CN106404884A - Method for quickly evaluating quality consistency of flavors and fragrances of volatile cigarettes by HS-IMR-MS - Google Patents
Method for quickly evaluating quality consistency of flavors and fragrances of volatile cigarettes by HS-IMR-MS Download PDFInfo
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- CN106404884A CN106404884A CN201611026536.6A CN201611026536A CN106404884A CN 106404884 A CN106404884 A CN 106404884A CN 201611026536 A CN201611026536 A CN 201611026536A CN 106404884 A CN106404884 A CN 106404884A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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Abstract
The invention discloses a method for quickly evaluating quality consistency of flavors and fragrances of volatile cigarettes by HS-IMR-MS (headspace sampler - ion molecule reaction mass spectrometry). The method has the advantages that the response value of ions of a volatile compound in the flavors and fragrances is obtained by a headspace sampler and IMR-MS, a spectrum fingerprint chromatogram is drawn, and the quality consistency of the flavors and fragrances of the cigarettes is quickly evaluated by combining with similarity analysis. The method has the beneficial effects that the volatile ingredient in the flavors and fragrances is visually represented by the spectrum fingerprint chromatogram; the quality consistency of the flavors and fragrances is quickly evaluated by utilizing similarity analysis; the whole process is simple, the implementing is easy, the popularizing is convenient, and the inherent quality of the flavors and fragrances of the cigarettes can be stably and strictly controlled.
Description
Technical field
The present invention relates to essence spice for cigarette evaluation and test technical field, particularly one kind is using HS IMR MS (head space ion
Molecule reacts mass spectrum) the conforming method of Fast Evaluation volatility quality of flavoring essence for tobacco.
Background technology
Essence spice for cigarette is the spice mixt or monomer for tobacco flavoring, has certain fragrance and note, is
Form the crucial additive of cigarette product characteristic.Essence spice for cigarette can project or modified product style in cigarette process, and
Excitant, miscellaneous gas etc. can be improved and inhale taste defect, make flue gas and suitable, mellow and full, cigarette perfume pleases people.
At present, China's tobacco business most industry enterprise is all according to YC/T 145 series standard, by organoleptic indicator
To monitor the quality of essence spice for cigarette with the mensure of physical and chemical index or assessment.Organoleptic indicator's detection is included to essence spice for cigarette
Outward appearance, miscible degree, aroma quality and flavor quality evaluated.Wherein aroma quality evaluation is mainly by sense of smell and comments perfume (or spice),
Whether the aroma quality (include odor type, fragrance deep or light, strong and weak, persistence, miscellaneous gas) of evaluation sample is consistent with standard sample；Fragrance
Performance rating, mainly by quantitative sample and standard sample dilution, is injected separately in pure cigarette or formula cigarette, by smokeing panel test
Whether the flavor quality (including fragrance, coordination, miscellaneous gas, excitant, pleasant impression) that sample evaluated by cigarette is consistent with standard sample.Cigarette is used
The judgement of essence fragrance and aroma quality, due to manually completing, can carry subjective tendency, and more time-consuming.Physical and chemical index is examined
Survey and then include relative density, refraction index, acid number, volatile ingredient total amount mensure etc..Wherein volatile ingredient total amount is to weigh
One important indicator of essence and flavoring agent quality, is the judge to overall volatile component content, but this method can not be to volatility thing
Matter is specifically distinguished discriminating.In addition, standard YC/T 145.11 clearly states, carrying out organoleptic indicator and physical and chemical index inspection
During survey, if flavouring essence for tobacco complex sample, also need it is diluted, pre-treatment work that ultrasonic dissolution and centrifugation are extracted.
Quality of flavoring essence for tobacco decision process is complex time-consuming, and organoleptic indicator easily causes human error.In recent years,
Some new technologies, such as gas-chromatography, gas chromatography combined with mass spectrometry, liquid chromatogram, ultraviolet spectra, near infrared spectrum, Electronic Nose skill
Art etc., is also increasingly used for the quality testing of essence spice for cigarette.
With continuing to bring out of new analytical instrument, for existing essence and flavoring agent quality control present on analytical technology
The problems such as take, need pre-treatment, it is necessary to utilize Modern New instrument analysis technology, researchs and develops method preferably and technology
Quality control for essence spice for cigarette.
Content of the invention
It is an object of the invention to overcoming the shortcoming of prior art, provide one kind quick, comprehensive, stable and without pre-treatment
The conforming method of utilization HS IMR MS Fast Evaluation volatility quality of flavoring essence for tobacco.
The purpose of the present invention is achieved through the following technical solutions：One kind utilizes HS IMR MS Fast Evaluation volatility cigarette
With the method for essence and flavoring agent quality conformance, obtain essence perfume using head-space sampler with IMR MS (ion molecule reaction mass spectrum)
The response (cps) of each volatile compound ion in material, draws mass spectrum fingerprint pattern, to realize cigarette in conjunction with similarity analysis and to use
The Fast Evaluation of essence and flavoring agent quality conformance.
The described conforming method of utilization HS IMR MS Fast Evaluation volatility quality of flavoring essence for tobacco, including with
Lower step：
S1, the preparation of testing sample；
Accurate weighing essence spice for cigarette standard items and each 0.50g of detected sample are placed in the 20mL ml headspace bottle of sealing,
The standard items by blank, weighing and each testing sample are positioned on head-space sampler sample injection disc in order, and in every two
Individual sample room insertion blank ml headspace bottle, for being spaced suction, removes pipeline residual；
S2, HS IMR MS instrumental conditions are arranged, including following sub-step：
S21, headspace autosampler analysis condition are as follows：
Sample equilibration temperature：50 DEG C 150 DEG C, quantitative loop temperature：50 DEG C 150 DEG C, transmission line temperature：50℃‐150℃；
Quantitative loop volume：1mL；Sample equilibration time：2min‐30min；Pressing time：0.2min；Loop fills the time：
0.2min；The loop balance time：0.05min；Sample injection time：1min；
S22, IMR MS analysis condition is as follows：
Open IMR MS system and preheat more than 48 hours, Single Masses method is set in IMR MS work station,
And carry out following parameter setting in the method：
Add each scanning ion that mass number is 16 500 in scanning ion inventory, each ion is set：During scanning
Between：50ms 500ms, MS acquisition pressure：25mbar；
Ionization reagents：Hg, reagent ionization energy：10.44eV；Or ionization reagents：Xe, reagent ionization energy：12.13eV；Or electricity
From reagent：Kr, reagent ionization energy：14.00eV；
Resolution ratio：1amu, cycles samples scanning times：5 times；
S3, mass spectrum fingerprint pattern obtain；
Calculate the mean value of each five scanning results of ion in standard items and testing sample, and deduct corresponding in blank
Ion mean value, obtains final product the response of each ion in standard items and testing sample；With the response of each ion and respective quality number
Mapping, obtains the mass spectrum fingerprint pattern of standard items and testing sample；Standard items can intuitively be understood by mass spectrum fingerprint pattern and treat
Mass number situation contained by test sample product, the response of each of mass spectrogram ion derives from the molecular ion of different compounds
Or intensity sum at this mass number for the fragment ion；
S4, similarity analysis；
Each mass number in standard items and testing sample mass spectrum fingerprint pattern and response are imported SPSS statistical analysis
Software, using Bivariate analysis, calculates standard items and each testing sample mass spectrum fingerprint image using Pearson correlation coefficient method
The similarity of spectrum.
Described employing Pearson correlation coefficient method calculates the similarity of standard items and each testing sample mass spectrum fingerprint pattern
Computing formula be：
R in formula 1xyThe i.e. coefficient correlation of two collection of illustrative plates, x and y represents two mass spectrum fingerprint patterns carrying out similarity-rough set, often
Opening collection of illustrative plates has n data point, wherein xiAnd yiRepresent the response of i-th data point of x and y,WithRepresent x and y spectra count
According to average, r describes the related strong and weak degree of two sample collection of illustrative plates top-stitchings, and the absolute value of r is bigger and is closer to 1,
The similarity degree of two sample collection of illustrative plates is higher, and that is, two sample qualities are more consistent；The absolute value of r is less and is closer to 0, two samples
Product collection of illustrative plates similarity degree is less, and that is, two sample qualities are more inconsistent.
In described step S21, Sample equilibration temperature is：80 DEG C, quantitative loop temperature is：100 DEG C, transmission line temperature is：
120℃.
In described step S21, Sample equilibration time is：5min.
In described step S22, sweep time：300ms.
In described step S22, add each scanning ion that mass number is 16 300 in scanning ion inventory.
A kind of described commenting using the HS IMR MS Fast Evaluation conforming method of volatility quality of flavoring essence for tobacco
Valency object includes spices, perfume base and the essence of cigarette use and non-cigarette, and its formulation includes liquid, tincture, medicinal extract and pressed powder.
As a kind of soft ionization mass-spectrometric technique, its general principle is using different electricity to ion molecule reaction mass spectrum (IMR MS)
There is charge transfer reaction with volatile materials in the gas ion reagent (Hg+, Xe+, Kr+) from energy, make volatile substance molecules
Ionization, thus be isolated by filtration generation signal.From suitable ionization reagents, IMR MS can avoid a large amount of fragment ions
Produce, obtain purer mass spectrometric data.IMR MS has powerful quick analysis advantage, is applied to essence spice for cigarette
Quality control, it becomes possible to provide a kind of quick, is stablized and the method without pre-treatment comprehensively.
The present invention has advantages below：
1st, the present invention selects direct headspace sampling mode, saves sample pretreatment process, easy and simple to handle.
2nd, the present invention is not required to adopt isolation technics, can analyze the Multiple components with different chemical property simultaneously, can achieve
The full analysis of volatile components to sample.
3rd, it is analyzed using IMR MS, quickly and accurately essence and flavoring agent can be carried out within a few minutes or even several seconds
Measure, meet laboratory and quickly analyze demand.
4th, the present invention can intuitively characterize essence and flavoring agent volatile ingredient, in combination with mass spectrum fingerprint by mass spectrum fingerprint pattern
Collection of illustrative plates similarity analysis, analysis process is reproducible, and data source science is reliable, and processing method is simple, the stable standard of result
Really, can be used for quality of flavoring essence for tobacco Conformance Assessment.
Brief description
Fig. 1 is 1 in embodiments of the invention 1#Flavouring essence for tobacco standard items mass spectrum fingerprint pattern.
Fig. 2 is 1 in embodiments of the invention 2#Flavouring essence for tobacco standard items mass spectrum fingerprint pattern.
Fig. 3 is 2 in embodiments of the invention 9#Flavouring essence for tobacco standard items mass spectrum fingerprint pattern.
Fig. 4 is 3 in embodiments of the invention 10#Flavouring essence for tobacco standard items mass spectrum fingerprint pattern.
Specific embodiment
With reference to embodiment and accompanying drawing, the present invention will be further described：
Embodiment 1：
One kind utilizes the conforming method of HS IMR MS Fast Evaluation volatility quality of flavoring essence for tobacco, using head space
Injector obtains the response of each volatile compound ion in essence and flavoring agent with IMR MS, draws mass spectrum fingerprint pattern, in conjunction with
Similarity analysis are realizing the conforming Fast Evaluation of quality of flavoring essence for tobacco.
Specifically include following steps：
Choose 1 respectively#1 A～1 H the flavouring essence for tobacco that the standard items of flavouring essence for tobacco and 8 different manufacturers produce, by with
Lower method is tested.
S1, the preparation of testing sample；
Accurate weighing 1#Flavouring essence for tobacco standard items and each 0.50g of 8 detected samples are placed in the 20mL ml headspace bottle of sealing,
The standard items by blank bottle, weighing and each testing sample order are positioned on head-space sampler sample injection disc, and in every two
The blank ml headspace bottle of individual sample room insertion.
S2, HS IMR MS instrumental conditions are arranged, including following sub-step：
S21, headspace autosampler analysis condition：
Sample equilibration temperature：80 DEG C, quantitative loop temperature：100 DEG C, transmission line temperature：120℃；In practical application, above three
Individual temperature selects in 50 DEG C of 150 DEG C of scopes also dependent on flavouring essence for tobacco proterties；
Quantitative loop volume：1mL；Sample equilibration time：5min, this time is in actual applications also dependent on flavouring essence for tobacco
Shape selects in 2min 30min scope；Pressing time：0.2min；Loop fills the time：0.2min；The loop balance time：
0.05min；Sample injection time：1min；
S22, IMR MS analysis condition is as follows：
Open IMR MS system and preheat more than 48 hours, Single Masses method is set in IMR MS work station,
And carry out following parameter setting in the method：
Add each scanning ion that mass number is 16 300 in scanning ion inventory, also dependent on cigarette in practical application
Select Scanning Section with major volatile constituents in essence in the range of 16 500 mass numbers；Each ion is set：Sweep time：
300ms, selects in the range of 50ms 500ms also dependent on major volatile constituents in flavouring essence for tobacco in practical application；Mass spectrum is adopted
Sample pressure：25mbar；
Ionization reagents：Hg, reagent ionization energy：10.44eV, also dependent on main volatile in flavouring essence for tobacco in practical application
Composition ionization potential scope selects other ionization reagents, such as Xe, reagent ionization energy：12.13eV；Kr, reagent ionization energy：14.00eV；
Resolution ratio：1amu, cycles samples scanning times：5 times.
S3, mass spectrum fingerprint pattern obtain；
Calculate the mean value of each five scanning results of ion in standard items and testing sample, and deduct corresponding in blank
Ion mean value, obtains final product the response of each ion in standard items and testing sample.With the response of each ion and respective quality number
Mapping, obtains standard items and testing sample mass spectrum fingerprint pattern.Wherein, 1#Standard items mass spectrum fingerprint pattern is as shown in Figure 1.
S4, similarity analysis；
Each mass number in standard items and testing sample mass spectrum fingerprint pattern and response are imported SPSS 19.0 count
Analysis software, using Bivariate analysis, is calculated standard items using Pearson correlation coefficient method and is referred to each testing sample mass spectrum
Similarity between line collection of illustrative plates, computing formula (formula 1) is：
R in formula 1xyThe i.e. coefficient correlation of two collection of illustrative plates, x and y represents two mass spectrum fingerprint patterns carrying out similarity-rough set, often
Opening collection of illustrative plates has n data point, wherein xiAnd yiRepresent the response of i-th data point of x and y,WithRepresent x and y spectra count
According to average, r describes the related strong and weak degree of two sample collection of illustrative plates top-stitchings, and the absolute value of r is bigger and is closer to 1,
The similarity degree of two sample collection of illustrative plates is higher, and that is, two sample qualities are more consistent；The absolute value of r is less and is closer to 0, two samples
Product collection of illustrative plates similarity degree is less, and that is, two sample qualities are more inconsistent.
Further, also include method repeatability and investigate step.
For verify above assay method stability, investigated the method in a few days, in the daytime repeatability：Take testing sample 1
E and 1#Standard items, repeat 6 above-mentioned experimental procedures, investigate the in a few days repeatability of the method, and result is as shown in table 1；In 5
In a few days, repeat 1 above-mentioned experimental procedure daily, investigate the repeatability in the daytime of the method, result is as shown in table 2.Table 1 and table
2 result shows, the relative standard deviation of mass spectrum fingerprint pattern similarity is respectively less than 3%.Similarity angle from whole collection of illustrative plates
Investigate, the method has repeatability and stability well.
The in a few days repeatability of table 1 HS IMR MS method investigates result (n=6)
| Coefficient correlation | r1 | r2 | r3 | r4 | r5 | r6 | Mean value | RSD% |
| 1#Mark～1 E | 0.990 | 0.988 | 0.983 | 0.989 | 0.986 | 0.988 | 0.987 | 0.25 |
In the daytime the repeatability of table 2 HS IMR MS method investigates result (n=5)
| Coefficient correlation | r1 | r2 | r3 | r4 | r5 | Mean value | RSD% |
| 1#Mark～1 E | 0.988 | 0.979 | 0.987 | 0.982 | 0.977 | 0.983 | 0.48 |
1#Flavouring essence for tobacco similarity measurement result
The 1 of 8 different manufacturers productions#Flavouring essence for tobacco and 1#Standard items Similarity Measure result is as shown in table 3.Can from table 3
Know, the 1 of 8 manufacturer production#The mass spectrum fingerprint pattern of flavouring essence for tobacco and 1#The each not phase of the similarity of the mass spectrum fingerprint pattern of standard items
With wherein 1 C flavouring essence for tobacco and 1#Standard items similarity is closest, and correlation coefficient r is up to 0.997,1 D flavouring essence for tobacco and 1#Mark
Quasi- product similarity is minimum, and correlation coefficient r is only 0.565.
Table 31#Flavouring essence for tobacco standard items and testing sample similarity (ionization reagents：Hg)
Result verification
With infra-red sepectrometry and sensory evaluating smoking's method determination sample 1 A～1 H and 1#The uniformity of standard items.Infrared analysis is tied
In fruit, 1 C sample and standard items have highest similarity matching value, are 0.996；In Analyses Methods for Sensory Evaluation Results, 1 C sample and 1#Mark
It is the most consistent that standard judges suction experience.The result of infrared spectrum detection and sensory evaluation method all keeps one with the inventive method result
Cause, demonstrate HS IMR MS method to evaluating the conforming correctness of volatility quality of flavoring essence for tobacco, also demonstrate that meanwhile
The method is used for controlling quality of flavoring essence for tobacco, ensures the operability of the quality of cigarette product from source.
Embodiment 2：
For investigating the impact that different ionization reagents are analyzed to sample detection, embodiment 2 is with the difference of embodiment 1：
In step s 2, IMR MS analysis condition is as follows：
Open IMR MS system and preheat more than 48 hours, Single Masses method is set in IMR MS work station,
And carry out following parameter setting in the method：
Add each scanning ion that mass number is 16 300 in scanning ion inventory, each ion is set：During scanning
Between：300ms, MS acquisition pressure：25mbar, ionization reagents：Kr, reagent ionization energy：14.00eV, resolution ratio：1amu, sample
Scan round number of times：5 times.
The result of embodiment 2 is as shown in table 4, and wherein 1#The mass spectrum fingerprint pattern of standard items is as shown in Figure 2.As shown in Table 4,
Embodiment 2 degree similar to Example 1 result of calculation is basically identical；But compared to Fig. 1, the standard mass spectrum fingerprint pattern in Fig. 2 has
Larger difference, m/z is that the response at 153 substantially reduces, and main peak number has reduced, excessive mainly due to ionization energy, causes
Fragment ion increases, therefore selects suitable ionization reagents to be also a need for according to sample.
Table 41#Flavouring essence for tobacco standard items and testing sample similarity (ionization reagents：Kr)
| Testing sample | 1‐A | 1‐B | 1‐C | 1‐D | 1‐E | 1‐F | 1‐G | 1‐H |
| Coefficient correlation (r) | 0.841 | 0.960 | 0.998 | 0.493 | 0.977 | 0.902 | 0.966 | 0.957 |
Embodiment 35：
Implemented according to embodiment 1, and adjusted accordingly in the following areas：
In order to investigate the impact to testing result for the different Sample equilibration temperature, embodiment 3 adopts Sample equilibration temperature 60 C,
Embodiment 4 adopts 100 DEG C of Sample equilibration temperature, and embodiment 5 adopts 120 DEG C of Sample equilibration temperature, under different equilibrium temperatures, than
Compared with the similarity of testing sample and standard items, result is as shown in table 5.
As shown in Table 5, shown by the result of implementation of embodiment 3～4：When Sample equilibration temperature is 60 DEG C and 100 DEG C,
Its similarity result is consistent with embodiment 1, is all 1 C and 1#Standard items have maximum similarity, 1 D and 1#Standard condition
Seemingly spend minimum；The result of embodiment 5 is inconsistent with embodiment 1,1 H and 1#Standard items similarity highest.The reality of embodiment 3～5
Apply and show, rationally low temperature need to be selected as far as possible, otherwise sample can cause property to change at an excessive temperature, and disturbed test is tied
The correctness of fruit.
The different impact to sample similarity measurement result for the Sample equilibration temperature of table 5
Embodiment 68：
Implemented according to embodiment 1, and adjusted accordingly in the following areas：
In order to investigate the impact to testing result for the different Sample equilibration time, embodiment 6 adopts Sample equilibration time
10min, embodiment 7 adopts Sample equilibration time 20min, and embodiment 8 adopts Sample equilibration time 30min, in not homostasis
Between under, compare the similarity of testing sample and standard items.
Result shows, HS IMR MS method is to 1#When sample carries out quality conformance analysis, Sample equilibration time is to enforcement
Result impact less, is all 1 C and 1#Standard items similarity highest, 1 D and 1#Standard items similarity is minimum.Ask in view of time-consuming
Topic, therefore when selecting Sample equilibration time, suitable low Sample equilibration time should be selected as far as possible.
Embodiment 9 10：
For investigating the applicability to other essence spice for cigarette sample analysis for the present invention, embodiment 9～10 is according to embodiment 1
Implemented, and adjusted accordingly in the following areas：
In embodiment 9, choose 2 respectively#2 A～2 F cigarettes of the standard items of flavouring essence for tobacco and 6 different manufacturers productions are used
Essence is tested, in IMR MS parameter setting, in scanning ion inventory in add mass number be 16 150 each scan from
Son, remaining is implemented according to embodiment 1.2#Standard items mass spectrum fingerprint pattern is as shown in figure 3, similarity experimental result such as table 6
Shown.
In embodiment 10, choose 3 respectively#The standard items of flavouring essence for tobacco and 3 A～3 I cigarettes of 9 different manufacturers productions
Tested with essence, in IMR MS parameter setting, added each scanning that mass number is 16 150 in scanning ion inventory
Ion, remaining is implemented according to embodiment 1.3#Standard items mass spectrum fingerprint pattern is as shown in figure 4, similarity experimental result such as table
Shown in 7.
As shown in Table 6,2 F and 2#Standard items have highest similarity, are 0.991.Tested with infrared spectrum detection method
Card, result is consistent with embodiment 9,2 F and 2#Standard items have highest similarity matching value, are 0.991.
As shown in Table 7,3 E and 3#Standard items have highest similarity, are 0.995.Tested with infrared spectrum detection method
Card, result is consistent with embodiment 10,3 E and 3#Standard items have highest similarity matching value, are 0.992.
Table 62#Essence spice for cigarette standard items and testing sample similarity (ionization reagents：Hg)
Table 73#Essence spice for cigarette standard items and testing sample similarity (ionization reagents：Hg)
Claims (7)
1. a kind of using the conforming method of HS IMR MS Fast Evaluation volatility quality of flavoring essence for tobacco it is characterised in that：
Using the response of head-space sampler and each volatile compound ion in IMR MS acquisition essence and flavoring agent, draw mass spectrum fingerprint image
Spectrum, to realize the conforming Fast Evaluation of quality of flavoring essence for tobacco in conjunction with similarity analysis.
2. according to claim 1 a kind of consistent using HS IMR MS Fast Evaluation volatility quality of flavoring essence for tobacco
The method of property it is characterised in that：Comprise the following steps：
S1, the preparation of testing sample；
Accurate weighing essence spice for cigarette standard items and each 0.50g of detected sample are placed in the 20mL ml headspace bottle of sealing, by sky
The standard items compare in vain, weighing and each testing sample are positioned on head-space sampler sample injection disc in order, and in each two sample
Insert blank ml headspace bottle between product, for being spaced suction, remove pipeline residual；
S2, HS IMR MS instrumental conditions are arranged, including following sub-step：
S21, headspace autosampler analysis condition are as follows：
Sample equilibration temperature：50 DEG C 150 DEG C, quantitative loop temperature：50 DEG C 150 DEG C, transmission line temperature：50℃‐150℃；
Quantitative loop volume：1mL；Sample equilibration time：2min‐30min；Pressing time：0.2min；Loop fills the time：
0.2min；The loop balance time：0.05min；Sample injection time：1min；
S22, IMR MS analysis condition is as follows：
Open IMR MS system and preheat more than 48 hours, Single Masses method is set in IMR MS work station, and
Carry out following parameter setting in the method：
Add each scanning ion that mass number is 16 500 in scanning ion inventory, each ion is set：Sweep time：
50ms 500ms, MS acquisition pressure：25mbar；
Ionization reagents：Hg, reagent ionization energy：10.44eV；Or ionization reagents：Xe, reagent ionization energy：12.13eV；Or ionization examination
Agent：Kr, reagent ionization energy：14.00eV；
Resolution ratio：1amu, cycles samples scanning times：5 times；
S3, mass spectrum fingerprint pattern obtain；
Calculate the mean value of each five scanning results of ion in standard items and testing sample, and deduct corresponding ion in blank
Mean value, obtains final product the response of each ion in standard items and testing sample；Mapped with the response of each ion and respective quality number,
Obtain the mass spectrum fingerprint pattern of standard items and testing sample；
S4, similarity analysis；
Each mass number in standard items and testing sample mass spectrum fingerprint pattern and response are imported SPSS statistical analysis software,
Using Bivariate analysis, calculate the phase of standard items and each testing sample mass spectrum fingerprint pattern using Pearson correlation coefficient method
Like degree.
3. according to claim 2 a kind of consistent using HS IMR MS Fast Evaluation volatility quality of flavoring essence for tobacco
The method of property it is characterised in that：In described step S21, Sample equilibration temperature is：80 DEG C, quantitative loop temperature is：100 DEG C, pass
Defeated line temperature is：120℃.
4. according to claim 2 a kind of consistent using HS IMR MS Fast Evaluation volatility quality of flavoring essence for tobacco
The method of property it is characterised in that：In described step S21, Sample equilibration time is：5min.
5. according to claim 2 a kind of consistent using HS IMR MS Fast Evaluation volatility quality of flavoring essence for tobacco
The method of property it is characterised in that：In described step S22, sweep time：300ms.
6. according to claim 2 a kind of consistent using HS IMR MS Fast Evaluation volatility quality of flavoring essence for tobacco
The method of property it is characterised in that：Add each scanning ion that mass number is 16 300 in scanning ion inventory.
7. according to claim 1 a kind of consistent using HS-IMR-MS Fast Evaluation volatility quality of flavoring essence for tobacco
The method of property it is characterised in that：Its evaluation object includes spices, perfume base and the essence of cigarette use and non-cigarette, and its formulation includes
Liquid, tincture, medicinal extract and pressed powder.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110161011A (en) * | 2019-06-12 | 2019-08-23 | 浙江中烟工业有限责任公司 | Rapid detection method of the Semblance to the essence spice for cigarette of the amounts of mixing different in production |
| CN111610290A (en) * | 2020-04-16 | 2020-09-01 | 云南中烟工业有限责任公司 | Method for quantitatively evaluating similarity of essence and flavor |
| CN112345654A (en) * | 2019-08-06 | 2021-02-09 | 红塔烟草(集团)有限责任公司 | Method for identifying oil stain smoke pollution source based on chromatographic fingerprint spectrum |
| CN113030007A (en) * | 2021-02-10 | 2021-06-25 | 河南中烟工业有限责任公司 | Method for rapidly testing quality stability of tobacco essence based on similarity learning algorithm |
| CN114264766A (en) * | 2021-12-31 | 2022-04-01 | 江苏艾兰得营养品有限公司 | Evaluation method of sweet orange essence for VC soft sweets |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101701949A (en) * | 2009-11-05 | 2010-05-05 | 中国烟草总公司郑州烟草研究院 | Measurement method of volatile organic compound in tobacco lining paper |
| CN105158385A (en) * | 2015-07-10 | 2015-12-16 | 云南中烟工业有限责任公司 | Method for accurately characterizing and evaluating flue-cured tobacco smoke aroma characteristic in cigarette aroma |
| CN105675785A (en) * | 2016-01-27 | 2016-06-15 | 云南中烟工业有限责任公司 | Method for fast gas chromatography identification of quality of tobacco flavors for invitation for bids |
-
2016
- 2016-11-22 CN CN201611026536.6A patent/CN106404884A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101701949A (en) * | 2009-11-05 | 2010-05-05 | 中国烟草总公司郑州烟草研究院 | Measurement method of volatile organic compound in tobacco lining paper |
| CN105158385A (en) * | 2015-07-10 | 2015-12-16 | 云南中烟工业有限责任公司 | Method for accurately characterizing and evaluating flue-cured tobacco smoke aroma characteristic in cigarette aroma |
| CN105675785A (en) * | 2016-01-27 | 2016-06-15 | 云南中烟工业有限责任公司 | Method for fast gas chromatography identification of quality of tobacco flavors for invitation for bids |
Non-Patent Citations (3)
| Title |
|---|
| WENQIAN HOU等: "Development of the mass spectral fingerprint by headspace- solid-phase microextraction-mass spectrometry and chemometric methods for rapid quality control of flavoring essence", 《MICROCHEMICAL JOURNAL》 * |
| 聂磊等: "顶空-气相色谱-质谱技术应用于卷烟真伪鉴别", 《中国烟草学报》 * |
| 陈敏等: "离子分子反应质谱(IMR-MS)在线逐口检测卷烟主流烟气中重要气相成分 ", 《中国烟草学报》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110161011A (en) * | 2019-06-12 | 2019-08-23 | 浙江中烟工业有限责任公司 | Rapid detection method of the Semblance to the essence spice for cigarette of the amounts of mixing different in production |
| CN112345654A (en) * | 2019-08-06 | 2021-02-09 | 红塔烟草(集团)有限责任公司 | Method for identifying oil stain smoke pollution source based on chromatographic fingerprint spectrum |
| CN111610290A (en) * | 2020-04-16 | 2020-09-01 | 云南中烟工业有限责任公司 | Method for quantitatively evaluating similarity of essence and flavor |
| CN113030007A (en) * | 2021-02-10 | 2021-06-25 | 河南中烟工业有限责任公司 | Method for rapidly testing quality stability of tobacco essence based on similarity learning algorithm |
| CN114264766A (en) * | 2021-12-31 | 2022-04-01 | 江苏艾兰得营养品有限公司 | Evaluation method of sweet orange essence for VC soft sweets |
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