CN108851173A - A kind of cigarette preparation method of mango fragrance and the application in cigarette - Google Patents

Abstract

The invention provides a preparation method of mango flavor for cigarettes: fresh ripe mangoes are dried, crushed and sieved, heated and extracted with ethanol, filtered, and concentrated to obtain mango extract; the mango extract is dissolved in ethanol, and macromolecules are removed by ceramic microfiltration membrane filtration. Substances: the permeated liquid of the microfiltration membrane is filtered by an organic ultrafiltration membrane to remove the filtered part of small molecular substances that affect the aroma and taste, and the intercepted part of the organic ultrafiltration membrane is distilled and concentrated under reduced pressure to obtain mango flavor. The invention also provides the application of the fragrance in cigarettes: the mango fragrance for tobacco is diluted with a non-toxic and non-irritating organic solvent, and sprayed in a certain proportion on shredded tobacco to make a cigarette. Adding this spice can significantly increase the amount of aroma, the fruity sweetness is prominent, the aroma is harmonious, the sweetness is increased, and the irritation and miscellaneous gas can be reduced, making the smoke soft and pleasant aftertaste.

Description

A kind of preparation method of mango flavor for tobacco and its application in cigarette

technical field

The invention belongs to the technical field of preparation of tobacco additives, and in particular relates to a preparation method of tobacco mango spice and its application in cigarettes.

technical background

As a fruit familiar to people, mango is rich in vitamins and amino acids. It is sweet and delicious, and the fresh fruit has a strong fragrance. Wei Changbin and others used headspace solid-phase microextraction to extract volatile components in mango, and carried out gas chromatography-mass spectrometry analysis and identification. The results showed that the volatile components in mango were mainly terpene compounds, such as α-terpinolene and δ-3-carene, and many of these volatile components were important components of natural flavors. There are few reports on the application of mango products in cigarette flavoring.

Natural flavor components extracted by conventional extraction methods, such as Soxhlet extraction, inevitably contain impurities such as protein, starch, wax, etc., which not only affect the quality of natural flavors, but also affect the flavoring effect of cigarettes. It has a certain impact on the safety of cigarette smoking.

Membrane separation technology refers to the technology that achieves selective separation of a mixture of molecules with different particle sizes at the molecular level when they pass through a semi-permeable membrane. Membrane separation technology can effectively remove macromolecular substances that have a negative impact on the sensory quality of smoke while retaining the original characteristic aroma of the extract, so as to improve the quality of the extract. However, there is no use of membrane separation technology to separate mango extract to prepare tobacco flavor.

Membrane separation technology is used to separate and purify the prepared mango extract, which can remove impurities such as protein, starch, wax, etc. in the extract. At the same time, through ultrafiltration or nanofiltration membrane separation and interception, some small molecular substances that affect the fragrance can also be removed , to obtain refined natural flavor components, which is expected to provide a new method for the utilization of natural flavors and open up a new way for cigarette flavoring.

Contents of the invention

The purpose of the present invention is to provide a method for preparing tobacco mango flavor with obvious flavoring effect and less impurities in view of the shortcomings of the existing tobacco flavor, especially the preparation method of mango tobacco flavor. The present invention is achieved through the following technical solutions:

In order to achieve the above object, the invention provides a method for preparing tobacco mango spice, which comprises the following steps:

(1) Drying: Take fresh ripe mangoes, peel them, cut them into uniform slices, place them in an oven, and dry them at 50°C for 12 hours;

(2) Pulverization: take the dried mango slices, beat them into coarse powder with a pulverizer, and pass through a 10-mesh stainless steel screen;

(3) Extraction: Accurately weigh the mango powder, wrap it with filter paper and put it into a Soxhlet extractor, add 3-10 times the amount of 50%-100% ethanol, heat at 50-90°C, and heat to reflux for 1-2.5h. Filter and distill the filtrate under reduced pressure until no ethanol flows out to obtain mango extract.

(4) Microfiltration membrane separation: Weigh the mango extract and place it in a quantitative glass container, add 50 times the amount of 20% ethanol to dissolve, and the dissolved solution is N1. After the dissolution is complete, use a 50-200nm ceramic microfiltration membrane to filter, and the cut-off section is N2;

(5)) Ultrafiltration membrane separation: microfiltration membrane permeate liquid 10-500kd organic membrane filtration, the interception section is recorded as N3, and the permeation section is recorded as N4.

(6) Take the N3 part and distill it under reduced pressure to a relative density of 1.05-1.15 to obtain mango flavor.

The fresh ripe mangoes include mangoes produced in Guangxi, Yunnan, Guangdong, Fujian and Taiwan; mangoes produced in India, Bangladesh, Indochina Peninsula and Malaysia, and one or more of all cultivated mangoes.

Further, in step (3), the amount of ethanol added is preferably 5-8 times, more preferably 5-6 times; the ethanol concentration is preferably 70-95%, more preferably 85-90%; the heating temperature is preferably 65 -85°C, more preferably 75-80°C;

Further, in step (4), the microfiltration membrane pore size is preferably 50nm;

Further, in step (5), the ultrafiltration membrane pore size is preferably 20-200KD, more preferably 50-100KD;

The application of a kind of mango flavor for cigarettes according to the present invention: dilute the mango flavor for cigarettes with a non-toxic and non-irritating organic solvent, and the dilution factor is 10-100 times; The mango spice is sprayed on shredded tobacco according to the mass ratio of 0.02%-1%, and rolled into cigarettes.

Further, for the application of the mango spice for tobacco, the dilution factor of the organic solvent is optimized to be 20-70 times, and further optimized to be 40-50 times; %.

Further, the organic solvent is ethanol, propylene glycol, sorbitol, xylitol or glycerin, or a mixture of any two or more thereof.

The application effect of the mango flavor for tobacco in cigarettes according to the present invention is characterized in that, after the mango flavor prepared is added to the cigarette, the amount of aroma can be significantly increased, the fruity sweetness is prominent, the aroma is harmonious, the sweetness is increased, and It can reduce irritation and miscellaneous gas, making the smoke soft and pleasant aftertaste.

The benefits of the present invention are:

Compared with the prior art, the method of membrane separation and microfiltration is used to remove a large amount of protein, pectin, starch, wax, cellulose and pigment substances contained in the mango extract, and avoid these components being added to shredded tobacco. The problem of poor sensory comfort when burning and smoking. In addition, the present invention uses the membrane separation ultrafiltration method to remove some small molecular substances in the mango extract that affect the aroma quality and aroma quality and are irritating, retain the appropriate aroma components in the spices as much as possible and reduce the miscellaneous gas and irritation Sex, while removing the macromolecular and small molecular impurities in the mango flavor, making the application of the flavor better.

Detailed ways

The present invention will be further described below in conjunction with the examples, but the scope of the present invention is not limited in any way.

Embodiment one

Fresh ripe mangoes were taken, peeled, cut into uniform slices, placed in an oven, and dried at 50°C for 12 hours. Take the dried mango slices, pulverize them into coarse powder, and pass through a 10-mesh stainless steel sieve. Accurately weigh 100g of mango powder, wrap it with filter paper and put it into a Soxhlet extractor, add 500mL of 90% ethanol, heat at 80°C, and heat to reflux for 2h. Filter and distill the filtrate under reduced pressure until no ethanol flows out to obtain mango extract. Accurately weigh 10g of mango extract and place it in a 1000mL beaker, add 500mL of 20% ethanol to dissolve (N1). After the dissolution is complete, use a 50nm ceramic microfiltration membrane to filter, and the interception section is N2; the microfiltration membrane permeate is then filtered with a 100kd organic membrane, and the interception section is recorded as N3, and the permeation section is recorded as N4. Take the N3 part and distill it under reduced pressure to a relative density of 1.10 to obtain the mango flavor for tobacco. Take the mango flavor for tobacco, dilute it 50 times with ethanol, spray it on shredded tobacco according to the ratio of 0.2%, roll it into cigarettes, and take another N1 part, operate in the same way as a control.

Embodiment two

Fresh ripe mangoes were taken, peeled, cut into uniform slices, placed in an oven, and dried at 50°C for 12 hours. Take the dried mango slices, pulverize them into coarse powder, and pass through a 10-mesh stainless steel sieve. Accurately weigh 50g of mango powder, wrap it with filter paper and put it into a Soxhlet extractor, add 500mL of 50% ethanol, heat at 50°C, and heat to reflux for 2.5h. Filter and distill the filtrate under reduced pressure until no ethanol flows out to obtain mango extract. Accurately weigh 10g of mango extract and place it in a 1000mL beaker, add 500mL of 20% ethanol to dissolve (N1). After the dissolution is complete, use a 200nm ceramic microfiltration membrane to filter, and the interception section is N2; the microfiltration membrane permeate is then filtered with a 500kd organic membrane, and the interception section is recorded as N3, and the permeation section is recorded as N4. Take the N3 part and distill it under reduced pressure to a relative density of 1.15 to obtain mango flavor for tobacco. Take the mango flavor for tobacco, dilute it 100 times with propylene glycol, spray it on shredded tobacco according to the ratio of 1%, and roll it into cigarettes. Another N1 part was taken and operated in the same way as a control.

Embodiment three

Fresh ripe mangoes were taken, peeled, cut into uniform slices, placed in an oven, and dried at 50°C for 12 hours. Take the dried mango slices, pulverize them into coarse powder, and pass through a 10-mesh stainless steel sieve. Accurately weigh 150g of mango powder, wrap it with filter paper and put it into a Soxhlet extractor, add 450mL of 100% ethanol (absolute ethanol), heat at 90°C, and heat to reflux for 1h. Filter and distill the filtrate under reduced pressure until no ethanol flows out to obtain mango extract. Accurately weigh 10g of mango extract and place it in a 1000mL beaker, add 500mL of 20% ethanol to dissolve (N1). After the dissolution is complete, use a 100nm ceramic microfiltration membrane to filter, and the cut-off section is N2; the microfiltration membrane permeate is then filtered with a 10kd organic membrane, and the cut-off section is recorded as N3, and the permeated section is recorded as N4. Take the N3 part and distill it under reduced pressure to a relative density of 1.05 to obtain mango flavor for tobacco. Take the mango flavor for tobacco, dilute it 10 times with glycerin, spray it on shredded tobacco according to the ratio of 0.01%, and roll it into cigarettes. Another N1 part was taken and operated in the same way as a control.

Embodiment Four

Fresh ripe mangoes were taken, peeled, cut into uniform slices, placed in an oven, and dried at 50°C for 12 hours. Take the dried mango slices, pulverize them into coarse powder, and pass through a 10-mesh stainless steel sieve. Accurately weigh 100g of mango powder, wrap it with filter paper and put it into a Soxhlet extractor, add 800mL of 70% ethanol, heat at 70°C, and heat to reflux for 1.5h. Filter and distill the filtrate under reduced pressure until no ethanol flows out to obtain mango extract. Accurately weigh 10g of mango extract and place it in a 1000mL beaker, add 500mL of 20% ethanol to dissolve (N1). After the dissolution is complete, use a 200nm ceramic microfiltration membrane to filter, and the cut-off section is N2; the microfiltration membrane permeate is then filtered with a 50kd organic membrane, and the cut-off section is recorded as N3, and the permeated section is recorded as N4. The N3 part was distilled under reduced pressure to a relative density of 1.08 to obtain mango flavor for tobacco. Take mango flavor for tobacco, dilute sorbitol 30 times, spray on shredded tobacco according to the ratio of 0.5%, and roll it into cigarettes. Another N1 part was taken and operated in the same way as a control.

Embodiment five

Fresh ripe mangoes were taken, peeled, cut into uniform slices, placed in an oven, and dried at 50°C for 12 hours. Take the dried mango slices, pulverize them into coarse powder, and pass through a 10-mesh stainless steel sieve. Accurately weigh 100g of mango powder, wrap it with filter paper and put it into a Soxhlet extractor, add 600mL of 60% ethanol, heat at 60°C, and heat to reflux for 2h. Filter and distill the filtrate under reduced pressure until no ethanol flows out to obtain mango extract. Accurately weigh 10g of mango extract and place it in a 1000mL beaker, add 500mL of 20% ethanol to dissolve (N1). After the dissolution is complete, use a 100nm ceramic microfiltration membrane to filter, and the cut-off section is N2; the microfiltration membrane permeate is then filtered with a 200kd organic membrane, and the cut-off section is marked as N3, and the permeated section is marked as N4. The N3 part was distilled under reduced pressure to a relative density of 1.13 to obtain mango flavor for tobacco. Take mango flavor for tobacco, dilute xylitol 80 times, spray on shredded tobacco according to the ratio of 0.05%, and roll it into cigarettes. Another N1 part was taken and operated in the same way as a control.

Embodiment six

Fresh ripe mangoes were taken, peeled, cut into uniform slices, placed in an oven, and dried at 50°C for 12 hours. Take the dried mango slices, pulverize them into coarse powder, and pass through a 10-mesh stainless steel sieve. Accurately weigh 100g of mango powder, wrap it with filter paper and put it into a Soxhlet extractor, add 400mL of 75% ethanol, heat at 55°C, and heat to reflux for 1.5h. Filter and distill the filtrate under reduced pressure until no ethanol flows out to obtain mango extract. Accurately weigh 10g of mango extract and place it in a 1000mL beaker, add 500mL of 20% ethanol to dissolve (N1). After the dissolution is complete, use a 50nm ceramic microfiltration membrane to filter, and the cut-off section is N2; the microfiltration membrane permeate is then filtered with a 30kd organic membrane, and the cut-off section is recorded as N3, and the permeated section is recorded as N4. The N3 part was distilled under reduced pressure to a relative density of 1.07 to obtain mango flavor for tobacco. Take the mango flavor for tobacco, dilute it 40 times with ethanol/propylene glycol mixed solution (ethanol:propylene glycol=1:1) xylitol, spray it on shredded tobacco at a ratio of 0.1%, and roll it into cigarettes. Another N1 part was taken and operated in the same way as a control.

Embodiment seven

Fresh ripe mangoes were taken, peeled, cut into uniform slices, placed in an oven, and dried at 50°C for 12 hours. Take the dried mango slices, pulverize them into coarse powder, and pass through a 10-mesh stainless steel sieve. Accurately weigh 100g of mango powder, wrap it with filter paper and put it into a Soxhlet extractor, add 400mL of 75% ethanol, heat at 55°C, and heat to reflux for 1.5h. Filter and distill the filtrate under reduced pressure until no ethanol flows out to obtain mango extract. Accurately weigh 10g of mango extract and place it in a 1000mL beaker, add 500mL of 20% ethanol to dissolve (N1). After the dissolution is complete, use a 50nm ceramic microfiltration membrane to filter, and the cut-off section is N2; the microfiltration membrane permeate is then filtered with a 30kd organic membrane, and the cut-off section is recorded as N3, and the permeated section is recorded as N4. The N3 part was distilled under reduced pressure to a relative density of 1.07 to obtain mango flavor for tobacco. Take mango flavor for tobacco, dilute xylitol 60 times with xylitol/sorbitol mixed solution (xylitol: sorbitol = 1:1), spray on shredded tobacco at a ratio of 0.1%, and roll it into cigarettes. Another N1 part was taken and operated in the same way as a control.

Experimental example

1. Analysis of volatile components of mango flavor for tobacco

Accurately measure 1.0 g of the mango flavor for tobacco prepared in Example 1 into a separatory funnel, add 20 mL of 20% ethanol to shake and dissolve, and after the dissolution is complete, add 50 mL of dichloromethane to extract for 24 hours. Remove the supernatant, add an appropriate amount of anhydrous sodium sulfate, and let stand overnight. Concentrate to 1 mL for GC-MS analysis.

GC-MS conditions are as follows: chromatographic column: HP-5MS capillary column (60m*0.32mm*0.25μm); inlet temperature: 250°C; temperature program: the initial temperature is 50°C for 3 minutes, and then rises at a speed of 4°C to 260°C, maintained for 5min; Vaporization temperature: 270°C; Carrier gas: He, 1mL min-1; Split ratio: 5:1; Ionization method: EI source; Detector temperature: FID, 300°C; Transfer line temperature: 280°C; Ionization energy: 70eV; ion source temperature: 230°C; mass scanning range: 30-700amu; search spectrum library: NIST11 library.

According to Table 1, a total of 31 substances were detected in mango flavor for tobacco. Farnesyl acetone has a sweet and rose fragrance, which can impart a fragrance to cigarettes; trans-squalene is a non-pigmented terpene substance in tobacco leaves, which can not only enhance the taste and aroma of tobacco leaves, but also can be transformed through degradation Form aroma components; myristic acid has the effect of waxy, sweet and soft smoke; palmitic acid has the effect of increasing the sweetness, waxy taste and fullness of smoke; ethyl oleate can increase the concentration of smoke, making the smoke Alcohol and alcohol; Ethyl palmitate can soften the smoke and increase sweetness, so that the cigarettes have a certain burnt sweetness and thick, long-lasting feeling; Ethyl linoleate can increase sweetness and soften the effect. These refined and enriched aroma components may be the material basis for tobacco mango spices to increase the aroma of tobacco and improve the taste.

Table 1 Volatile Components of Mango Flavor for Tobacco

2. Evaluation of the sensory effects of tobacco mango flavoring applied to cigarettes

Cigarettes rolled with 7 types of mango flavors for tobacco prepared in Examples 1-7, including N1 mango flavors in seven preparation processes. Submit to more than 7 judges to comprehensively evaluate smoking, take the control cigarette without adding any mango flavor as contrast, the result (table 2) shows: compared with the control sample, a kind of mango flavor for tobacco of the present invention is added in the cigarette after , can significantly increase the amount of aroma, the fruity sweetness is prominent, the aroma is coordinated, the sweetness is increased, and it can reduce irritation and miscellaneous gas, making the smoke soft and comfortable aftertaste. The overall effect of increasing aroma, improving taste and removing impurities and thorns in regular mango spice.

Table 2. Effect of mango flavor for tobacco on sensory quality of cigarettes

Claims (12)

1. a kind of cigarette preparation method of mango fragrance, which is characterized in that be achieved through the following technical solutions：

(1) dry：It takes fresh mature mango, after peeling, be cut into uniform sheet, is placed in baking oven, 50 DEG C of dry 12h；

(2) it crushes：Dry mango piece is taken, pulverizer breaks into coarse powder, crosses 10 mesh stainless steel mesh；

(3) it extracts：Mango powder is accurately weighed, loading Soxhlet extractor is wrapped with filter paper, is added 3-10 times and measures 50%-100% second Alcohol, is heated to reflux 1-2.5h by 50-90 DEG C of heating temperature.Filtering, filtrate decompression are distilled to no ethyl alcohol and are flowed out, and mango extractum is obtained；

(4) micro-filtration UF membrane：It really weighs mango extractum to be placed in quantitative glass container, the ethyl alcohol of 50 times of amounts 20% is added, dissolve, Dissolved solution is N1.It is to be dissolved completely after, filtered using 50-200nm ceramic micro filter film, retention section be N2；

(5)) Ultra filtration membrane：Microfiltration membranes permeate 10-500kd organic membrane filter, retention section are denoted as N3, are denoted as N4 through section；

(6) it takes N3 part reduced pressure to distill to relative density 1.05-1.15, obtains mango fragrance.

2. the preparation method of a kind of cigarette mango fragrance according to claim 1, which is characterized in that in step (3), be added 5-8 times is measured 70%-95% ethyl alcohol, 65-85 DEG C of heating temperature, is heated to reflux 1-2.5h.Filtering, filtrate decompression are distilled to no ethyl alcohol Outflow, obtains mango extractum.

3. the preparation method of a kind of cigarette mango fragrance according to claim 1, which is characterized in that in step (3), be added 5-6 times is measured 85%-90% ethyl alcohol, 75-80 DEG C of heating temperature, is heated to reflux 1-2.5h.Filtering, filtrate decompression are distilled to no ethyl alcohol Outflow, obtains mango extractum.

4. the preparation method of a kind of cigarette mango fragrance according to claim 1, which is characterized in that in step (4), micro-filtration Membrane aperture is 50nm.

5. the preparation method of a kind of cigarette mango fragrance according to claim 1, which is characterized in that in step (5), ultrafiltration Membrane aperture is 20-200KD.

6. the preparation method of a kind of cigarette mango fragrance according to claim 1, which is characterized in that in step (5), ultrafiltration Membrane aperture is 50-100KD.

7. application of a kind of cigarette of one of -6 the methods preparation with mango fragrance in cigarette according to claim 1, feature It is, the cigarette is diluted with mango fragrance with the nontoxic organic solvent having no irritating odor, extension rate 10-100 Times；The cigarette is sprayed on pipe tobacco according to the mass ratio of 0.02%-1% with mango fragrance before preparing cigarette, is rolled coiled Cigarette.

8. application of a kind of cigarette of one of -6 the methods preparation with mango fragrance in cigarette according to claim 1, feature It is, the cigarette is diluted with mango fragrance with the nontoxic organic solvent having no irritating odor, extension rate 20-70 Times；The cigarette is sprayed on pipe tobacco according to the mass ratio of 0.05-0.5% with mango fragrance before preparing cigarette, is rolled coiled Cigarette.

9. application of a kind of cigarette of one of -6 the methods preparation with mango fragrance in cigarette according to claim 1, feature It is, the cigarette is diluted with mango fragrance with the nontoxic organic solvent having no irritating odor, extension rate 40-50 Times；The cigarette is sprayed on pipe tobacco according to the mass ratio of 0.1-0.3% with mango fragrance before preparing cigarette, is rolled coiled Cigarette.

10. application of a kind of cigarette with mango fragrance in cigarette according to claim 7, which is characterized in that described is organic Solvent is ethyl alcohol, propylene glycol, sorbierite, xylitol or glycerol, or wherein any mixed liquor of more than two kinds.

11. application of a kind of cigarette with mango fragrance in cigarette according to claim 8, which is characterized in that described is organic Solvent is ethyl alcohol, propylene glycol, sorbierite, xylitol or glycerol, or wherein any mixed liquor of more than two kinds.

12. application of a kind of cigarette with mango fragrance in cigarette according to claim 9, which is characterized in that described is organic Solvent is ethyl alcohol, propylene glycol, sorbierite, xylitol or glycerol, or wherein any mixed liquor of more than two kinds.