CN102166038B - Method for extracting snakegourd peel, application of snakegourd peel extract to cigarettes and cigarettes - Google Patents

Method for extracting snakegourd peel, application of snakegourd peel extract to cigarettes and cigarettes Download PDF

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CN102166038B
CN102166038B CN 201110061986 CN201110061986A CN102166038B CN 102166038 B CN102166038 B CN 102166038B CN 201110061986 CN201110061986 CN 201110061986 CN 201110061986 A CN201110061986 A CN 201110061986A CN 102166038 B CN102166038 B CN 102166038B
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pericarpium trichosanthis
mixed liquor
extract
enzyme
cigarette
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CN102166038A (en
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余汉谋
肖海鸿
姜兴涛
曲家妮
强耀峰
李庆廷
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BODUN PERFUME Co Ltd SHENZHEN
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BODUN PERFUME Co Ltd SHENZHEN
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Abstract

The invention discloses a method for extracting snakegourd peel, which comprises the following steps of: 1) crushing, namely drying a snakegourd peel raw material to be extracted at the temperature of between 40 and 70 DEG C, and crushing to form coarse powder of which the grain size is between 150 and 420mu m; 2) performing enzymolysis and ultrasonic extraction, namely stirring and mixing the snakegourd peel coarse powder and buffer solution of phosphoric acid in a mass ratio of 1:6-1:15 to form mixed liquor, and putting the mixed liquor into an ultrasonic extraction tank to perform the enzymolysis and the ultrasonic extraction; 3) inactivating enzymes, namely heating the mixed liquor subjected to the enzymolysis to the temperature of between 80 and 90 DEG C, and maintaining for 15 to 30 minutes to inactivate the enzymes; 4) filtering, namely filtering the mixed liquor subjected to enzyme inactivating to obtain filter liquor; and 5) concentrating, concentrating the filter liquor to obtain a snakegourd peel extract. The method for extracting the snakegourd peel is simple and low in energy consumption. The extracted snakegourd peel extract is applied to cigarette preparation, so that the inherent quality of cigarettes can be improved.

Description

A kind of extracting method of PERICARPIUM TRICHOSANTHIS and extract thereof application and the cigarette in cigarette
[technical field]
The present invention relates to plant extract and application thereof, particularly relate to a kind of extracting method and the application of extract in cigarette and cigarette that comprises this Pericarpium Trichosanthis extract of PERICARPIUM TRICHOSANTHIS.
[background technology]
PERICARPIUM TRICHOSANTHIS is the maturate peel of cucurbitaceous plant snakegourd or trichosanthes rosthornii Harms etc., Shennong's Herbal begins to be stated from, have moistening lung, reduce phlegm, dissipating bind, purging and intestine lubricating action, be China's tcm clinical practice medication commonly used, be mainly used in the sick treatment such as tracheitis, pulmonary heart disease, coronary heart disease.
For the extraction of PERICARPIUM TRICHOSANTHIS, in traditional handicraft, usually adopt the mixed solvent of water, ethanol to obtain after distilling, filter, concentrating.The method length consuming time, efficient are low.And some extractive techniques that newly-developed gets up, as enzymatic isolation method, ultrasonic assisted Extraction follow the example of, NF membrane partition method etc. has obvious superiority aspect selective, operating efficiency, energy-conserving and environment-protective, shown great application prospect, but it is to be solved that these methods still have some problems to have on suitability for industrialized production, and as long in enzymolysis time, production power consumption is large etc.How to improve, make extracting method simple, power consumption is few, and efficient is high, is easy to industrializing implementation, is the direction that people make great efforts.On the other hand, present stage, the application study of domestic relevant PERICARPIUM TRICHOSANTHIS mainly concentrates on the industries such as chemical constitution study, cosmetics skin care, and the application in cigarette has no relevant report.
[summary of the invention]
Technical problem to be solved by this invention is: make up above-mentioned the deficiencies in the prior art, propose a kind of extracting method of PERICARPIUM TRICHOSANTHIS, method is simple, produces power consumption less.
Another technical problem to be solved by this invention is: Pericarpium Trichosanthis extract is applied to can greatly improve the interior quality of cigarette in the cigarette manufacturing.
Technical problem of the present invention is solved by following technical scheme:
A kind of extracting method of PERICARPIUM TRICHOSANTHIS comprises the following steps: 1) pulverize: PERICARPIUM TRICHOSANTHIS raw material to be extracted is dried under 40~70 ℃ of conditions, and be crushed to the meal that granularity is 150~420 μ m; 2) enzymolysis and ultrasonic extraction: the ratio that is 1:6~1:15 according to mass ratio with described PERICARPIUM TRICHOSANTHIS meal and phosphate buffer solution mixes the composition mixed liquor, described mixed liquor is placed in enzymolysis and the ultrasonic extraction that ultrasonic extractor carries out 10~40min, hydrolysis temperature is 37 ± 1 ℃, the ultrasonic power of ultrasonic extraction is 30-100W, dutycycle is 20%-80%, and frequency is 20KHz-80KHz; Wherein, described phosphate buffer solution is for containing complex enzyme, and the pH value is 3.5~4.5 phosphate buffer solution; 3) enzyme that goes out is processed: with step 2) in the mixed liquor of enzymolysis after finishing be heated to 80~90 ℃ and keep 15~30min to carry out enzyme-deactivating; 4) filter: the mixed liquor filtration treatment after the enzyme that will go out gets filtrate; 5) concentrated: the described filtrate that obtains in step 4) is carried out concentration, and the thick solution after concentrating is Pericarpium Trichosanthis extract.
In preferred technical scheme,
Described step 2) in, the mass ratio of described PERICARPIUM TRICHOSANTHIS meal and described phosphate buffer solution is 1:12.When getting this mass ratio and be mixed with mixed liquor, can guarantee that PERICARPIUM TRICHOSANTHIS fully soaks in phosphate buffer solution, the amount of phosphate buffer solution also is unlikely to when follow-up concentration, can not consume long time concentration too much simultaneously, also just can not consume excessive power.
Described step 2) in, contain the complex enzyme of 1-5% in described phosphate buffer solution.Like this, can guarantee that macromolecules degradation is complete, can avoid waste again.
Described step 2) in, described complex enzyme is comprised of cellulase, pectase and protease, and three's mass ratio is: cellulase: pectase: protease=1~2:1~3:1~2.Like this, by using the complex enzyme that is formed by cellulase, pectase and protease to carry out enzymolysis, make the macromolecules degradations such as cellulose, pectin and protein in extract complete, coordinate the ul-trasonic irradiation that applies in enzymolysis process, can improve enzymolysis efficiency, shorten extraction time, industrializing implementation is easier to.
In described step 4), the mixed liquor after the enzyme that will go out is the screen cloth by 48 μ m apertures successively, and the microfiltration membranes of 0.45 μ m and molecular weight are that 6000 milipore filter carries out filtration treatment.As a kind of embodiment, can select above-mentioned filter type to carry out filtration treatment.
In described step 5), described filtrate is concentrated into quality and is 1/2~1/8 thick solution of PERICARPIUM TRICHOSANTHIS material quality described in step 1).Get 1/2~1/8 this scope of material quality, can guarantee extract the thickness state, be easy to preserve, and also can satisfy the follow-up concentration application demand that is applied on cigarette.
Described concentrating is to adopt the reduced vacuum concentrator to carry out concentration to filtrate.
Technical problem of the present invention is solved by following further technical scheme:
A kind of application of Pericarpium Trichosanthis extract in cigarette of extracting according to said method diluted described Pericarpium Trichosanthis extract with the nontoxic organic solvent that has no irritating odor, extension rate is 10-15 times; Before the preparation cigarette, described Pericarpium Trichosanthis extract dilution is sprayed at the cured tobacco leaf surface according to the mass ratio of 0.1%-1%.
Described organic solvent is propane diols, sorbierite, xylitol or glycerine, perhaps any mixed liquor more than 2 kinds wherein.
Technical problem of the present invention is solved by following further technical scheme:
A kind of cigarette is added with the Pericarpium Trichosanthis extract that extracts according to said method in described cigarette.
The beneficial effect that the present invention is compared with the prior art is:
The extracting method of PERICARPIUM TRICHOSANTHIS of the present invention adopts ul-trasonic irradiation to extract, and can accelerate active ingredient to the diffusion rate of solvent, and extraction time is shortened greatly, need not high-temperature process in prior art, and power consumption is few; Enzymolysis process and ultrasonic leaching process carry out simultaneously simultaneously, and ul-trasonic irradiation puts on enzymolysis process, also can improve enzymolysis efficiency, shorten extraction time, make industrializing implementation easy; And the ultrasonic extraction device automaticity is high, simple to operate, makes the extracting method integrated operation also simple.Further, in ultrasonic leaching process, the complex enzyme that is comprised of cellulase, pectase and protease carries out enzymolysis, make the large molecule such as cellulose, pectin and protein in extract be degraded, can shorten enzymolysis time, raise the efficiency, be suitable for industrializing implementation.On the other hand, the Pericarpium Trichosanthis extract that extracting method of the present invention is prepared is applied in the cigarette preparation, and is easy to use, and can greatly improve the interior quality of cigarette, and cigarette fragrance is increased, and dried-up assorted gas alleviates, the sweet property raising of flue gas.
[specific embodiment]
Below in conjunction with the specific embodiment, the present invention is described in further details.
A kind of extracting method of PERICARPIUM TRICHOSANTHIS comprises the following steps:
1) pulverize: PERICARPIUM TRICHOSANTHIS raw material to be extracted is dried under 40~70 ℃ of conditions, and be crushed to the meal that granularity is 150~420 μ m., be crushed into the meal that granule size is 150-420 μ m herein, be because, if granularity less than 150 μ m, too thin, material easily is bonded together, and causes the problem of filtration difficulty and ul-trasonic irradiation Efficiency Decreasing; And if granularity is too thick greater than 420 μ m, the ultrasonic disruption cell processes is obstructed, and makes ul-trasonic irradiation extend, and time consumption and energy consumption increases.
2) enzymolysis and ultrasonic extraction: the ratio that is 1:12 according to mass ratio with PERICARPIUM TRICHOSANTHIS meal and phosphate buffer solution mixes the composition mixed liquor, mixed liquor is placed in enzymolysis and the ultrasonic extraction that ultrasonic extractor carries out 10~40min, hydrolysis temperature is 37 ± 1 ℃, the ultrasonic power of ultrasonic extraction is 30-100W, dutycycle is 20%-80%, and frequency is 20KHz-80KHz; Wherein, described phosphate buffer solution is for containing complex enzyme, and the pH value is 3.5~4.5 phosphate buffer solution.Wherein, phosphate buffer solution is that the pH value that contains complex enzyme is 3.5~4.5 phosphate buffer solution.In this step, adopt ultrasonic wave to extract, power consumption is few, and the ultrasonic extraction device automaticity is high, and is simple to operate.Simultaneously, enzymolysis process and ultrasonic leaching process are synchronous, and ul-trasonic irradiation can improve enzymolysis efficiency in enzymolysis process, shorten extraction time, and industrializing implementation is easier to.
Preferably, contain the complex enzyme that mass fraction is 1-5% in phosphate buffer solution, this be because, if complex enzyme is very little, enzyme activity is inadequate, macromolecules degradation is incomplete; If complex enzyme is too much, easily cause waste, raise the cost, be set at 1-5%, can satisfy application requirements.And the pH value is made as 3.5~4.5, be the best pH scope when being complex enzyme enzyme activity maximum because of this scope.
Further preferably, complex enzyme is comprised of cellulase, pectase and protease, and three's mass ratio is: cellulase: pectase: protease=1~2:1~3:1~2.Like this, make the large molecule such as cellulose, pectin and protein in extract be degraded fully.
3) enzyme that goes out is processed: with step 2) in the mixed liquor of enzymolysis after finishing be heated to 80~90 ℃ and keep 15~30min to carry out enzyme-deactivating.
4) filter: the hybrid filtering after the enzyme that will go out is processed, and gets filtrate.Preferably, can be with the mixed liquor after the enzyme that goes out the screen cloth by 48 μ m apertures successively, the microfiltration membranes of 0.45 μ m and molecular weight are that 6000 milipore filter carries out filtration treatment.
5) concentrated: the filtrate that obtains in step 4) is carried out concentration, and the thick solution after concentrating is Pericarpium Trichosanthis extract.Preferably, filtrate is concentrated into 1/2~1/8 thick solution of quality PERICARPIUM TRICHOSANTHIS material quality.Can adopt the reduced vacuum concentrator to carry out concentration to filtrate when concentrated.
The PERICARPIUM TRICHOSANTHIS that obtains according to the method described above is applied in cigarette, at first, Pericarpium Trichosanthis extract is diluted with the nontoxic organic solvent that has no irritating odor, extension rate is 10-15 times.Wherein, organic solvent can be propane diols, sorbierite, xylitol or glycerine, perhaps any mixed liquor more than 2 kinds wherein.Secondly, before the preparation cigarette, the Pericarpium Trichosanthis extract dilution is sprayed at the cured tobacco leaf surface according to the mass ratio of 0.1%-1%.Then, cigarette process is routinely processed, and namely after spraying the dilution of Pericarpium Trichosanthis extract, with flue-cured tobacco tobacco storage 4 hours, then makes cigarette finished product through chopping, baking silk, perfuming, storage silk, cigarette and packaging process.
The specific embodiment one
Accurately take the 200g PERICARPIUM TRICHOSANTHIS, 45 ℃ of oven dry, and be crushed to the meal that granularity is 250 μ m, the pH that adds 2400g to contain 2% complex enzyme is 3.5 phosphate buffer solution and mixes, and wherein complex enzyme is comprised of cellulase, pectase and protease, and its mass ratio is cellulase: pectase: protease=1:2:1, temperature is controlled at carries out ultrasonic extraction and enzymolysis 30min under 37 ± 1 ℃, wherein ultrasonic power is 40W, and dutycycle is 50%, and frequency is 20KHz.Be warming up to 85 ℃ and keep the 15min enzyme that goes out to live after enzymolysis.Go out mixed liquor after enzyme through the screen filtration in 48 μ m apertures, and the filtrate microfiltration membranes by 0.45 μ m and molecular weight successively is 6000 milipore filter, and the filtrate that obtains directly is concentrated into the thick solution of 80g, is the Pericarpium Trichosanthis extract I.
The specific embodiment two
Accurately take the 200g PERICARPIUM TRICHOSANTHIS, 50 ℃ of oven dry, and be crushed to the meal that granularity is 420 μ m, the pH that adds 2400g to contain 1% complex enzyme is 4.0 phosphate buffer solution and mixes, and wherein complex enzyme is comprised of cellulase, pectase and protease, and its mass ratio is cellulase: pectase: protease=2:2:1, temperature is controlled at carries out ultrasonic extraction and enzymolysis 25min under 37 ± 1 ℃, wherein ultrasonic power is 60W, and dutycycle is 40%, and frequency is 20KHz.Be warming up to 85 ℃ and keep the 20min enzyme that goes out to live after enzymolysis.Go out mixed liquor after enzyme through the screen filtration in 48 μ m apertures, and the filtrate microfiltration membranes by 0.45 μ m and molecular weight successively is 6000 milipore filter, and the filtrate that obtains directly is concentrated into the thick solution of 50g, is the Pericarpium Trichosanthis extract II.
The specific embodiment three
Accurately take the 200g PERICARPIUM TRICHOSANTHIS, 65 ℃ of oven dry, and be crushed to the meal that granularity is 150 μ m, the pH that adds 2400g to contain 1.5% complex enzyme is 4.0 phosphate buffer solution and mixes, and wherein complex enzyme is comprised of cellulase, pectase and protease, and its mass ratio is cellulase: pectase: protease=1:2:2, temperature is controlled at carries out ultrasonic extraction and enzymolysis 20min under 37 ± 1 ℃, wherein ultrasonic power is 100W, and dutycycle is 60%, and frequency is 20KHz.Be warming up to 85 ℃ and keep the 30min enzyme that goes out to live after enzymolysis.Go out mixed liquor after enzyme through the screen filtration in 48 μ m apertures, and the filtrate microfiltration membranes by 0.45 μ m and molecular weight successively is 6000 milipore filter, and the filtrate that obtains directly is concentrated into the thick solution of 75g, is the Pericarpium Trichosanthis extract III.
Experimental test: the Pericarpium Trichosanthis extract I, II, the III that make in above-mentioned embodiment one, two, three all are diluted to 10 times with 50% propylene glycol solution, then are sprayed at the middle-grade blank of same (not flavoring and casing) flue-cured tobacco pipe tobacco surperficial.Each Pericarpium Trichosanthis extract is all set 4 kinds of additions and is tested (addition be pipe tobacco 0.1%, 0.5%, 0.8%, 1.0%).Subsequent treatment cigarette process routinely carries out, and namely after spraying the dilution of Pericarpium Trichosanthis extract, with flue-cured tobacco tobacco storage 4 hours, then makes cigarette finished product through chopping, baking silk, perfuming, storage silk, cigarette and packaging process.To the contrast of smokeing panel test of above-mentioned sample, the overall sensory test result that obtains is as shown in the table respectively in the group of smokeing panel test that is comprised of 8 people.Wherein, the interior quality of blank sample all is set as 0, improves to some extent (increase as fragrance, dried-up assorted gas alleviates, the sweet property raising of flue gas, mouthfeel improves) with respect to the blank sample interior quality, mutually deservedly just divide, score value is higher, and it is better to improve; Decrease (reduce as fragrance, dried-up assorted gas increases, the sweet property minimizing of flue gas, mouthfeel variation) with respect to the blank sample interior quality, mutually deserved negative minute, negative minute lower, and it is poorer to improve.
Figure GDA00001872428500051
From above table as can be known, with respect to the cigarette of blank sample, the cigarette flavor of the Pericarpium Trichosanthis extract that increases on tobacco leaf all increases to some extent, and dried-up assorted gas reduces, the sweet property raising of flue gas, and mouthfeel improves.And for the Pericarpium Trichosanthis extract of concrete how many mass ratios of increase, need to obtain according to the setting routine tests of each parameter in extracting method, for example, for the Pericarpium Trichosanthis extract I of extracting in embodiment one, increase by 0.8% amount, can reach best general improvements, and for Pericarpium Trichosanthis extract II and the III extracted in other dual mode, needing increases by 1% amount, just reaches best general improvements.
Above content is in conjunction with concrete preferred embodiment further description made for the present invention, can not assert that concrete enforcement of the present invention is confined to these explanations.For the general technical staff of the technical field of the invention, make without departing from the inventive concept of the premise some substituting or obvious modification, and performance or purposes identical, all should be considered as belonging to protection scope of the present invention.

Claims (10)

1. the extracting method of a PERICARPIUM TRICHOSANTHIS is characterized in that: comprise the following steps:
1) pulverize: PERICARPIUM TRICHOSANTHIS raw material to be extracted is dried under 40~70 ℃ of conditions, and be crushed to the meal that granularity is 150~420 μ m;
2) enzymolysis and ultrasonic extraction: the ratio that is 1:6~1:15 according to mass ratio with described PERICARPIUM TRICHOSANTHIS meal and phosphate buffer solution mixes the composition mixed liquor, described mixed liquor is placed in enzymolysis and the ultrasonic extraction that ultrasonic extractor carries out 10~40min, hydrolysis temperature is 37 ± 1 ℃, the ultrasonic power of ultrasonic extraction is 30-100W, dutycycle is 20%-80%, and frequency is 20KHz-80KHz; Wherein, described phosphate buffer solution is for containing complex enzyme, and the pH value is 3.5~4.5 phosphate buffer solution;
3) enzyme that goes out is processed: with step 2) in the mixed liquor of enzymolysis after finishing be heated to 80~90 ℃ and keep 15~30min to carry out enzyme-deactivating;
4) filter: the mixed liquor filtration treatment after the enzyme that will go out gets filtrate;
5) concentrated: the described filtrate that obtains in step 4) is carried out concentration, and the thick solution after concentrating is Pericarpium Trichosanthis extract.
2. the extracting method of PERICARPIUM TRICHOSANTHIS according to claim 1, it is characterized in that: described step 2), the mass ratio of described PERICARPIUM TRICHOSANTHIS meal and described phosphate buffer solution is 1:12.
3. the extracting method of PERICARPIUM TRICHOSANTHIS according to claim 1, is characterized in that: described step 2), contain the complex enzyme of 1-5% in described phosphate buffer solution.
4. the extracting method of PERICARPIUM TRICHOSANTHIS according to claim 1 and 2, it is characterized in that: described step 2), described complex enzyme is comprised of cellulase, pectase and protease, and three's mass ratio is: cellulase: pectase: protease=1~2:1~3:1~2.
5. the extracting method of PERICARPIUM TRICHOSANTHIS according to claim 1 is characterized in that: in described step 4), the mixed liquor after the enzyme that will go out is the screen cloth by 48 μ m apertures successively, and the microfiltration membranes of 0.45 μ m and molecular weight are that 6000 milipore filter carries out filtration treatment.
6. the extracting method of PERICARPIUM TRICHOSANTHIS according to claim 1 is characterized in that: 1/2~1/8 the thick solution that in described step 5), described filtrate is concentrated into quality and is PERICARPIUM TRICHOSANTHIS material quality described in step 1).
7. the extracting method of PERICARPIUM TRICHOSANTHIS according to claim 6 is characterized in that: described concentrated be to adopt the reduced vacuum concentrator to carry out concentration to filtrate.
8. the application of Pericarpium Trichosanthis extract in cigarette that method according to claim 1 is extracted is characterized in that: described Pericarpium Trichosanthis extract is diluted with the nontoxic organic solvent that has no irritating odor, and extension rate is 10-15 times; Before the preparation cigarette, described Pericarpium Trichosanthis extract dilution is sprayed at the cured tobacco leaf surface according to the mass ratio of 0.1%-1%.
9. the application of Pericarpium Trichosanthis extract according to claim 8 in cigarette is characterized in that: described organic solvent is propane diols, sorbierite, xylitol or glycerine, perhaps any mixed liquor more than 2 kinds wherein.
10. a cigarette, is characterized in that: be added with the Pericarpium Trichosanthis extract that method according to claim 1 is extracted in described cigarette.
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