CN107894413A - A kind of three-dimensional fluorescence detection method of flavouring essence for tobacco quality - Google Patents
A kind of three-dimensional fluorescence detection method of flavouring essence for tobacco quality Download PDFInfo
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- CN107894413A CN107894413A CN201711090746.6A CN201711090746A CN107894413A CN 107894413 A CN107894413 A CN 107894413A CN 201711090746 A CN201711090746 A CN 201711090746A CN 107894413 A CN107894413 A CN 107894413A
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- 241000208125 Nicotiana Species 0.000 title claims abstract description 38
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000001917 fluorescence detection Methods 0.000 title claims abstract description 15
- 230000005284 excitation Effects 0.000 claims abstract description 30
- 238000001228 spectrum Methods 0.000 claims abstract description 20
- 238000005070 sampling Methods 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 238000002189 fluorescence spectrum Methods 0.000 claims abstract description 6
- 239000000796 flavoring agent Substances 0.000 claims abstract description 5
- 238000004458 analytical method Methods 0.000 claims abstract description 4
- 235000013355 food flavoring agent Nutrition 0.000 claims abstract description 4
- 238000013441 quality evaluation Methods 0.000 claims description 2
- 238000012921 fluorescence analysis Methods 0.000 abstract description 4
- 235000019504 cigarettes Nutrition 0.000 description 12
- 238000001514 detection method Methods 0.000 description 8
- 235000013599 spices Nutrition 0.000 description 7
- 238000012360 testing method Methods 0.000 description 4
- 238000001506 fluorescence spectroscopy Methods 0.000 description 3
- 230000010354 integration Effects 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 230000005622 photoelectricity Effects 0.000 description 3
- 238000012372 quality testing Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000001303 quality assessment method Methods 0.000 description 2
- 230000001953 sensory effect Effects 0.000 description 2
- 210000000697 sensory organ Anatomy 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000021466 carotenoid Nutrition 0.000 description 1
- 150000001747 carotenoids Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000001394 metastastic effect Effects 0.000 description 1
- 206010061289 metastatic neoplasm Diseases 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
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- Health & Medical Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
A kind of three-dimensional fluorescence detection method of flavouring essence for tobacco quality, comprises the following steps：Step 1: batch sampling is carried out to the different production batch flavouring essence for tobaccos deposited according to standard；Step 2: carrying out aesthetic quality's judgement according to Standard to above-mentioned sampling sample, take 5 samples to carry out three-dimensional fluorescence detection and analysis after qualified and obtain three-dimensional fluorescence spectrum data；Step 3: com-parison and analysis is carried out to three-dimensional fluorescence spectrum data, remove interference signal, choose the data in peak signal scope >=10%, determine 4~10 groups of maximum fluorescence emissions and absorb data group as normal data group, on the basis of above-mentioned normal data group, standard and fluoroscopic examination error are prepared according to essence, determine qualified essence standard fluorescence strength range；Step 4: carrying out three-dimensional fluorescence scanning under similarity condition to essence and flavoring agent to be measured, judge whether the batch essence is qualified when corresponding to peak height intensity whether in standard fluorescence strength range according to excitation/emission in the three-dimensional fluorescence scanning spectra of essence sample.
Description
Technical field
The present invention relates to flavouring essence for tobacco detection technique field, specifically a kind of three-dimensional fluorescence detection side of flavouring essence for tobacco quality
Method.
Background technology
In Modern cigarette industry industry, the addition shapeable of essence spice for cigarette and reinforcing cigarette product style characteristic, improve
And lift the aesthetic quality of cigarette product.Essence spice for cigarette is typically using extract, the compound for meeting state related requirements
One or more allotments obtain.The quality of quality of flavoring essence for tobacco influences cigarette quality to a certain degree.
The main component of essence spice for cigarette is water, ethanol, propane diols equal solvent.Industry examination criteria using organoleptic indicator as
It is main, such as the comparison of outward appearance, clarity, miscible degree, aroma quality, flavor quality and standard sample；And physical and chemical index is combined, including
Relative density, refraction index, acid number, volatile ingredient total amount etc..
It is quick in order to detect, and result is accurate, Chinese patent CN201310047819.9 discloses one kind and uses near-infrared
Technology is to the method for flavouring essence for tobacco quality testing, the threshold by data processing and with predetermined essence spice for cigarette quartile length
Value, obtains the quality of testing sample.Chinese patent CN201210362171.X discloses flavouring essence for tobacco quality in a kind of storage period
Detection method, by flavouring essence for tobacco carry out chromatography, establish regression model matrix, obtain the preservation situation of testing sample
And quality condition.The above method is by being detected to crucial inherent index and data analysis, obtaining essence and flavoring agent quality
Situation.But essence spice for cigarette is as COMPLEX MIXED objects system, in the more difficult reflection system of near-infrared spectrum technique it is crucial into
Divide information, and the deficiencies of wasting time and energy then be present in chromatography.
The content of the invention
For deficiencies of the prior art, the present invention provides a kind of three-dimensional fluorescence detection side of flavouring essence for tobacco quality
Method, it is respectively provided with using flavonoids, carotenoid, phenols, the key aroma material such as vegetable soda contained in essence spice for cigarette
Characteristic absorption and fluorescent characteristic, three-dimensional fluorescence analysis is carried out to essence spice for cigarette using detection technique of fluorescence, it can be obtained
The fluorescence information of middle key component, efficient and sensible, there is preferable application value.
The invention provides a kind of three-dimensional fluorescence detection method of flavouring essence for tobacco quality, comprise the following steps：
Step 1: carrying out batch sampling to the different production batch flavouring essence for tobaccos deposited according to standard, 5~10 are sampled；
Step 2: carrying out aesthetic quality's judgement according to Standard to above-mentioned sampling sample, 5 samples are taken to carry out after qualified
Three-dimensional fluorescence detection and analysis obtain three-dimensional fluorescence spectrum data；
Step 3: three-dimensional fluorescence spectrum data are carried out with com-parison and analysis, removal interference signal, selection peak signal scope >=
Data in 10%, determine 4~10 groups of maximum fluorescence emissions and absorb data group as normal data group, with above-mentioned normal data
On the basis of group, standard and fluoroscopic examination error are prepared according to essence, determine qualified essence standard fluorescence strength range；
It is three-dimensional glimmering when essence sample Step 4: carry out three-dimensional fluorescence scanning under similarity condition to essence and flavoring agent to be measured
When excitation/emission corresponds to peak height intensity in standard fluorescence strength range in optical scanning collection of illustrative plates, judge that the batch essence quality is closed
Lattice；When excitation/emission corresponds to peak height intensity not in standard value range in three-dimensional fluorescence scanning spectra, sense organ need to be further carried out
Quality evaluation.
Further, the interference signal includes scattering, times half-wave voltage signal.
Further, if in the step 4 in three-dimensional fluorescence scanning spectra collection of illustrative plates Plays excitation/emission to being not present,
Or there is the strong signal of other excitation/emissions, then judge that the batch essence is off quality.
The beneficial effects of the present invention are：
1st, in flavouring essence for tobacco key substance content typically in ppm~ppb levels, general physical and chemical index such as relative density, refractive power
The more difficult reactions change situation such as index, acid number, volatile ingredient total amount.And fluorescent technique has the advantages that highly sensitive, metastatic.
It is the features such as sensitive, single-minded based on fluoroscopic examination of the present invention, more accurate for the Partial key material of flavouring essence for tobacco, quality testing
Really；
2nd, the present invention uses detection technique of fluorescence, and quantity of sampling quantity is less, it is not necessary to and complicated pretreatment process, cost is low,
Detection speed is fast, suitable for daily multiple batches of quality testing；
3rd, the data obtained of the present invention has preferable selectivity, data processing using specific wavelength and respective intensities as data
Measure small.
Brief description of the drawings
Fig. 1 is flavouring essence for tobacco A three-dimensional fluorescence scanning spectra；
Fig. 2 is flavouring essence for tobacco B three-dimensional fluorescence scanning spectra；
Fig. 3 is flavouring essence for tobacco C three-dimensional fluorescence scanning spectra.
Embodiment
Below in conjunction with specific embodiment, the technical scheme in the present invention is described, but present disclosure is not only
It is limited only to embodiment.
Embodiment 1：Flavouring essence for tobacco A
A kind of three-dimensional fluorescence detection method of flavouring essence for tobacco quality, comprises the following steps：
Batch sampling is carried out to the different production batch flavouring essence for tobaccos deposited according to standard, samples 8.
National Standard of the People's Republic of China GB5606.4-2005 is used according to the present invention to above-mentioned sampling sample《Cigarette
4th part sense organ technical requirements》It is required that carrying out aesthetic quality's judgement, 5 samples are taken to carry out three-dimensional fluorescence detection and analysis after qualified.
Fluoroscopic examination, scanning wavelength scope are carried out using F-7000FL Spectrophotometer：Excite 200-
600nm, transmitting 200-600nm, sweep spacing 3nm, sweep speed 240nm/min, excitation/emission width is 5.0nm, photoelectricity
Double pipe pressure 700V, and peak integration integrates for right angle, obtains three-dimensional fluorescence scanning spectra (see Fig. 1) and tables of data 1.
The flavouring essence for tobacco A three-dimensional fluorescence scan data tables of table 1
Remove scattering and times wavelength etc. and disturb data, obtain following excitation/emission data.Selection 248.0/422.0,
302.0/422.0,347.0/419.0,350.0/422.0 equal excitation/transmitting data group, 5 groups of samples are carried out three-dimensional glimmering
Optical scanning, average to obtain fluorescence intensity, thus establish normal data group, such as table 2 below：
The flavouring essence for tobacco A standard three-dimensional fluorescence datas of table 2
| EX(nm) | EM(nm) | Height(Data) |
| 248 | 422 | 1444 |
| 302 | 422 | 1431 |
| 347 | 419 | 869.4 |
| 350 | 422 | 868.7 |
From the normal data of screening can be seen that flavouring essence for tobacco A principal excitation wavelength 248,302,347,350nm,
Corresponding dominant emission wavelength is 422,422,419,422nm.
Error and essence production standard error are scanned according to three-dimensional fluorescence, the standard detection scope for determining qualified essence is mark
Quasi- peak height intensity ± 10%.When 248.0/422.0,302.0/422.0,347.0/ in the three-dimensional fluorescence scanning spectra of essence sample
419.0th, when 350.0/422.0 equal excitations/transmitting corresponds to peak height intensity and standard value deviation≤10%, batch essence A is judged
It is up-to-standard；As 248.0/422.0,302.0/422.0,347.0/419.0,350.0/422.0 in three-dimensional fluorescence scanning spectra
Equal excitation/transmitting corresponds to peak height intensity and standard value deviation >=10%, need to further carry out sensory quality assessment.Work as three-dimensional fluorescence
248.0/422.0,302.0/422.0,347.0/419.0,350.0/422.0 equal excitation/transmitting pair in collection of illustrative plates in scanning spectra
It is not present or the strong signal of other excitation/emissions (be above standard signal intensity) occurs, then the batch essence is off quality.
Embodiment 2：Flavouring essence for tobacco B
A kind of three-dimensional fluorescence detection method of flavouring essence for tobacco quality, comprises the following steps：
Batch sampling is carried out to the different production batch flavouring essence for tobaccos deposited according to standard, samples 6.
Aesthetic quality's judgement is carried out according to Standard to above-mentioned sampling sample, takes 5 samples to carry out after qualified three-dimensional glimmering
Light tests and analyzes.
Fluoroscopic examination, scanning wavelength scope are carried out using F-7000FL Spectrophotometer：Excite 200-
600nm, transmitting 200-600nm, sweep spacing 3nm, sweep speed 240nm/min, excitation/emission width is 5.0nm, photoelectricity
Double pipe pressure 700V, and peak integration integrates for right angle, obtains three-dimensional fluorescence scanning spectra (see Fig. 2) and tables of data 3.
The flavouring essence for tobacco B three-dimensional fluorescence scan data tables of table 3
Remove scattering and times wavelength etc. and disturb data, obtain following excitation/emission data.Selection 203.0/365.0,
221.0/308.0,224.0/305.0,257.0/395.0,260.0/398.0 equal excitation/transmitting are to data group, to 5 groups of sampling
Sample carries out three-dimensional fluorescence scanning, averages to obtain fluorescence intensity, thus establishes normal data, such as table 4 below：
The flavouring essence for tobacco B standard three-dimensional fluorescence data of table 4
| EX(nm) | EM(nm) | Height(Data) |
| 203.0 | 365.0 | 155.1 |
| 221.0 | 308.0 | 211.9 |
| 224.0 | 305.0 | 208.1 |
| 257.0 | 395.0 | 139.3 |
| 260.0 | 398.0 | 138.0 |
Error and essence production standard error are scanned according to three-dimensional fluorescence, the standard detection scope for determining qualified essence is mark
Quasi- peak height intensity ± 15%.When 203.0/365.0,221.0/308.0,224.0/ in the three-dimensional fluorescence scanning spectra of essence sample
305.0th, when 257.0/395.0,260.0/398.0 equal excitation/transmitting correspond to peak height intensity and standard value deviation≤15%, judge
Batch essence B is up-to-standard；When 248.0/422.0,302.0/422.0 in three-dimensional fluorescence scanning spectra, 347.0/419.0,
350.0/422.0 equal excitation/transmitting corresponds to deviation >=15% of peak height intensity and standard value, need to further carry out aesthetic quality and comment
Valency.When 203.0/365.0,221.0/308.0,224.0/305.0,257.0/395.0,260.0/ in three-dimensional fluorescence scanning spectra
398.0 equal excitations/transmitting is in the absence of or there is the strong signal of other excitation/emissions (be above standard signal intensity), then this batch
Secondary essence is off quality.
Embodiment 3：Flavouring essence for tobacco C
A kind of three-dimensional fluorescence detection method of flavouring essence for tobacco quality, comprises the following steps：
Batch sampling is carried out to the different production batch flavouring essence for tobaccos deposited according to standard, samples 10.
Aesthetic quality's judgement is carried out according to Standard to above-mentioned sampling sample, takes 5 samples to carry out after qualified three-dimensional glimmering
Light tests and analyzes.
Fluoroscopic examination, scanning wavelength scope are carried out using F-7000FL Spectrophotometer：Excite 200-
600nm, transmitting 200-600nm, sweep spacing 3nm, sweep speed 240nm/min, excitation/emission width is 5.0nm, photoelectricity
Double pipe pressure 700V, and peak integration integrates for right angle, obtains three-dimensional fluorescence scanning spectra (see Fig. 3) and tables of data 5.
The flavouring essence for tobacco C three-dimensional fluorescence scan data tables of table 5
Remove scattering and times wavelength etc. and disturb data, obtain following excitation/emission data.Selection 218.0/302.0,
227.0/329.0,251.0/314.0,254.0/350.0,254.0/365.0,278.0/305.0,278.0/326.0 etc. swash
Hair/transmitting carries out three-dimensional fluorescence scanning to 5 groups of samples, averages to obtain fluorescence intensity, thus establish mark to data group
Quasi- data, such as table 6 below：
The flavouring essence for tobacco B standard three-dimensional fluorescence data of table 6
| EX(nm) | EM(nm) | Height(Data) |
| 218.0 | 302.0 | 1056 |
| 227.0 | 329.0 | 2142 |
| 251.0 | 314.0 | 740.1 |
| 254.0 | 350.0 | 654.7 |
| 254.0 | 365.0 | 676.6 |
| 278.0 | 305.0 | 834.2 |
| 278.0 | 326.0 | 941 |
Error and essence production standard error are scanned according to three-dimensional fluorescence, the standard detection scope for determining qualified essence is mark
Quasi- peak height intensity ± 20%.
When 218.0/302.0,227.0/329.0 in the three-dimensional fluorescence scanning spectra of essence sample, 251.0/314.0,
254.0/350.0,254.0/365.0,278.0/305.0,278.0/326.0 equal excitation/transmitting corresponds to peak height intensity and standard
When being worth deviation ± 20%, judge that batch essence C is up-to-standard；When 218.0/302.0,227.0/ in three-dimensional fluorescence scanning spectra
329.0th, 251.0/314.0,254.0/350.0,254.0/365.0,278.0/305.0,278.0/326.0 equal excitation/transmitting
Corresponding peak height intensity need to further carry out sensory quality assessment in deviation >=20% of standard value and≤50%.When three-dimensional glimmering
203.0/365.0,221.0/308.0,224.0/305.0,257.0/395.0,260.0/398.0 etc. swash in optical scanning collection of illustrative plates
Deviation >=50% of hair/emission peak high intensity and standard value, or excitation/emission is in the absence of other excitation/emissions occur and believe by force
Number (be above standard signal intensity), then the batch essence is off quality.
The foregoing is only a specific embodiment of the invention, but protection scope of the present invention is not limited thereto, any
Belong to those skilled in the art the invention discloses technical scope in, the change or replacement that can readily occur in, all should
It is included within the scope of the present invention.Therefore, protection scope of the present invention should be defined by scope of the claims.
Claims (3)
1. a kind of three-dimensional fluorescence detection method of flavouring essence for tobacco quality, it is characterised in that comprise the following steps：
Step 1: carrying out batch sampling to the different production batch flavouring essence for tobaccos deposited according to standard, 5~10 are sampled；
Step 2: carrying out aesthetic quality's judgement according to Standard to above-mentioned sampling sample, 5 samples are taken to carry out after qualified three-dimensional
Fluorimetric analysis obtains three-dimensional fluorescence spectrum data；
Step 3: carrying out com-parison and analysis to three-dimensional fluorescence spectrum data, interference signal is removed, chooses peak signal scope >=10%
Interior data, determine 4~10 groups of maximum fluorescence emissions and absorb data group as normal data group, using above-mentioned normal data group as
Benchmark, standard and fluoroscopic examination error are prepared according to essence, determine qualified essence standard fluorescence strength range；
Step 4: three-dimensional fluorescence scanning is carried out under similarity condition to essence and flavoring agent to be measured, when the three-dimensional fluorescence of essence sample is swept
When excitation/emission corresponds to peak height intensity in standard fluorescence strength range in tracing spectrum, judge that the batch essence is up-to-standard；When
Excitation/emission corresponds to peak height intensity not in standard value range in three-dimensional fluorescence scanning spectra, need to further carry out aesthetic quality
Evaluation.
2. the three-dimensional fluorescence detection method of flavouring essence for tobacco quality as claimed in claim 1, it is characterised in that：The interference signal
Including scattering, times half-wave voltage signal.
3. the three-dimensional fluorescence detection method of flavouring essence for tobacco quality as claimed in claim 1, it is characterised in that：In the step 4
If collection of illustrative plates Plays excitation/emission is to being not present or occurring the strong signal of other excitation/emissions in three-dimensional fluorescence scanning spectra,
Then judge that the batch essence is off quality.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101526470A (en) * | 2009-04-22 | 2009-09-09 | 川渝中烟工业公司 | Method for detecting essence for tobacco |
| CN103217408A (en) * | 2013-05-14 | 2013-07-24 | 贵州大学 | Method for identifying two flue-cured tobaccos with different odor types in Guizhou |
| CN105223175A (en) * | 2015-09-28 | 2016-01-06 | 江南大学 | A kind of three-dimensional fluorescence spectrum differentiates the method in aromatic Chinese spirit time in conjunction with Non-negative Matrix Factorization |
| CN105334198A (en) * | 2015-11-14 | 2016-02-17 | 常州大学 | Method for analyzing DOMs (dissolved organic matters) in water on basis of three-dimensional fluorescence spectra |
-
2017
- 2017-11-08 CN CN201711090746.6A patent/CN107894413A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101526470A (en) * | 2009-04-22 | 2009-09-09 | 川渝中烟工业公司 | Method for detecting essence for tobacco |
| CN103217408A (en) * | 2013-05-14 | 2013-07-24 | 贵州大学 | Method for identifying two flue-cured tobaccos with different odor types in Guizhou |
| CN105223175A (en) * | 2015-09-28 | 2016-01-06 | 江南大学 | A kind of three-dimensional fluorescence spectrum differentiates the method in aromatic Chinese spirit time in conjunction with Non-negative Matrix Factorization |
| CN105334198A (en) * | 2015-11-14 | 2016-02-17 | 常州大学 | Method for analyzing DOMs (dissolved organic matters) in water on basis of three-dimensional fluorescence spectra |
Non-Patent Citations (1)
| Title |
|---|
| 雍克岚 等: "烟草三维荧光特征和品质评吸的关系", 《化学研究与应用》 * |
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Application publication date: 20180410 |