volatile components can be effectively enriched, which can significantly improve the sensory effect of the extract and enhance the quality of cigarettes.

[0025] (6) Compared with the single angelica absolute oil, the Yunyan absolute oil and the tobacco flavoring obtained by blending the two, the tobacco flavoring prepared by the present invention can better improve the harmony, richness, aroma quality and taste of the smoke, reduce irritation and reduce impurities. DETAILED DESCRIPTION

[0026] The technical solution of the present invention is described in detail below through examples. The following examples are merely exemplary and can only be used to explain and illustrate the technical solution of the present invention, but cannot be construed as limiting the technical solution of the present invention.

[0027] Example 1

[0028] 1. Weigh 50g of 2020 Yunnan Kunming DCJ14 fragments, 25g of Guangxi Lingxiangcao and 600g of 95% ethanol in turn, add them into a distillation bottle, and reflux extract at 85℃ for 6 h. After the extraction, cool and filter, and concentrate the filtrate under reduced pressure at 40℃ and 80Pa to obtain an extract.

[0029] 2. Take 12g of the obtained extract, add 12g of distilled water, 0.18g of proline, 0.18g of threonine, 0.18g of leucine and 0.18g of tryptophan, then add 0.12g of citric acid and 0.12g of malic acid, react at 95°C for 8 h, cool and filter after the reaction, and concentrate the filtrate under reduced pressure at 40°C and 80Pa to obtain the Maillard reaction spice extract.

[0030] 3. The obtained Maillard reaction spice extract was placed in an extraction kettle for supercritical carbon dioxide extraction. The main parameters were: extraction pressure 20 MPa, extraction temperature 45°C, separation kettle pressure 7 MPa, separation temperature 60°C, separation kettle II pressure 5 MPa, separation temperature 30°C, and extraction time 2.5 h. After the extraction, the extracts from separation kettles I and II were combined.

[0031] 4. Combine the extracts obtained from separation kettles I and II, add 10 times the mass of 95% ethanol to dissolve, heat with stirring in a water bath for 30 min, centrifuge at -5°C, and filter to obtain tobacco oil with a sweet herbal aroma.

[0032] The tobacco oil was diluted with 2 times the amount of propylene glycol, added to the tobacco at an addition amount of 80ppm, and placed in a constant temperature and humidity environment with a humidity of 55% and a temperature of 25°C for 48 hours. The sensory evaluation showed that it had a distinctive sweet and herbal aroma, and the aroma was harmonious, the aroma quality was high, and the aftertaste was sweet and comfortable.

[0033] Example 2

[0034] 1. Weigh 50g of 2021 Yunnan Kunming CJ34 fragments, 50g of Guangxi Lingxiangcao and 800g of 95% ethanol in turn, add them into a distillation bottle, and reflux extract at 85℃ for 6 h. After the extraction, cool and filter, and concentrate the filtrate under reduced pressure at 40℃ and 100Pa to obtain an extract.

[0035] 2. Take 15g of the obtained extract, add 30g of distilled water, 0.45g of proline, 0.45g of threonine, 0.45g of leucine and 0.45g of tryptophan, then add 0.3g of citric acid and 0.3g of sorbic acid, react at 95°C for 8 h, cool and filter after the reaction, and concentrate the filtrate under reduced pressure at 40°C and 80Pa to obtain the Maillard reaction spice extract.

[0036] 3. The obtained Maillard reaction spice extract was placed in an extraction kettle for supercritical carbon dioxide extraction. The main parameters were: extraction pressure 30 MPa, extraction temperature 45°C, separation kettle pressure 7 MPa, separation temperature 60°C, separation kettle II pressure 5 MPa, separation temperature 30°C, and extraction time 2.5 h. After the extraction, the extracts from separation kettles I and II were combined.

[0037] 4. Combine the extracts obtained from separation kettles I and II, add 10 times the mass of 95% ethanol to dissolve, heat with stirring in a water bath for 30 min, centrifuge at -5°C, and filter to obtain tobacco oil with a sweet herbal aroma.

[0038] The tobacco oil was diluted with 2 times the amount of propylene glycol, added to the tobacco at an addition amount of 100ppm, and placed in a constant temperature and humidity environment with a humidity of 55% and a temperature of 25°C for 48 hours. The sensory evaluation showed that it had a distinctive sweet and herbal aroma, and the aroma was harmonious, the aroma quality was high, and the aftertaste was sweet and comfortable.

[0039] Example 3

[0040] 1. Weigh 50g of 2020 Yunnan Kunming DCJ59 fragments, 25g of Guangxi Lingxiangcao and 750g of 95% ethanol in turn, add them into a distillation bottle, and reflux extract at 85℃ for 6 h. After the extraction, cool and filter, and concentrate the filtrate under reduced pressure at 40℃ and 100Pa to obtain an extract.

[0041] 2. Take 12g of the obtained extract, add 24g of distilled water, 0.6g of proline, 0.6g of threonine, 0.6g of leucine and 0.6g of tryptophan, and then add 0.48g of tartaric acid, react at 95°C for 8 h, cool and filter after the reaction, and concentrate the filtrate under reduced pressure at 40°C and 100Pa to obtain the Maillard reaction spice extract.

[0042] 3. The obtained Maillard reaction spice extract was placed in an extraction kettle for supercritical carbon dioxide extraction. The main parameters were: extraction pressure 25 MPa, extraction temperature 45°C, separation kettle pressure 7 MPa, separation temperature 60°C, separation kettle II pressure 5 MPa, separation temperature 30°C, and extraction time 2.5 h. After the extraction, the extracts from separation kettles I and II were combined.

[0043] 4. Combine the extracts obtained from separation kettles I and II, add 10 times the mass of 95% ethanol to dissolve, heat with stirring in a water bath for 30 min, centrifuge at -5°C, and filter to obtain tobacco oil with a sweet herbal aroma.

[0044] The tobacco oil was diluted with 2 times the amount of propylene glycol, added to the tobacco at an addition amount of 70ppm, and placed in a constant temperature and humidity environment with a humidity of 55% and a temperature of 25°C for 48 hours. The sensory evaluation showed that it had a distinctive sweet and herbal aroma, and the aroma was harmonious, the aroma quality was high, and the aftertaste was sweet and comfortable.

[0045] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Any equivalent changes or modifications made according to the essence of the present invention should be included in the protection scope of the present invention.

Claims

1. A process for preparing a sweet herbal fragrance with a prominent Maillard reaction flavor, characterized in that: The following steps are involved: S1, weighing a set mass of tobacco leaf fragments produced in Yunnan, angelica officinalis fragments and a solvent, adding them together into a distillation flask, heating and refluxing for a set time, filtering, and concentrating under reduced pressure to obtain an extract; S2, mixing distilled water, composite amino acid, catalyst and the extract of step S1, reacting at a set temperature for a set time, cooling to room temperature, filtering, and concentrating under reduced pressure to obtain a Maillard reaction spice extract; S3, putting the Maillard reaction spice extract obtained in the step into an extraction kettle and performing supercritical carbon dioxide extraction; S4. Combine the extracts obtained from separation kettles I and II in step S3, add 10 times the mass of 95% ethanol to dissolve, stir and heat in a water bath for 30 minutes, separate the system into two layers, cool the upper ethanol solution to room temperature, centrifuge at -5°C, and filter to obtain tobacco flavor with a sweet herbal aroma.

2. The process for preparing the sweet herbal aroma Maillard reaction fragrance according to claim 1, characterized in that: In step S1, the mass ratio of the Yunnan tobacco leaf fragments to the Angelica dahurica fragments is 1:1 or 2:

1.

3. The process for preparing the sweet herbal aroma Maillard reaction fragrance according to claim 1, characterized in that: In step S1, the solvent is an ethanol aqueous solution with a mass percentage of 60-95%, the added amount is 8-10 times the mass of the tobacco leaf fragments and the angelica fragments, the heating temperature is 50-100°C, the extraction time is 2-6 h, and during reduced pressure concentration, the temperature is 40-60°C and the vacuum pressure is 50-100Pa.

4. The process for preparing the sweet herbal aroma Maillard reaction fragrance according to claim 1, characterized in that: In step S2, the amount of distilled water added is 0.5-2 times the mass of the extract in step S1.

5. The process for preparing the sweet herbal aroma Maillard reaction flavor according to claim 1, characterized in that: In step S2, the composite amino acid is composed of proline, threonine, tryptophan and leucine, with a mass ratio of 1:1:1:1, and the added amount is 6%-10% of the mass of the added distilled water, and the catalyst is at least one of citric acid, tartaric acid, malic acid and sorbic acid, and the added amount is 2%-6% of the added distilled water. The reaction temperature is 60-100°C, the reaction time is 6-12h, and the temperature is 40-60°C and the vacuum pressure is 50-100Pa during reduced pressure concentration.

6. The process for preparing the sweet herbal aroma Maillard reaction flavor according to claim 1, characterized in that: In step S3, the pressure of supercritical carbon dioxide extraction is 20-30MPa, the extraction temperature is 40-50°C, the carbon dioxide flow rate is 80L / h, the pressure of separation kettle I is 6-8Mpa, the temperature is 50-60°C, the pressure of separation kettle II is 4-6Mpa, the temperature is 30-50°C, and the extraction time is 2-3 h.

7. The process for preparing the sweet herbal aroma Maillard reaction flavor according to claim 1, characterized in that: In step S4, the water bath temperature is 80°C, and the timing is 30 minutes starting from the slightly boiling state.

8. An application, characterized in that, Use of the sweet herbal aroma and Maillard reaction flavor prepared according to any one of claims 1 to 7 in cigarettes.

9. The use according to claim 8, characterized in that: The sweet herbal aroma and the Maillard reaction spices are added in an amount of 20-60ppm in the tobacco.