CN106520367A - Preparation method of wolfberry reactant for cigarette - Google Patents

Preparation method of wolfberry reactant for cigarette Download PDF

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Publication number
CN106520367A
CN106520367A CN201610854655.4A CN201610854655A CN106520367A CN 106520367 A CN106520367 A CN 106520367A CN 201610854655 A CN201610854655 A CN 201610854655A CN 106520367 A CN106520367 A CN 106520367A
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China
Prior art keywords
fructus lycii
reactant
cigarette
temperature
preparation
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CN201610854655.4A
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Chinese (zh)
Inventor
苗丽坤
喻世涛
庞登红
王萍
张磊
张辉
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China Tobacco Hunan Industrial Co Ltd
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China Tobacco Hunan Industrial Co Ltd
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Priority to CN201610854655.4A priority Critical patent/CN106520367A/en
Publication of CN106520367A publication Critical patent/CN106520367A/en
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B3/00Preparing tobacco in the factory
    • A24B3/12Steaming, curing, or flavouring tobacco
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/0003Compounds of unspecified constitution defined by the chemical reaction for their preparation

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention provides a preparation method of a wolfberry reactant for cigarette. The wolfberry reactant for cigarette is prepared by the following steps: freeze-drying wolfberry and then crushing, carrying out low-temperature extraction by adding 40-70% ethanol, filtering an extracting solution and carrying out low-temperature vacuum concentration, and finally carrying out a Maillard reaction. According to the invention, wolfberry can be extracted and concentrated at low temperature so as to maintain the original flavor of the extract to the maximum, and through the maillard reaction, aroma and fragrance of the extract are further enriched and smoke panel test effect of the extract in the cigarette is improved. In comparison with a common wolfberry extract, the prepared reactant has good compatibility with smoke, has rich fragrance, increases sweet taste, and can be applied to cigarette so as to increase sweet aroma, refine and soften smoke and reduce stimulation.

Description

A kind of preparation method of cigarette medlar reactant
Technical field
The invention belongs to essence spice for cigarette additive preparing technical field, and in particular to a kind of cigarette medlar reactant Preparation method.
Background technology
Fructus Lycii is Solanaceae Lycium defoliation bush plant, is the important economic plant resources of China, and it is not only nutritious, And there are multiple pharmacological effect and the physiological active functionses such as antitumor, anti-aging, lowering blood pressure and blood fat.Containing abundant carbon in Fructus Lycii Hydrate, up to 39.5%, content of reducing sugar is also higher for its total sugar content, accounts for the 1/3 of dried fruit of lycium barbarum total amount;Except tool in Fructus Lycii Have outside the lycium barbarum polysaccharide of physiological activity, also containing various monosaccharide such as glucose, Fructose.In addition, in Fructus Lycii containing ferrum, zinc, The various trace elements such as calcium, lithium, selenium, germanium, and 18 kinds of aminoacid needed by human, wherein with aspartic acid, glutamic acid, third The content of propylhomoserin and proline is higher, and free amino acid accounts for more than the 50% of total amino acid content, is conducive to absorption of human body.
In recent years, the research of Fructus Lycii is focused mostly in lycium barbarum polysaccharide, Fructus Lycii acid and Fructus Lycii total alkaloidss isoreactivity into Divide and extracted, extracting method mainly has immersion method, ultrasonic method, microwave method and enzyme process etc., as technics comparing falls behind so that carry Take yield and purity is relatively low, it is impossible to which its effective ingredient is made full use of, cause the serious waste of resource.And for Fructus Lycii is extracted Thing is less as the research that spice is applied in Medicated cigarette.
Maillard reaction is a kind of non-enzymatic browning for being widely present in food industry, be carbonyl compound (recuding sugars) and Reaction between amino-compound (amino acid and protein), so react also known as carbonyl ammonia.The technology is fragrant in meat flavoring and Nicotiana tabacum L. There is extraordinary application in essence, the essence for being formed has the vivid effect of natural essence, have the work that blending technology is incomparable With.As Fructus Lycii itself contains substantial amounts of aminoacid and reducing sugar composition, therefore, it is especially suitable for carrying out Maillard reaction.
The content of the invention
It is an object of the invention to provide a kind of preparation method of cigarette medlar reactant, the method combine leach at low temperature and Maillard reaction technology is realizing the preparation to cigarette medlar reactant.
For achieving the above object, the technical scheme of present invention offer is:A kind of preparation side of the cigarette medlar reactant Method, it comprises the following steps:
(1) pre-treatment:The impurity in Fructus Lycii is removed, and Fructus Lycii is cleaned;
(2) pre-cooling and lyophilization:The Fructus Lycii pre-cooling that will be handled well in step (1), and be -30~-40 DEG C in temperature Under the conditions of carry out vacuum lyophilization process 1~2h, vacuum keep 5~10Pa;
(3) crush:Fructus Lycii after lyophilization is crushed, degree of grinding is 80~100 mesh;
(4) leach at low temperature:Fructus Lycii powder after pulverization process is placed in thermostat water bath according to solid-to-liquid ratio 1:6~1:10 Ratio add the alcohol solvent that concentration is 40~70%, then extract 3~6h under conditions of 50~60 DEG C of temperature, and to carrying Taking liquid carries out sucking filtration, collects filtrate;
(5) it is concentrated in vacuo:Cryogenic vacuum concentration is carried out to the filtrate after leach at low temperature in step (4), and thickening temperature is set For 50~60 DEG C, cycles of concentration is 5~7 times, obtains wolfberry fruit extract;
(6) Maillard reaction:Wolfberry fruit extract in step (5) is placed in oil bath pan, and adds its weight 2%~5% Ammonia (ammonia concn is 28%), 90~110 DEG C of keeping temperature, 120~150r/min of stir speed (S.S.), 2~3h of response time; After Maillard reaction terminates, stopping is heated and is down to room temperature;
(7) allocate:To in step (6), reaction terminates and is reduced to addition reactant quality percentage ratio in the reactant of room temperature For 3%~5% fruital Mel, Fructus Lycii maillard reaction thing after stirring, is.
The present invention preferably technical scheme:The precooling temperature before lyophilization is carried out in step (2) to Fructus Lycii for -20 ~-25 DEG C, pre-coo time is 1~2h.
The present invention preferably technical scheme:The Fructus Lycii after leach at low temperature is extracted using buchner funnel in step (4) Liquid is filtered.
Preferably, in step (4), the concentration of ethanol is 50%, and extraction temperature is 55 DEG C, extraction time 5h, Solid-to-liquid ratio 1:8.
Preferably, the ammonia of its weight 3%, 100 DEG C of keeping temperature, stir speed (S.S.) is added in step (6) For 130r/min, the response time is 2.5h.
Preferably:The fruital Mel in step (7) includes Fructus Litchi Mel, Citrus Mel, jujube flower honey.
In the present invention, involved concentration of alcohol, each means weight concentration, such as 50% ethanol, refers to every 100g ethanol waters In solution, containing ethanol 50g.
It is an advantage of the current invention that:
1st, the present invention carries out freeze-drying process to Fructus Lycii, and the processing method is dried to raw material at low temperature, can Preserve the original flavor characteristic of Fructus Lycii;Meanwhile, Fructus Lycii quality can be made to become fragile, it is easy to carry out next step crushing.
2nd, the present invention adopts pulverization process to Fructus Lycii, is conducive to more fully extracting the effective ingredient of Fructus Lycii.
3rd, the present invention adopts leach at low temperature to Fructus Lycii powder, and the method Extracting temperature is low, effective ingredient can be avoided to be heated Destruction, so that ensure that the aroma quality of extract.
4th, the present invention carries out Maillard reaction to wolfberry fruit extract, further enriches its fragrance, fragrance so as to Neng Gougeng Coordinate with Gas phase Smoke well, so as to improve the effect of smokeing panel test of Medicated cigarette;And the Maillard reaction in the present invention can be by means of Chinese holly The abundant aminoacid of Qi itself and reducing sugar composition, without the need for additional amino and reducing sugar composition, make reactant at utmost keep The unique flavor characteristic of Fructus Lycii, fragrance are more coordinated, and operate easier.
Specific embodiment
With reference to specific embodiment, the present invention is further illustrated.
Embodiment 1, a kind of preparation method of cigarette medlar reactant, it comprises the following steps:
(1) pre-treatment:The impurity in Fructus Lycii is removed, and Fructus Lycii is cleaned;
(2) lyophilization:The Fructus Lycii handled well in step (1) is carried out into freeze-drying process, wherein, precooling temperature for- 25 DEG C, pre-coo time is 1h;Vacuum lyophilization temperature is -40 DEG C, and time 1h, vacuum keep 5~10Pa;
(3) crush:Fructus Lycii after lyophilization is crushed, degree of grinding is 80 mesh;
(4) leach at low temperature:Fructus Lycii powder after pulverization process is placed in thermostat water bath, the second that concentration is 50% is added Alcoholic solvent, carries out extracts active ingredients to which;50 DEG C of extraction temperature, extraction time 4h, solid-to-liquid ratio 1:7;
(5) filter:Sucking filtration is carried out to the fructus lycii extracted solution after leach at low temperature using buchner funnel, collects filtrate;
(6) it is concentrated in vacuo:Cryogenic vacuum concentration is carried out to the filtrate after leach at low temperature in step (5), and thickening temperature is set For 50 DEG C, cycles of concentration is 5 times, obtains wolfberry fruit extract;
(7) Maillard reaction:Wolfberry fruit extract in step (6) is placed in oil bath pan, and adds the ammonia of its weight 3% (concentration 28%), 90 DEG C of keeping temperature, stir speed (S.S.) 120r/min, response time 2h;
(8) cool down:After in step (7), Maillard reaction terminates, stopping is heated and is down to room temperature;
(9) allocate:The fruital Mel that its mass percent is 3% is added in the reactant in step (8), is stirred Fructus Lycii maillard reaction thing is afterwards.
Embodiment 2, a kind of preparation method of cigarette medlar reactant, it comprises the following steps:
(1) pre-treatment:The impurity in Fructus Lycii is removed, and Fructus Lycii is cleaned;
(2) lyophilization:The Fructus Lycii handled well in step (1) is carried out into freeze-drying process, wherein, precooling temperature for- 23 DEG C, pre-coo time is 1.5h;Vacuum lyophilization temperature is -35 DEG C, and time 1.5h, vacuum keep 5~10Pa;
(3) crush:Fructus Lycii after lyophilization is crushed, degree of grinding is 90 mesh;
(4) leach at low temperature:Fructus Lycii powder after pulverization process is placed in thermostat water bath, the second that concentration is 60% is added Alcoholic solvent, carries out extracts active ingredients to which;55 DEG C of extraction temperature, extraction time 5h, solid-to-liquid ratio 1:8;
(5) filter:Sucking filtration is carried out to the fructus lycii extracted solution after leach at low temperature using buchner funnel, collects filtrate;
(6) it is concentrated in vacuo:Cryogenic vacuum concentration is carried out to the filtrate after leach at low temperature in step (5), and thickening temperature is set For 55 DEG C, cycles of concentration is 6 times, obtains wolfberry fruit extract;
(7) Maillard reaction:Wolfberry fruit extract in step (6) is placed in oil bath pan, and adds the ammonia of its weight 4% (concentration 28%), 100 DEG C of keeping temperature, stir speed (S.S.) 130r/min, response time 2.5h;
(8) cool down:After in step (7), Maillard reaction terminates, stopping is heated and is down to room temperature;
(9) allocate:The fruital Mel that its mass percent is 4% is added in reactant in step (8), after stirring As Fructus Lycii maillard reaction thing.
Embodiment 3, a kind of preparation method of cigarette medlar reactant, it comprises the following steps:
(1) pre-treatment:The impurity in Fructus Lycii is removed, and Fructus Lycii is cleaned;
(2) lyophilization:The Fructus Lycii handled well in step (1) is carried out into freeze-drying process, wherein, precooling temperature for- 20 DEG C, pre-coo time is 2h;Vacuum lyophilization temperature is -30 DEG C, and time 2h, vacuum keep 5~10Pa;
(3) crush:Fructus Lycii after lyophilization is crushed, degree of grinding is 100 mesh;
(4) leach at low temperature:Fructus Lycii powder after pulverization process is placed in thermostat water bath, the second that concentration is 70% is added Alcoholic solvent, carries out extracts active ingredients to which;60 DEG C of extraction temperature, extraction time 6h, solid-to-liquid ratio 1:10;
(5) filter:Sucking filtration is carried out to the fructus lycii extracted solution after leach at low temperature using buchner funnel, collects filtrate;
(6) it is concentrated in vacuo:Cryogenic vacuum concentration is carried out to the filtrate after leach at low temperature in step (5), and thickening temperature is set For 60 DEG C, cycles of concentration is 7 times, obtains wolfberry fruit extract;
(7) Maillard reaction:Wolfberry fruit extract in step (6) is placed in oil bath pan, and adds the ammonia of its weight 5% (concentration 28%), 110 DEG C of keeping temperature, stir speed (S.S.) 150r/min, response time 3h;
(8) cool down:After in step (7), Maillard reaction terminates, stopping is heated and is down to room temperature;
(9) allocate:The fruital Mel that its mass percent is 5% is added in reactant in step (8), after stirring As Fructus Lycii maillard reaction thing.
Fructus Lycii maillard reaction thing obtained in embodiment 1-3 is added separately to Medicated cigarette in 0.5 ‰ ratio by test example 1 In tobacco shred, while with common wolfberry fruit extract embodiment 1 and comparative example 2 as a comparison, wherein comparative example 1 be by Fructus Lycii carries out microwave extraction, extracts what is be concentrated to give after filtering;Comparative example 2 is, by Fructus Lycii alcohol reflux, to extract Obtain after liquid is filtered and after concentration, effect of specifically smokeing panel test is shown in Table 1.
The effect test of smokeing panel test of 1 embodiment of table and comparative example
Test finds that the Fructus Lycii maillard reaction thing prepared using the method for the present invention can significantly improve the fragrance of Medicated cigarette, The zest of flue gas, good with flue gas harmony and fine and smooth soft flue gas is reduced, effect is substantially better than and is prepared using conventional method Wolfberry fruit extract.And the synthesis of embodiment 2 smokes panel test effect slightly better than embodiment 1 and 3.
Test example 2, the composition of the Fructus Lycii maillard reaction thing in embodiment 2 is analyzed, its concrete component analyses knot Fruit is shown in Table 2.
2 Fructus Lycii maillard reaction thing component analyses of table
Analyzed by makings, detect 35 kinds of volatile ingredients in embodiment 2 altogether, including various acids, ketone and esters Deng material, composition quantity will be more than comparative example.Experiment results proved, can make the fragrance of Fructus Lycii richer through Maillard reaction It is rich.

Claims (6)

1. a kind of preparation method of cigarette medlar reactant, it is characterised in that comprise the following steps:
(1) pre-treatment:The impurity in Fructus Lycii is removed, and Fructus Lycii is cleaned;
(2) pre-cooling and lyophilization:The Fructus Lycii pre-cooling that will be handled well in step (1), and carry out under conditions of -30~-40 DEG C Vacuum lyophilization processes 1~2h, and vacuum keeps 5~10Pa;
(3) crush:Fructus Lycii after lyophilization is crushed, degree of grinding is 80~100 mesh;
(4) leach at low temperature:Fructus Lycii powder after pulverization process is placed in thermostat water bath according to solid-to-liquid ratio 1:6~1:10 ratio Example adds the alcohol solvent that concentration is 40~70%, then extracts 3~6h under conditions of 50~60 DEG C of temperature, and to extracting solution Sucking filtration is carried out, filtrate is collected;
(5) it is concentrated in vacuo:Cryogenic vacuum concentration is carried out to the filtrate after leach at low temperature in step (4), and it is 50 to arrange thickening temperature ~60 DEG C, cycles of concentration is 5~7 times, obtains wolfberry fruit extract;
(6) Maillard reaction:Wolfberry fruit extract in step (5) is placed in oil bath pan, and adds the ammonia of its weight 2%~5% Water, 90~110 DEG C of keeping temperature, 120~150r/min of stir speed (S.S.), 2~3h of response time;After Maillard reaction terminates, Stopping is heated and is down to room temperature;
(7) allocate:Terminating and be reduced to addition reactant quality percentage ratio in the reactant of room temperature to the middle reaction of step (6) is 3%~5% fruital Mel, is Fructus Lycii maillard reaction thing after stirring.
2. the preparation method of cigarette medlar reactant as claimed in claim 1, it is characterised in that:To Fructus Lycii in step (2) The precooling temperature before lyophilization is carried out for -20~-25 DEG C, pre-coo time is 1~2h.
3. the preparation method of cigarette medlar reactant as described in the appended claim 1, it is characterised in that:Adopt in step (4) Buchner funnel is filtered to the fructus lycii extracted solution after leach at low temperature.
4. the preparation method of cigarette medlar reactant as described in the appended claim 1, it is characterised in that:Ethanol in step (4) Concentration be 50%, extraction temperature be 55 DEG C, extraction time 5h, solid-to-liquid ratio 1:8.
5. the preparation method of cigarette medlar reactant as described in the appended claim 1, it is characterised in that:Add in step (6) The ammonia of its weight 3%, 100 DEG C of keeping temperature, stir speed (S.S.) are 130r/min, and the response time is 2.5h.
6. the preparation method of cigarette medlar reactant as described in the appended claim 1, it is characterised in that:The fruit in step (7) Fragrant Mel includes Fructus Litchi Mel, Citrus Mel, jujube flower honey.
CN201610854655.4A 2016-09-27 2016-09-27 Preparation method of wolfberry reactant for cigarette Pending CN106520367A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108424814A (en) * 2018-03-20 2018-08-21 甘肃烟草工业有限责任公司 A kind of preparation method of matrimony vine essence and the application in cigarette
CN109275952A (en) * 2018-12-06 2019-01-29 武汉纺织大学 A kind of preparation method of compound cigarette filter
CN109275953A (en) * 2018-12-06 2019-01-29 武汉纺织大学 A kind of preparation method of fiber base cigarette filter
CN111374345A (en) * 2018-12-29 2020-07-07 贵州中烟工业有限责任公司 Method for preparing Maillard reaction product by using medlar extract, Maillard reaction product and application
CN111808681A (en) * 2020-07-20 2020-10-23 广西中烟工业有限责任公司 Preparation method of lycium ruthenicum murr spice for cigarettes and application of lycium ruthenicum murr spice in cigarettes

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CN104830530A (en) * 2015-04-27 2015-08-12 湖北中烟工业有限责任公司 Preparation method of red date Maillard reactant for cigarettes

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CN104830530A (en) * 2015-04-27 2015-08-12 湖北中烟工业有限责任公司 Preparation method of red date Maillard reactant for cigarettes

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108424814A (en) * 2018-03-20 2018-08-21 甘肃烟草工业有限责任公司 A kind of preparation method of matrimony vine essence and the application in cigarette
CN109275952A (en) * 2018-12-06 2019-01-29 武汉纺织大学 A kind of preparation method of compound cigarette filter
CN109275953A (en) * 2018-12-06 2019-01-29 武汉纺织大学 A kind of preparation method of fiber base cigarette filter
CN109275953B (en) * 2018-12-06 2021-02-02 武汉纺织大学 Preparation method of fiber-based cigarette filter
CN109275952B (en) * 2018-12-06 2021-02-02 武汉纺织大学 Preparation method of composite cigarette filter tip
CN111374345A (en) * 2018-12-29 2020-07-07 贵州中烟工业有限责任公司 Method for preparing Maillard reaction product by using medlar extract, Maillard reaction product and application
CN111808681A (en) * 2020-07-20 2020-10-23 广西中烟工业有限责任公司 Preparation method of lycium ruthenicum murr spice for cigarettes and application of lycium ruthenicum murr spice in cigarettes

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