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CN106198809B - A kind of flat-flavor flue-cured tobacco identification method based on activity threshold - Google Patents

A kind of flat-flavor flue-cured tobacco identification method based on activity threshold Download PDF

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CN106198809B
CN106198809B CN201610596555.6A CN201610596555A CN106198809B CN 106198809 B CN106198809 B CN 106198809B CN 201610596555 A CN201610596555 A CN 201610596555A CN 106198809 B CN106198809 B CN 106198809B
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flue
flavor
cured tobacco
activity threshold
tobacco
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CN106198809A (en
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马宇平
陈芝飞
杨靖
孙志涛
蔡莉莉
芦昶彤
李国政
李成刚
毛多斌
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China Tobacco Henan Industrial Co Ltd
Zhengzhou University of Light Industry
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China Tobacco Henan Industrial Co Ltd
Zhengzhou University of Light Industry
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography

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Abstract

The invention belongs to flue-cured tobacco technical fields, and in particular to a kind of flat-flavor flue-cured tobacco identification method based on activity threshold.This method includes that tobacco leaf suction, granule phase substance trapping, aroma component qualitative and quantitative analysis, activity threshold calculate adduction, result judgement.The present invention is using Guizhou Province and Xunyang County, shaanxi Province, Chongqing WuLong area flue-cured tobacco as carrier, the note type of different flavor matters in its flue gas system, the threshold condition of different aroma components are studied and screened, finally using belong to the flavor matter of same note activity threshold adduction size of data as measurement index, to specify the main body note of flue gas system and odor type has been determined.And then based on this, a kind of identification method of flat-flavor flue-cured tobacco based on activity threshold is established.Compared with prior art, it is easy, quickly to include determination method by the present invention, determines objective, the reliable advantage of result, also the judgement for other odor types of flue-cured tobacco and other types tobacco different flavor provides reference and reference.

Description

A kind of flat-flavor flue-cured tobacco identification method based on activity threshold
Technical field
The invention belongs to flue-cured tobacco technical fields, and in particular to a kind of flat-flavor flue-cured tobacco identification side based on activity threshold Method.
Background technique
Flue-cured tobacco is with a long history in China's growing and cultivation, and planting range is extensive, is important one of the industrial crops in China.Weather It is different from the ecological factors such as soil, so that China's tobacco aroma type is generally divided into Luzhou-flavor, delicate fragrance type and centre compared with horn of plenty Odor type.Due to the difference of each cigarette district ecological condition, tobacco leaf odor type style and features also there is notable difference.Flue-cured tobacco flavor types are cigarette The important evidence of the purchasing of raw materials and cigarette composition design need to be to each ecotope tobacco leaf wind in order to show different-style characteristic tobacco Lattice characteristic carries out accurate evaluation and positioning, meets Chinese-style cigarette brand to the stabilization supply requirement of core material with this, ensures The sustainable development of leaf tobacco production.Therefore, the research of flue-cured tobacco flavor types is paid more and more attention, odor type already becomes characteristic tobacco A kind of type code, raw material of the tobacco leaf of different flavor style in cigarette industry it is transregional combination and tobacco leaf formulation played in Ever more important is acted on, and has become the hot issue in current tobacco scientific research.
Tobacco leaf odor type is also related to weather, landform, soil and alcoholization modulation etc. in addition to having outside the Pass with hereditary capacity, most Determine flue-cured tobacco flavor types eventually is the chemical component of flue-cured tobacco and composition, content and the ratio of flavor matter.Currently, to flue-cured tobacco flavor types Differentiate mainly using traditional sensory evaluating smoking or physico-chemical analysis method.The former is this multiple by human body direct feeling flue-cured tobacco Miscellaneous system, it is desirable that the expert that smokes panel test must have a large amount of industry background knowledge and experience abundant of smokeing panel test, by factor and individual subjective factor It is affected with experience etc.;The latter's detection project is various, is related to total reducing sugar, reduced sugar, total nitrogen, protein, total alkaloid, chlorine, shallow lake The chemical components such as powder, minerals and Main Fragrance, operating process is time-consuming, cumbersome, needs a large amount of instrument and equipment, detects It is costly, and the correlation between various indexs is very complicated, is difficult to promote and apply in actual production.Therefore, seek one kind Accurately, the detection method for fast and effeciently identifying flue-cured tobacco flavor types is particularly important.
Summary of the invention
Present invention aims to overcome that flue-cured tobacco style differentiate in existing traditional sensory evaluating smoking's method by factor and individual subjective factor and The defect that experience etc. is affected;It puts forth effort on simultaneously and overcomes existing physico-chemical analysis method operating process time-consuming, cumbersome, need a large amount of Instrument and equipment, detection project is more, and testing cost is high, is difficult to the defect promoted and applied in actual production.Based on object above, originally Invention is weighing apparatus with the activity threshold size of each note in flue-cured tobacco system by the activity threshold concept of flavor matter in reference flue-cured tobacco Figureofmerit specifies the main body note of flue gas system and determines odor type, so that it is roasting to establish a kind of flat-flavor based on activity threshold The identification method of cigarette.
To achieve the above object, the present invention adopts the following technical scheme that.
A kind of flat-flavor flue-cured tobacco identification method based on activity threshold, includes the following steps:
(1) content of representative flavor matter in flue gas is measured, specifically:
Firstly, cured tobacco leaf is rolled into single-tobacco-typed cigarette, smoking machine is placed according to national standard condition (GB/T 19609-2004) On aspirated, in aspiration procedure, the granule phase substance in main flume is collected;Preferably Cambridge is used to filter when collecting granule phase substance Piece is trapped;
Secondly, carry out the processing such as Simultaneous distillation-extraction, pickling and alkali cleaning to granule phase substance respectively, with obtain alkalinity, it is acid and GC-MS and GC-Q-TOF second order ms counter point is respectively adopted to obtained flavor component, thus to flue-cured tobacco in neutral flavor constituents Main aroma component carries out qualitative analysis in flue gas;
Finally, determining the threshold value of correlation aroma component, and screen threshold value≤1.0 × 10-3Aroma component as representative Aroma component carries out quantitative analysis using internal standard method, determines content of the representativeness aroma component in flue gas;
Identified representativeness aroma component has 66 kinds, and affiliated note type and its threshold value are as shown in the table:
(2) representative flavor matter activity threshold is determined
Firstly, according to the content of the representative aroma component measured in step (1), respectively with it is various it is representative cause it is fragrant at Divide the content in flue gas divided by its threshold value, obtains the activity threshold of various representative aroma components;
Secondly, aroma component is carried out note ownership according to odor characteristic, and by the active threshold of identical note flavor matter Value sums up;
Finally, the main body note feature that tobacco aroma is determined according to adduction numerical values recited, so that it is determined that flue-cured tobacco type;If The note based on fragrant and sweet, radix aucklandiae then can determine that flue-cured tobacco is flat-flavor flue-cured tobacco.
Preliminary studies have shown that flat-flavor flue-cured tobacco be flue-cured tobacco this perfume ((also referred to as hay is fragrant, be it is a kind of with burley tobaccos and The comprehensive impression of Turkish tobaccos in contrast)) on the basis of, the odor characteristic of note, just fragrant and sweet based on just fragrant and sweet and radix aucklandiae Rhythm is prominent.And flue gas main body note determines its affiliated odor type.The ratio between content Yu threshold value of various flavor matters are known as in flue-cured tobacco Activity threshold of the substance in flue-cured tobacco system.The bigger flavor matter of activity threshold, the effect to tobacco aroma feature is shown It is stronger, contribution it is bigger, vice versa.Together by the activity threshold adduction of identical note flavor matter, big according to adduction quantity Small to can determine whether which note is flue-cured tobacco main body note, which is secondary note, thus can determine the odor type classification of flue-cured tobacco.
It is domestic mainly to originate in Guizhou Province and Xunyang County, shaanxi Province, Chongqing WuLong area for the flat-flavor flue-cured tobacco place of production.Cause This, inventor is using Guizhou Province and Xunyang County, shaanxi Province, Chongqing WuLong area flue-cured tobacco as carrier, to belong to same note in flue gas system It is measurement index that flavor matter activity threshold, which sums it up size of data, specifies the main body note of flue gas system and determines odor type, thus Establish a kind of identification method of flat-flavor flue-cured tobacco based on activity threshold.
Compared with prior art, major technique advantage of the invention is embodied in:
1, determination method relative ease, and more quickly;Relative to survey project in traditional physico-chemical analysis method more, index it Between correlation is complicated, testing cost is high defect, the present invention innovatively introduces activity threshold in the differentiation of tobacco aroma style Standard, and need to only measure the content of main flavor matter in flue-cured tobacco, obtain its activity threshold, according to adduction population size It is accurate to determine flue-cured tobacco flavor types, thus utilize the odor type of the invention that can relatively more easy and quickly determine flue-cured tobacco;
2, determine that result is not affected by human factors, it is more objective and reliable;Determination method of the invention preferably overcomes Existing flue-cured tobacco style differentiate employed in sensory evaluating smoking's method excessively relies on factor and individual subjective factor and subjective experience influence it is scarce Fall into, determine result it is more objective and reliable, while have it is preferably comparative, while also be other odor types of flue-cured tobacco and other types The judgement of tobacco different flavor provides reference and reference.
Specific embodiment
Technical solution of the present invention is further discussed in detail below with reference to embodiment, is introducing specific embodiment Before, tobacco and detection device situation used in following embodiments is briefly briefly discussed below.
Tobacco material: zunyi, guizhou C3F tobacco leaf, Xunyang County, shaanxi Province C2F tobacco leaf, Chongqing WuLong B3F tobacco leaf are by cigarette in Henan Group Co., Ltd provides;
Normal process cigarette will be pressed into cigarette after corresponding pure tobacco leaf chopping;
Detection device:
RM20H smoking machine, German Borgwaldt kc company;
6890/5973N type Gc/ms Analyser, Agilent company, the U.S.;
7200 GC-Q-TOF second order ms, Agilent company, the U.S..
Embodiment 1
The present embodiment is determined by taking zunyi, guizhou C3F tobacco leaf as an example its odor type that specific decision process is as follows.
Flat-flavor flue-cured tobacco identification method based on activity threshold, specific determination step are as follows.
(1) content of representative flavor matter in flue gas is measured, specifically:
Firstly, zunyi, guizhou C3F tobacco leaf is rolled into single-tobacco-typed cigarette, then upper smoking machine is aspirated under the conditions of national standard; In aspiration procedure, the granule phase substance in main flume is collected;To ensure the collecting effect to granule phase substance, 20 single-tobacco-typed cigarettes Granule phase substance is trapped with a filter disc;The cambridge filter in trap is taken out after cigarette smoking is complete, and with absorbent cotton wiped clean, one It rises and is put into 500mL conical flask, it is one group that 3 filter discs are put in each conical flask.
Secondly, carry out the processing such as Simultaneous distillation-extraction, pickling and alkali cleaning to granule phase substance respectively, with obtain alkalinity, it is acid and Neutral flavor constituents, specifically:
1. Simultaneous distillation-extraction is handled: 3 groups of cambridge filters being placed in 1000mL round-bottomed flask, are then added 500mL's Ultrapure water carries out Simultaneous distillation-extraction, 2.5 h of extraction time with the methylene chloride of 100mL chromatographically pure;
2. alkaline flavor component sample preparation: after the completion of distillation extraction, obtained extract liquor first being used 5% (volume basis Than similarly hereinafter) aqueous hydrochloric acid solution washing (20 mL × 5), merge hydrochloric acid cleaning solution, and adjust pH value with 5% sodium hydrate aqueous solution With chromatographic grade methylene chloride extraction (20 mL × 3) after to 10.0, merges organic phase and obtain alkaline solution, enough anhydrous sulphur is added Sour sodium freeze-drying lyophilization is stayed overnight and is concentrated into 1mL;
3. acid flavor component sample preparation: water-soluble with 5% sodium hydroxide by the dichloromethane extract after chlorohydric acid pickling Liquid, which washs (20 mL × 5) and merges sodium hydroxide afterwards, washs liquid, and washs adjusting pH value to using color after 1.0 with 5% aqueous hydrochloric acid solution Spectrum level methylene chloride extracts (20 mL × 3), merges organic phase and obtains alkaline solution, enough anhydrous sodium sulfate freeze-drying lyophilizations are added It stays overnight and is concentrated into 1mL;
4. neutral flavor constituents sample preparation: the methylene chloride successively after hydrochloric acid and sodium hydrate aqueous solution washing is extracted Taking liquid is neutral flavor constituents, and enough anhydrous sodium sulfate freeze-drying lyophilizations are added and stays overnight and is concentrated into 1mL;
GC-MS and GC-Q-TOF second order ms counter point is respectively adopted to alkalinity, acidity and neutral flavor constituents are obtained, To carry out qualitative analysis to aroma component main in flue-cured tobacco.
Finally, being noted down by reference to existing literature, with threshold value≤1.0 × 10-3As screening criteria, determine that representative cause is fragrant Ingredient has 66 kinds, and using internal standard method, it is (specific to survey to carry out quantitative analysis to content of this 66 kinds representative aroma components in flue gas Determine result and see below table 1).
(2) representative flavor matter activity threshold is determined
Firstly, according in step (1) to the assay of this 66 kinds representative aroma components as a result, being removed respectively with its content With its threshold value, obtain the activity threshold of various representative aroma components (specific calculated result sees below table 1);
Secondly, according to odor characteristic by this 66 kinds representative aroma components be attributed to fragrant camerlsed, nut, clear (blueness) perfume, 11 kinds of notes such as fruity, the fragrant and sweet, fragrance of a flower, milk, herbal, cream perfume, radix aucklandiae, sour;Belong to according to its note, by identical note The activity threshold of flavor matter sums up;
Finally, the activity threshold of 11 kinds of notes in zunyi, guizhou C3F tobacco leaf is obtained according to adduction numerical value, and then determines flue-cured tobacco Main body note feature in fragrance, so that it is determined that flue-cured tobacco type.
Assay result and activity threshold calculated result such as the following table 1 of the above-mentioned 66 kinds representative aroma components in flue gas It is shown,
Table 1:
By table 1 it can be concluded that the activity threshold of each note are as follows: fragrant and sweet is 9.03 × 108, radix aucklandiae be 7.75 × 108, fruity be 2.89×108, the fragrance of a flower be 1.49 × 108, camerlsed be 1.42 × 108, fragrant clear (blueness) be 1.12 × 108, nut perfume (or spice) be 4.87 × 107, milk be 1.98 × 107, herbal be 6.13 × 106, sour be 2.94 × 106, cream perfume (or spice) be 1.97 × 107
As can be seen from the above results, zunyi, guizhou C3F odor characteristic is the note based on fragrant and sweet, radix aucklandiae, is aided with fruit Perfume, the fragrance of a flower, caramel, clear (blueness) fragrant note;Therefore, it can determine that zunyi, guizhou C3F tobacco leaf is flat-flavor flue-cured tobacco.
Embodiment 2
The present embodiment is determined by taking Xunyang County, shaanxi Province C2F tobacco leaf as an example its odor type that the operation of specific decision process is same Embodiment 1.It is only just related to determine that result brief explanation is described as follows.
After aroma component analysis in granule phase substance, with reference to existing literature, equally with threshold value≤1.0 × 10-3It is marked as screening Standard, it is final to determine that representative aroma component has 66 kinds (type is with embodiments 1), using internal standard method, to 66 kinds it is representative cause it is fragrant at The content in flue gas is divided to be determined;And the activity threshold of 66 kinds of representative aroma components is calculated respectively.
Finally, according to odor characteristic by 66 kinds of representative aroma components be attributed to clear (blueness) perfume, fruity, fragrant and sweet, nut is fragrant, 11 kinds of notes such as camerlsed, the fragrance of a flower, milk, herbal, cream perfume, radix aucklandiae, sour;
It is calculated by adduction, the activity threshold of 11 kinds of notes of Xunyang County, shaanxi Province C2F tobacco leaf is as follows:
Radix aucklandiae is 8.57 × 108, it is fragrant and sweet be 8.81 × 108, fruity be 3.28 × 108, the fragrance of a flower be 2.07 × 108, clear (blueness) Perfume is 1.53 × 108, camerlsed be 1.13 × 108, nut perfume (or spice) be 6.79 × 107, milk be 1.68 × 107, herbal 7.55 ×106, sour be 3.19 × 106, cream perfume (or spice) be 1.06 × 107
It may determine that by result above, Xunyang County, shaanxi Province C2F tabacco fragrance is characterized in the note based on fragrant and sweet, radix aucklandiae, auxiliary With fruity, the fragrance of a flower, clear (blueness) perfume, camerlsed note.Therefore, it can determine that Xunyang County, shaanxi Province C2F tobacco leaf is flat-flavor flue-cured tobacco.
Embodiment 3
The present embodiment determines its odor type, the operation of specific decision process is same by taking the WuLong's B3F tobacco leaf of Chongqing as an example Embodiment 1.It is only just related to determine that result brief explanation is described as follows.
After aroma component analysis in granule phase substance, with reference to existing literature, equally with threshold value≤1.0 × 10-3It is marked as screening Standard, it is final to determine that representative aroma component has 66 kinds (type is with embodiments 1), using internal standard method, to 66 kinds it is representative cause it is fragrant at The content in flue gas is divided to be determined;And the activity threshold of 66 kinds of representative aroma components is calculated respectively.
Finally, according to odor characteristic by 66 kinds of representative aroma components be attributed to clear (blueness) perfume, fruity, fragrant and sweet, nut is fragrant, 11 kinds of notes such as camerlsed, the fragrance of a flower, milk, herbal, cream perfume, radix aucklandiae, sour;
It is calculated by adduction, the activity threshold of 11 kinds of notes of Chongqing WuLong's B3F tobacco leaf is as follows:
Fragrant and sweet is 9.52 × 108, radix aucklandiae be 8.91 × 108, fruity be 4.01 × 108, the fragrance of a flower be 3.28 × 108, clear (blueness) Perfume is 1.46 × 108, camerlsed be 1.19 × 108, nut perfume (or spice) be 5.33 × 107, milk be 2.51 × 107, herbal 5.23 ×106, sour be 2.87 × 106, cream perfume (or spice) be 1.29 × 107
As can be seen from the above results, Chongqing WuLong B3F odor characteristic is the note based on fragrant and sweet, radix aucklandiae, is aided with fruit Perfume, the fragrance of a flower, clear (blueness) perfume, camerlsed note.Therefore, it can determine that Chongqing WuLong's B3F tobacco leaf is flat-flavor flue-cured tobacco.

Claims (2)

1. a kind of flat-flavor flue-cured tobacco identification method based on activity threshold, which is characterized in that include the following steps:
(1) content of representative flavor matter in flue gas is measured, specifically:
Firstly, cured tobacco leaf is rolled into single-tobacco-typed cigarette, it is placed on smoking machine and is aspirated according to national standard condition, in aspiration procedure, Granule phase substance in main flume is collected;
Secondly, carry out alkali cleaning, pickling and methylene chloride extraction respectively to granule phase substance, with obtain acid, alkalinity and neutral flavor at Point, GC-MS and GC-Q-TOF second order ms counter point is respectively adopted to obtained flavor component, thus to main in flue-cured tobacco Aroma component carries out qualitative analysis;
Finally, determining the threshold value of correlation aroma component, and screen threshold value≤1.0 × 10-3Aroma component as it is representative cause it is fragrant Ingredient carries out quantitative analysis using internal standard method, determines content of the representativeness aroma component in flue gas;
The representativeness aroma component has 66 kinds, and affiliated note type and its threshold value are as shown in the table:
Continuous upper table:
Continuous upper table:
(2) representative flavor matter activity threshold is determined
Firstly, being existed respectively with various representative aroma components according to the content of the representative aroma component measured in step (1) Content in flue gas obtains the activity threshold of various representative aroma components divided by its threshold value;
Secondly, according to odor characteristic by aroma component carry out note ownership, and by the activity threshold of identical note flavor matter into Row adduction;
Finally, the main body note feature of tobacco aroma is determined according to adduction numerical values recited, if with fragrant and sweet, radix aucklandiae for main body note Rhythm then can determine that flue-cured tobacco is flat-flavor flue-cured tobacco.
2. the flat-flavor flue-cured tobacco identification method based on activity threshold as described in claim 1, which is characterized in that collect granule phase substance Shi Caiyong cambridge filter is trapped.
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CN111554364A (en) * 2020-04-26 2020-08-18 武汉市第一医院 Traditional Chinese medicine prescription information detection method and detection system for clinical treatment of rheumatoid arthritis
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