CN106908550A - A kind of method of Usneaceae plant characteristics composition in detection tobacco sample - Google Patents
A kind of method of Usneaceae plant characteristics composition in detection tobacco sample Download PDFInfo
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Abstract
The present invention relates to a kind of method for detecting Usneaceae plant characteristics composition in tobacco sample, the method is comprised the following steps：A) with the extractant extracted tobacco sample of containing the internal standard thing, sample solution is obtained；B) series concentration standard liquid is prepared with Usneaceae plant characteristics composition, internal standard compound and the extractant；C) the Usneaceae plant characteristics composition in the series concentration standard liquid is determined with GC-MS, draws standard working curve；D) content of the Usneaceae plant characteristics composition in the sample solution is determined with GC-MS, it is quantitative using Internal standard curve method；E) content of Usneaceae plant characteristics composition in tobacco sample is calculated.The method is reproducible, and analysis detection sensitivity is high.
Description
Technical field
The invention belongs to Field of Tobacco, and in particular to the side of Usneaceae plant characteristics composition in a kind of detection tobacco sample
Method.
Background technology
Usneaceae plant extracts has unique natural delicate fragrance and strong resin breath, and lasting is more lasting, is weight
The natural perfume material wanted.After Usneaceae plant extracts is applied to perfuming cigarette, old cigarette local flavor can be promoted, the miscellaneous gas of tobacco can be covered
With soil breath, the cigarette style of uniqueness is set off, assign the green grass or young crops perfume aromatic style of cigarette tongue sample, hence it is evident that increase flue gas concentration, and
And the comfort of oral cavity and throat can be improved, very important effect is also played in the allotment of flavouring essence for tobacco.
The processing technology of Usneaceae plant extracts is different, and product exists with medicinal extract or absolute oil form, wherein also having a large amount of
The impurity such as pigment, vegetable wax, cause its aroma quality and purity not good enough, bring adverse effect to cigarette pleasant impression.Medicinal extract quality
Change with changes such as soil constituent, weather conditions, the season of growth, generation age, harvesting time, accumulating situations with composition, i.e.,
Make the tree moss raw material of areal, the slight change of the technique such as fermentation, processing can also cause the fluctuation of wherein characteristic component content.
The characteristic component of Usneaceae plant in tobacco sample is determined, the content fluctuation of composition is directly objectively judged, cigarette composition is set
The aspects such as meter, product maintenance and quality control instruct reference.
The content of the invention
Inventor has found, using Usneaceae plant characteristics composition in GC-MS (GC-MS) detection tobacco sample,
If the method for only relying on total ion current abundance, it is difficult to realize the tracking to its characteristic component, reason is：
1. applied amount of the Usneaceae plant extracts in tobacco is no more than 0.005%, and feature aroma component therein is only
Account for therein 1/10；
2., containing substantial amounts of acid, alkali, sugar, albumen, starch, pectin, wax etc. in pipe tobacco, complicated matrix severe jamming is special
Levy the discriminating of composition；
3. after pipe tobacco pyrolysis and combustion, the active ingredient for migrating into oral cavity with flue gas is more rare.
Therefore, in addition to sensory evaluation, in order to more effectively recognize form of this feature spices in tobacco sample, it is necessary to
The method for preferably detecting Usneaceae plant characteristics composition in tobacco sample.
First aspect present invention provides a kind of detection method of Usneaceae plant characteristics composition in tobacco sample, including following
Step：
A) with the extractant extracted tobacco sample of containing the internal standard thing, sample solution is obtained；
B) series concentration standard liquid is prepared with Usneaceae plant characteristics composition, internal standard compound and the extractant；
C) with the Usneaceae plant characteristics composition in series concentration standard liquid described in Gas Chromatography-Mass Spectrometry, paint
Standard working curve processed；
D) with the content of the Usneaceae plant characteristics composition in sample solution described in Gas Chromatography-Mass Spectrometry, use
Internal standard curve method is quantified；
E) content of Usneaceae plant characteristics composition in tobacco sample is calculated；
The internal standard compound is phenethyl acetate；
The extractant is dichloromethane；
The gas chromatography-mass spectrography parameter includes：Using selective ion, chromatographic column is phenyl arylene polymers
(being equal to 5%- phenyl in performance)-methyl polysiloxane capillary chromatographic column；
The Usneaceae plant characteristics composition is selected from：Orcin, orcin monomethyl ether, orcin carboxylic acid, ethyl ester and β-Tai Hei
One or more in phenol carboxylate methyl ester.
The Usneaceae plant characteristics composition can include orcin.
The Usneaceae plant characteristics composition can include orcin monomethyl ether.
The Usneaceae plant characteristics composition can include orcin carboxylic acid, ethyl ester.
The Usneaceae plant characteristics composition can include β-orcin carboxylate methyl ester.
In one embodiment, the method described in any one of the present invention, the chromatographic parameter of the gas chromatography-mass spectrography
Including following one or more：
- chromatogram column type number：J&W DB-5ms；
- column size：30m×0.25mm×0.25μm；
- injector temperature：240~260 DEG C (such as 250 DEG C)；
- sample size：0.5~1.5 μ L (such as 1 μ L)；
- split ratio：8~12:1 (such as 10:1)；
- flow rate of carrier gas：1~2mL/min (such as 1.5mL/min)；
- purging gas velocity：4~6mL/min (such as 5mL/min)；
- temperature programming is used, heating schedule is：
Initial 50~70 DEG C (such as 60 DEG C), keep 1~3min (such as 2min),
It is warming up to 230~250 DEG C (such as 240 DEG C) with 3~5 DEG C/min (such as 4 DEG C/min) speed, holding 0.5~
1.5min (such as 1min),
It is warming up to 250~270 DEG C (such as 260 DEG C) with 15~25 DEG C/min (such as 20 DEG C/min) speed, holding 4~
6min (such as 5min).
In one embodiment, the method described in any one of the present invention, the mass spectrometry parameters of the gas chromatography-mass spectrography
Including following one or more：
- ion gun：Electron bombardment ionization source；
- electronic energy：60~80eV；
- transmission line temperature：200~300 DEG C (such as 250 DEG C)；
- ion source temperature：200~300 DEG C (such as 250 DEG C)；
100~200 DEG C of-level Four bar temperature (such as 150 DEG C)；
- solvent delay：6~10min (such as 8min)；
- scanned simultaneously using SCAN and SIM, mass scan range m/z 45~300；
In one embodiment, the method described in any one of the present invention, the mass spectrometry parameters of the gas chromatography-mass spectrography
Including following one or more：
The qualitative ion of-phenethyl acetate is the ion of m/z43,91 and 104, and quota ion is the ion of m/z104；
The qualitative ion of-orcin monomethyl ether is the ion of m/z76,107 and 138, and quota ion is the ion of m/z138；
The qualitative ion of-orcin is the ion of m/z67,95 and 124, and quota ion is the ion of m/z124；
The qualitative ion of-β-orcin carboxylate methyl ester is the ion of m/z136,164 and 196, and quota ion is m/z136's
Ion；
The qualitative ion of-orcin carboxylic acid, ethyl ester is the ion of m/z122,150 and 196, quota ion for m/z150 from
Son.
In one embodiment, the method described in any one of the present invention, step a) includes：
- by the extractant ultrasonic extraction of tobacco sample containing the internal standard, filtrate is collected in filtering；
- add saturated nacl aqueous solution and hydrochloric acid, vibration, centrifugation point liquid to collect organic phase in filtrate；
- by organic phase anhydrous sodium sulfate drying, PTFE membrane filtrations are used, obtain sample solution.
In one embodiment, the method described in any one of the present invention, the tobacco sample is cigarette mainstream flue gas
TPM, step a) includes：
- with cambridge filter collect cigarette mainstream flue gas TPM；
- by the extractant ultrasonic extraction of the cambridge filter containing the internal standard containing TPM, filtrate is collected in filtering；
- add saturated nacl aqueous solution and hydrochloric acid, vibration, centrifugation point liquid to collect organic phase in filtrate.
In one embodiment, the method described in any one of the present invention, the tobacco sample is pipe tobacco, step a) bags
Include：
- by the extractant ultrasonic extraction of pipe tobacco containing the internal standard, filtrate is collected in filtering；
- add saturated nacl aqueous solution and hydrochloric acid, vibration, centrifugation point liquid to collect organic phase in filtrate.
In one embodiment, the method described in any one of the present invention, in step b), the series concentration standard liquid
It is matrix matching series concentration standard liquid；
Preferably, the preparation method of the matrix matching series concentration standard liquid is comprised the following steps：
- solvent extraction tobacco sample is used, obtain the matrix solution of tobacco sample；
- the Usneaceae for preparing various concentrations with Usneaceae plant characteristics composition, the internal standard compound and the extractant is planted
The solution of thing characteristic component；
- be blown to matrix solution nitrogen closely to do, then the solution of the Usneaceae plant characteristics composition of various concentrations is separately added into, obtain
To matrix matching series standard solution.
In one embodiment, the method described in any one of the present invention, the concentration model of the series concentration standard liquid
It is 0.01 μ g/mL~2.0 μ g/mL to enclose.
In one embodiment, the method described in any one of the present invention, the concentration of hydrochloric acid scope is 2%~5%.
In one embodiment, the method described in any one of the present invention, its one or multi-step in comprising the following steps：
1. the preparation of standard liquid
The preparation of 1.1 inner mark solutions and standard liquid：The standard items of phenethyl acetate are weighed, solvent constant volume is added, is made into
Internal standard stock solution.It is accurate to weigh Usneaceae plant characteristics composition, solvent constant volume is added, it is made into Standard Stock solutions.Pipette and be
Row dimension criteria stock solution and appropriate internal standard stock solution, are configured to general series standard solution.
The preparation of 1.2 matrix matching standard liquids：The different tobacco products of correspondence, are extracted and pre-treatment using extractant,
Obtain the matrix solution of tobacco product.Proper amount of matrix solution is pipetted, nitrogen is blown to closely do, and adds the one of 1.1 isometric preparations
As standard liquid, obtain matrix matching series standard solution.
2. sample pre-treatments
The preparation of 2.1 extraction solution：Appropriate internal standard stock solution is added in extractant, internal standard extraction is obtained molten
Liquid.
The pre-treatment of 2.2 tobacco products：Tobacco product extracts solution and is aided with ultrasonic extraction using the internal standard of proper volume,
Filtrate uses saturated aqueous common salt and salt acid elution after filtering.Mixed solution is centrifuged layering after standing, and removes water phase, organic phase nothing
After aqueous sodium persulfate is dried, gaschromatographic mass spectrometry sample introduction.
3. the qualitative detection of sample：Gaschromatographic mass spectrometry total ion current figure determines the retention time of component to be measured, it is determined that treating
Survey the qualitative ion and quota ion of component.
4. the quantitative determination of sample
4.1 draw standard working curve：Matrix matching standard liquid in step 1.2 is carried out into gaschromatographic mass spectrometry selection
Ion measurement, with target component with interior target quota ion peak area ratio as ordinate, be horizontal with the mass concentration of target component
Coordinate, draws the standard working curve of the Usneaceae plant characteristics composition in correspondence tobacco product matrix, obtains linear regression side
Journey.
The measure of 4.2 samples：Solution to be measured in step 2.2 is carried out into gaschromatographic mass spectrometry selection ion measurement, will be obtained
Target component/interior target quota ion peak area ratio substitutes into the equation of linear regression in 4.1 in the solution to be measured for obtaining, and is calculated
The mass concentration of target component, and then conversion obtains the content in tobacco product.
In one embodiment, the method described in any one of the present invention, the tobacco sample is selected from tobacco leaf, pipe tobacco, again
Make one or more in tobacco leaf, electronic cigarette liquid, cigarette paper, internal lining paper, filter stick, cigarette packing box.
In one embodiment, the method for the present invention includes：
1. the preparation of standard liquid
The preparation of 1.1 inner mark solutions and standard liquid：The standard items of phenethyl acetate are weighed, extractant constant volume is added,
It is made into internal standard stock solution.Usneaceae plant characteristics composition is weighed, extractant constant volume is added, Standard Stock solutions are made into.Move
Serial dimension criteria stock solution and appropriate internal standard stock solution are taken, general series standard solution is configured to.
The preparation of 1.2 matrix matching standard liquids：It is right without Usneaceae plant characteristics composition to be extracted using extractant
According to tobacco sample, the matrix solution of tobacco sample is obtained.Proper amount of matrix solution is pipetted, nitrogen is blown to closely do, adds isometric
The 1.1 general series standard solution prepared, obtain matrix matching series standard solution.
2. sample pre-treatments
The preparation of 2.1 extraction solution：Appropriate internal standard stock solution is added in extractant, internal standard extraction is obtained molten
Liquid.
The pre-treatment of 2.2 tobacco samples：Tobacco sample extracts solution and is aided with ultrasonic extraction using the internal standard of proper volume,
Filtrate uses saturated aqueous common salt and salt acid elution after filtering.Mixed solution is centrifuged layering after standing, and removes water phase, organic phase nothing
After aqueous sodium persulfate is dried, gaschromatographic mass spectrometry sample introduction.
3. the qualitative detection of sample：Gaschromatographic mass spectrometry total ion current figure determines the retention time of component to be measured, it is determined that treating
Survey the qualitative ion and quota ion of component.
4. the quantitative determination of sample
4.1 draw standard working curve：Matrix matching standard liquid in step 1.2 is carried out into gaschromatographic mass spectrometry selection
Ion measurement, with target component with interior target quota ion peak area ratio as ordinate, be horizontal with the mass concentration of target component
Coordinate, draws the standard working curve of the Usneaceae plant characteristics composition in correspondence tobacco sample matrix, obtains linear regression side
Journey.
The measure of 4.2 samples：Solution to be measured in step 2.2 is carried out into gaschromatographic mass spectrometry selection ion measurement, will be obtained
Target component/interior target quota ion peak area ratio substitutes into the equation of linear regression in 4.1 in the solution to be measured for obtaining, and is calculated
The mass concentration of target component, and then conversion obtains the content in tobacco sample.
Beneficial effects of the present invention
One or more methods of open embodiment have following one or more advantage：
1. extractant direct extraction method is used, while classics compared with Water distillation extractor, it is to avoid high-temperature heating institute
The forfeiture of the ingredient degradation and micro constitutent that cause, also shortens the time of pre-treatment；
2. gaschromatographic mass spectrometry selective ion is used, the interference of tobacco sample complex matrices is significantly reduced, improve
The sensitivity of detection；
3., in order to further reduce influence of the matrix effect to quantitative result, corresponding work is drawn for different substrates bent
Line, it is ensured that the comparativity of data between different tobacco samples；
4. by optimizing gaschromatographic mass spectrometry parameter so that the detection limit and quantitative limit of detection method are relatively low, mark-on reclaims
Rate is relatively low close to 100%, relative standard deviation (RSD).
Brief description of the drawings
Fig. 1 concentration is the TIC and selection chromatography of ions figure of the general standard solution of 0.1 μ g/mL；
Fig. 2 concentration is the TIC and selection chromatography of ions figure of the matrix matching standard liquid of 1.0 μ g/mL；
In Fig. 1,2, each curve implication is as follows：The total ionic chromatographic of 0- Usneaceae plant characteristics compositions；1- orcin lists
The selection chromatography of ions of methyl ether, the selection chromatography of ions of 2- orcins, the selection chromatography of ions of 3- β-orcin carboxylate methyl ester, 4-
The selection chromatography of ions of orcin carboxylic acid, ethyl ester.
Specific embodiment
To in detail refer to specific embodiments of the present invention now.The example of specific embodiment is illustrated in the drawings.To the greatest extent
Pipe combines these specific embodiments and describes the present invention, it is appreciated that being not intended to limit the invention to these specific embodiment parties
Case.Conversely, these embodiments be intended to cover may include in the spirit and scope being defined by the claims replacement, change
Become or equivalent embodiments.In the following description, elaborate a large amount of details to provide complete understanding of the present invention.
The present invention can be carried out in the case of without part or all of these details.In other cases, in order to send out this
It is bright unnecessarily to obscure, it is not described in well known technological operation.
In following examples, the reagent of the method for Usneaceae plant characteristics composition is as follows with instrument in detection tobacco sample：
Reagent：Cigarette sample (Fujian China Tobacco Industrial Co., Ltd. technique center provides)；Orcin (>98%,
Arcos), orcin monomethyl ether, orcin carboxylic acid, ethyl ester (>98%, TCI), β-orcin carboxylate methyl ester (>98%, Sigma-
Aldrich), phenethyl acetate (standard items, JKChemical)；Dichloromethane (HPLC, JKChemicl), hydrochloric acid (37%,
JKChemical), pure water (self-control)；Sodium chloride, anhydrous sodium sulfate (A.R., traditional Chinese medicines).
Instrument：TRACE1310 gas-chromatography+ISQ LT quadrupole rods mass spectrum (Thermo companies of the U.S.)；RM-20H rotating disks are inhaled
Cigarette machine (German Borgwaldt companies)；S150 ultrasonic extractions instrument (German Elma companies)；2-16P centrifuges (German SIGMA
Company)；Turbo Vap II Nitrogen evaporators (Biotage companies of Sweden)；(Metler Toledo are public for Switzerland for ML204 electronic balances
Department, sensibility reciprocal 0.1mg).
In following examples, the use gaschromatographic mass spectrometry of the method for Usneaceae plant characteristics composition in detection tobacco sample
Method.
In following examples, the chromatographic condition of gaschromatographic mass spectrometry is as follows：
Chromatographic column：J&W DB-5ms(30m×0.25mm×0.25μm)；Injector temperature：250℃；Sample size：1.0μL；
Split ratio：10:1；Flow rate of carrier gas：1.5mL/min；Purging gas velocity：5mL/min；Heating schedule：60 DEG C, holding min → with 4
DEG C/→ 240 DEG C of min intensifications, holding 1min → heated up → 260 DEG C with 20 DEG C/min, holding 5min.
In following examples, the Mass Spectrometry Conditions of gaschromatographic mass spectrometry are as follows：
Ion gun：EI；Electronic energy：70eV；Transmission line temperature：250℃；Ion source temperature：250℃；Level Four bar temperature 150
℃；Solvent delay：8min；Scanned simultaneously using SCAN and SIM, mass scan range m/z 45~300；In following examples,
In detection tobacco sample in the method for Usneaceae plant characteristics composition, the compound method of general series standard solution is as follows：
The sterling for weighing orcin, orcin monomethyl ether, orcin carboxylic acid, ethyl ester and β-orcin carboxylate methyl ester respectively is each
50mg, adds the dissolving of extractant dichloromethane, and is settled to 50mL, is configured to the Standard Stock solutions of the μ g/mL of concentration 1000.
The standard items 32mg of phenethyl acetate is weighed, the dissolving of extractant dichloromethane is added, and is settled to 50mL, prepared
Into the internal standard stock solution of the μ g/mL of concentration 640.
The interior of 1.0 μ L, 2.5 μ L, 5.0 μ L, 10 μ L, 25 μ L, the Standard Stock solutions of 50 μ L and 25 μ L is accurately pipetted respectively
Mark stock solution, into the volumetric flask of 50mL, dichloromethane constant volume is stand-by.General series standard solution is obtained, concentration is respectively：
0.02μg/mL(S1)、0.05μg/mL(S2)、0.1μg/mL(S3)、0.2μg/mL(S4)、0.5μg/mL(S5)、1.0μg/mL
(S6), internal standard concentration is 0.32 μ g/mL.
The internal standard stock solution of 1.0mL accurately is pipetted in 2000mL dichloromethane, is configured to containing the internal standard concentration for 0.32 μ
The internal standard extractant of g/mL.
Fig. 1 is the TIC and selection chromatography of ions figure of the general standard solution that concentration is 0.1 μ g/mL.Fig. 1
In, each curve implication is as follows：The total ionic chromatographic of 0- Usneaceae plant characteristics compositions；The selection ion of 1- orcin monomethyl ethers
Chromatogram, the selection chromatography of ions of 2- orcins, the selection chromatography of ions of 3- β-orcin carboxylate methyl ester, 4- orcin carboxylic acid, ethyl esters
Selection chromatography of ions.
The retention time of component to be measured is determined according to gaschromatographic mass spectrometry total ion current figure, determine component to be measured it is qualitative from
Son and quota ion.
Selection ion scan parameter is as shown in table 1：
Table 1
The detection of the cigarette rags of embodiment 1.
1. the preparation of pipe tobacco matrix matching series standard solution
The preparation of 1.1 pipe tobacco matrix solutions：2 control cigarette shreds without Usneaceae plant characteristics composition are divested, is used
The extraction solution extraction of 20mL internal standards, ultrasonic 20min, filtering.10mL saturated aqueous common salts and the hydrochloric acid of 0.5mL 5% are added in filtrate,
Concussion 10min, 6000rpm centrifugation 10min is sufficiently separated two-phase, removes water phase.Organic phase is used after anhydrous sodium sulfate drying
(0.45 μm) filtering of PTFE filter membranes, subsequent filtrate is stand-by.
The preparation of 1.2 matrix matching standard liquids：In pipetting 2.0mL pipe tobaccos matrix solution to six nitrogen bottle blowings respectively,
The lower purging of nitrogen protection is closely dry to solution.Again toward general series standard solution is separately added into nitrogen bottle blowing, that is, obtain pipe tobacco matrix
Matching series standard solution, concentration is respectively 0.02 μ g/mL (S1l), 0.05 μ g/mL (S2l), 0.1 μ g/mL (S3l), 0.2 μ g/
ML (S4l), 0.5 μ g/mL (S5l), 1.0 μ g/mL (S6l), internal standard concentration are 0.32 μ g/mL.
2. sample pre-treatments
Two pipe tobaccos of sample cigarette are weighed, 20mL internal standards extraction solution, ultrasonic extraction 20min, filtering is added.In filtrate
10mL saturated sodium-chlorides are added, and the hydrochloric acid of 0.5mL 5% is added dropwise, vibrate 10min, 6000rpm centrifugations point liquid 10min.Remove water
Phase.Organic phase anhydrous sodium sulfate drying, with (0.45 μm) filtering of PTFE filter membranes.Chromatography column feed materials.
3. the measure of sample size
3.1 working curves, detection limit and test limit
The pipe tobacco matrix matching series standard solution for taking above-mentioned preparation carries out gaschromatographic mass spectrometry detection, with object with it is interior
The quota ion peak area ratio for marking thing is ordinate, and the mass concentration with object carries out regression analysis, obtains cigarette as abscissa
The standard working curve and its coefficient correlation of four kinds of objects in silk, concrete outcome is as shown in table 1.1.
From table 1.1, to the object response signal in matrix matching standard liquid, repeated using least concentration standard specimen
10 sample introductions, take 3 times of signal to noise ratios as the detection limit (LOD) of method, and 10 times of signal to noise ratios are quantitative limit (LOQ), it is known that method has
Sensitivity higher.
Fig. 2 concentration is the TIC and selection chromatography of ions figure of the matrix matching standard liquid of 1.0 μ g/mL.
In Fig. 2, each curve implication is as follows：The total ionic chromatographic of 0- Usneaceae plant characteristics compositions；The selection of 1- orcin monomethyl ethers
Chromatography of ions, the selection chromatography of ions of 2- orcins, the selection chromatography of ions of 3- β-orcin carboxylate methyl ester, 4- orcin carboxylic acids
The selection chromatography of ions of ethyl ester.
The working curve of table 1.1, detection limit and test limit
3.2 rate of recovery and precision
Control cigarette shreds sample is taken, 3 object sterling solution of various concentrations is added, and add internal standard to extract solution
The sample pre-treatments of the above are carried out, gaschromatographic mass spectrometric analysis is carried out, according to mark-on amount (0.1 μ g/mL, 0.2 μ g/mL and 0.5 μ
) and measured value calculates its rate of recovery g/mL.Simultaneously to same sample solution parallel determination 5 times (n=5), four kinds of compositions are obtained
Precision determination data, is shown in Table 1.2.By table 1.2 as can be seen that four kinds of rate of recovery of composition are between 70.4%~114.5%,
Relative standard deviation (RSD) is respectively less than 11.7%, illustrates that the rate of recovery of this method is high, accuracy and reproducible, can meet
It is quantitative to need.
The rate of recovery of table 1.2 and precision
Content in 3.3 pipe tobaccos
With method of testing established above, four cigarette rags of the trade mark are tested respectively, such as table 1.3, four
Orcin monomethyl ether is not detected in the individual trade mark, the content of orcin is close, and the β-orcin carboxylate methyl ester in the pipe tobacco of the trade mark 4
With the orcin equal highest of carboxylic acid, ethyl ester content.
The test result of Usneaceae plant characteristics component content in the pipe tobacco of table 1.3
Comparative example 1
Micro Usneaceae plant extracts is added in cigarette shreds, with reference to the method for embodiment 1, dichloromethane is used respectively
Alkane, three kinds of conventional organic solvents of ethyl acetate and n-hexane are extracted to pipe tobacco, using phenethyl acetate as internal standard, use gas phase
Chromatogram relative peak area investigates extraction efficiency of three kinds of solvents to Usneaceae plant component.As shown in table 1.4, for orcin,
The extraction efficiency of dichloromethane is significantly better than ethyl acetate and n-hexane；For other three kinds of compositions, dichloromethane and acetic acid second
The extraction efficiency of ester is approached, and is superior to n-hexane.Based on the above results, for Usneaceae plant component, dichloromethane is more
Suitable extractant.With reference to the recovery of standard addition result of table 1.2, the testing result of embodiment 1 closer to actual value is also illustrated.
1.4 3 kinds of solvents of table compare the extraction efficiency of composition
The detection of the cigarette mainstream flue gas of embodiment 2.
1. the preparation of flue gas matrix matching standard liquid
The preparation of 1.1 flue gas matrix solutions：According to GB/T 5606.1-2004 national standards and ISO 3308:2012 tobaccos
Professional standard specifies, 20 pure tobacco shred cigarettes is aspirated that using carousel-type smoking machine cambridge filter traps TPM.Filter
Piece 40mL internal standards extract solution and extract, ultrasonic 15min.Remove filter disc, toward extractant add 10mL saturated aqueous common salts with
The hydrochloric acid of 0.5mL 5%, shakes 10min, and 6000rpm centrifugations 10min is sufficiently separated two-phase, removes water phase.Organic phase is through anhydrous
After sodium sulphate is dried, PTFE membrane filtrations are used, subsequent filtrate is stand-by.
The preparation of 1.2 matrix matching standard liquids：In pipetting 2.0mL flue gases matrix solution to six nitrogen bottle blowings respectively,
The lower purging of nitrogen protection is closely dry to solution.Again toward general series standard solution is added in nitrogen bottle blowing, that is, obtain flue gas matrix matching
Standard liquid.Gained calibration curve solution concentration is respectively 0.02 μ g/mL (S1f), 0.05 μ g/mL (S2f), 0.1 μ g/mL
(S3f), 0.2 μ g/mL (S4f), 0.5 μ g/mL (S5f), 1.0 μ g/mL (S6f), internal standard concentration are 0.32 μ g/mL.
2. sample pre-treatments
20 TPMs of cigarette are collected with carousel-type smoking machine, cambridge filter adds 40mL internal standards extraction solution, surpasses
Sound extracts 15min.20mL extractants are pipetted, 10mL saturated sodium-chlorides are added, the hydrochloric acid of 0.5mL 5% is added, vibrated
10min, centrifugation point liquid (6000rpm, 10min).Remove water phase, oil phase anhydrous sodium sulfate drying, filter membrane (PTFE, 0.45 μ
m).Chromatography column feed materials.
3. the measure of sample size
3.1 working curves, detection limit and test limit
The flue gas matrix matching standard liquid for taking above-mentioned preparation carries out gaschromatographic mass spectrometry detection, with object and internal standard compound
Quota ion peak area ratio be ordinate, the mass concentration with object carries out regression analysis as abscissa, in obtaining flue gas
The standard working curve and its coefficient correlation of four kinds of objects, concrete outcome is as shown in table 2.1.
From table 2.1, to the object response signal in standard liquid, using least concentration standard specimen be repeated 10 times into
Sample, take 3 times of signal to noise ratios as the detection limit (LOD) of method, and 10 times of signal to noise ratios are quantitative limit (LOQ), it is known that method has higher
Sensitivity.
The working curve of table 2.1, detection limit and test limit
3.2 rate of recovery and precision
20 TPMs of cigarette are collected with carousel-type smoking machine, 3 object sterling solution of various concentrations are added,
And add internal standard to extract solution to carry out the sample pre-treatments of the above, gaschromatographic mass spectrometric analysis is carried out, according to mark-on amount (0.1 μ g/
ML, 0.2 μ g/mL and 0.5 μ g/mL) and measured value calculate its rate of recovery.Simultaneously to 5 (n=of same sample solution parallel determination
5) four kinds of precision determination datas of composition, are obtained, 2.2 are shown in Table.By table 2.2 as can be seen that the rate of recovery of four kinds of compositions exists
Between 71.5%~108.5%, relative standard deviation (RSD) is respectively less than 9.3%, illustrates that the rate of recovery of this method is high, accuracy
With it is reproducible, quantitative needs can be met.
The rate of recovery of table 2.2 and precision
Content in 3.3 flue gases
With method of testing established above, three finished cigarettes flue gases of the trade mark are tested respectively, such as table 2.3, three
Do not detect orcin monomethyl ether and orcin in the individual trade mark, and the β of the main flume of the trade mark 7-orcin carboxylate methyl ester and Tai Hei
Phenol carboxylic acid, ethyl ester content is minimum.
The test result of Usneaceae plant characteristics component content in the flue gas of table 2.3
Above-described embodiment determines four kinds of contents of Usneaceae plant characteristics composition using selection ion method, it is possible to achieve
The measure of Usneaceae plant characteristics composition in cigarette products, thus for cigarette flavoring essence allotment, apply and sensory evaluating smoking, there is provided it is accurate
True data reference.The present invention is directly extracted using solvent, and gaschromatographic mass spectrometry selective ion is analyzed, using matrix
It is quantitative with Internal standard curve method.With extraction efficiency it is high, easy to operate, exclude matrix interference, quantitative accurate etc. one or many
Item advantage.
Finally it should be noted that：The above embodiments are merely illustrative of the technical solutions of the present invention rather than its limitations；To the greatest extent
Pipe has been described in detail with reference to preferred embodiment to the present invention, and those of ordinary skill in the art should be understood：Still
Specific embodiment of the invention can be modified or equivalent is carried out to some technical characteristics；Without deviating from this hair
The spirit of bright technical scheme, it all should cover in the middle of claimed technical scheme scope of the invention.
Claims (12)
1. in a kind of tobacco sample Usneaceae plant characteristics composition detection method, comprise the following steps：
A) with the extractant extracted tobacco sample of containing the internal standard thing, sample solution is obtained；
B) series concentration standard liquid is prepared with Usneaceae plant characteristics composition, internal standard compound and the extractant；
C) with the Usneaceae plant characteristics composition in series concentration standard liquid described in Gas Chromatography-Mass Spectrometry, mark is drawn
Quasi- working curve；
D) with the content of the Usneaceae plant characteristics composition in sample solution described in Gas Chromatography-Mass Spectrometry, using internal standard
Standard curve standard measure；
E) content of Usneaceae plant characteristics composition in tobacco sample is calculated；
The internal standard compound is phenethyl acetate；
The extractant is dichloromethane；
The gas chromatography-mass spectrography parameter includes：Using selective ion, chromatographic column is phenyl arylene polymers (performance
On be equal to 5%- phenyl)-methyl polysiloxane capillary chromatographic column；
The Usneaceae plant characteristics composition is selected from：Orcin, orcin monomethyl ether, orcin carboxylic acid, ethyl ester and β-orcin carboxylic
One or more in sour methyl esters.
2. method according to claim 1, the chromatographic parameter of the gas chromatography-mass spectrography is included with the next item down or many
：
- chromatogram column type number：J&W DB-5ms；
- column size：30m×0.25mm×0.25μm；
- injector temperature：240~260 DEG C；
- sample size：0.5~1.5 μ L；
- split ratio：8~12:1；
- flow rate of carrier gas：1~2mL/min；
- purging gas velocity：4~6mL/min；
- temperature programming is used, heating schedule is：
Initial 50~70 DEG C, 1~3min is kept,
230~250 DEG C are warming up to 3~5 DEG C/min speed, 0.5~1.5min is kept,
250~270 DEG C are warming up to 15~25 DEG C/min speed, 4~6min is kept.
3. method according to claim 1, the mass spectrometry parameters of the gas chromatography-mass spectrography are included with the next item down or many
：
- ion gun：Electron bombardment ionization source；
- electronic energy：60~80eV；
- transmission line temperature：200~300 DEG C；
- ion source temperature：200~300 DEG C；
100~200 DEG C of-level Four bar temperature；
- solvent delay：6~10min；
- scanned simultaneously using SCAN and SIM, mass scan range m/z 45~300.
4. method according to claim 1, the mass spectrometry parameters of the gas chromatography-mass spectrography are included with the next item down or many
：
The qualitative ion of-phenethyl acetate is the ion of m/z43,91 and 104, and quota ion is the ion of m/z104；
The qualitative ion of-orcin monomethyl ether is the ion of m/z76,107 and 138, and quota ion is the example of m/z138；
The qualitative ion of-orcin is the ion of m/z67,95 and 124, and quota ion is the ion of m/z124；
The qualitative ion of-β-orcin carboxylate methyl ester is the ion of m/z136,164 and 196, quota ion for m/z136 from
Son；
The qualitative ion of-orcin carboxylic acid, ethyl ester is the ion of m/z122,150 and 196, and quota ion is the ion of m/z150.
5. method according to claim 1, step a) includes：
- by the extractant ultrasonic extraction of tobacco sample containing the internal standard, filtrate is collected in filtering；
- add saturated nacl aqueous solution and hydrochloric acid, vibration, centrifugation point liquid to collect organic phase in filtrate；
- by organic phase anhydrous sodium sulfate drying, PTFE membrane filtrations are used, obtain sample solution.
6. method according to claim 1, the tobacco sample is the TPM of cigarette mainstream flue gas, step a) bags
Include：
- with cambridge filter collect cigarette mainstream flue gas TPM；
- by the extractant ultrasonic extraction of the cambridge filter containing the internal standard containing TPM, filtrate is collected in filtering；
- add saturated nacl aqueous solution and hydrochloric acid, vibration, centrifugation point liquid to collect organic phase in filtrate.
7. method according to claim 1, the tobacco sample is pipe tobacco, and step a) includes：
- by the extractant ultrasonic extraction of pipe tobacco containing the internal standard, filtrate is collected in filtering；
- add saturated nacl aqueous solution and hydrochloric acid, vibration, centrifugation point liquid to collect organic phase in filtrate.
8. it is according to claim 1 it is a kind of detect tobacco sample in Usneaceae plant characteristics composition detection method, step
B) in, the series concentration standard liquid is matrix matching series concentration standard liquid；
Preferably, the preparation method of the matrix matching series concentration standard liquid is comprised the following steps：
- the control tobacco sample without Usneaceae plant characteristics composition is extracted using extractant, obtain the matrix of tobacco sample
Solution；
- Usneaceae the plant with Usneaceae plant characteristics composition, the internal standard compound and the extractant preparation various concentrations is special
Levy the solution of composition；
- be blown to matrix solution nitrogen closely to do, then the solution of the Usneaceae plant characteristics composition of various concentrations is separately added into, obtain base
Matter matches series standard solution.
9. method according to claim 1, the concentration range of the series concentration standard liquid is 0.01 μ g/mL~2.0 μ
g/mL。
10. the method according to any one of claim 6~8, the concentration of hydrochloric acid scope is 2wt%~5wt%.
11. method according to any one of claim 1~9, its one or multi-step in comprising the following steps：
1. the preparation of standard liquid
The preparation of 1.1 inner mark solutions and standard liquid：The standard items of phenethyl acetate are weighed, solvent constant volume is added, internal standard is made into
Stock solution, accurately weighs Usneaceae plant characteristics composition, adds solvent constant volume, is made into Standard Stock solutions, pipettes serial body
Product Standard Stock solutions and appropriate internal standard stock solution, are configured to general series standard solution；
The preparation of 1.2 matrix matching standard liquids：The control cigarette without Usneaceae plant characteristics composition is extracted using extractant
Careless sample, obtains the matrix solution of tobacco product, pipettes proper amount of matrix solution, and nitrogen is blown to closely do, adds isometric 1.1 and match somebody with somebody
The general series standard solution of system, obtains matrix matching series standard solution；
2. sample pre-treatments
The preparation of 2.1 extraction solution：Appropriate internal standard stock solution is added in extractant, internal standard extraction solution is obtained；
The pre-treatment of 2.2 tobacco products：Tobacco product extracts solution and is aided with ultrasonic extraction using the internal standard of proper volume, filters
Filtrate uses saturated aqueous common salt and salt acid elution, mixed solution that layering is centrifuged after standing afterwards, removes water phase, the anhydrous sulphur of organic phase
After sour sodium is dried, gaschromatographic mass spectrometry sample introduction；
3. the qualitative detection of sample：Gaschromatographic mass spectrometry total ion current figure determines the retention time of component to be measured, determines to be measured group
The qualitative ion and quota ion for dividing；
4. the quantitative determination of sample
4.1 draw standard working curve：Matrix matching standard liquid in step 1.2 is carried out into gaschromatographic mass spectrometry selection ion
Determine, with target component with interior target quota ion peak area ratio as ordinate, the mass concentration with target component as abscissa,
The standard working curve of the Usneaceae plant characteristics composition in correspondence tobacco product matrix is drawn, equation of linear regression is obtained；
The measure of 4.2 samples：Solution to be measured in step 2.2 is carried out into gaschromatographic mass spectrometry selection ion measurement, by what is obtained
Target component/interior target quota ion peak area ratio substitutes into the equation of linear regression in 4.1 in solution to be measured, is calculated target
The mass concentration of composition, and then conversion obtains the content in tobacco product.
12. method according to any one of claim 1~9, the tobacco sample is selected from tobacco leaf, pipe tobacco, reconstituted tobacco, electricity
One or more in sub- tobacco juice, cigarette mainstream flue gas, cigarette paper, internal lining paper, filter stick, cigarette packing box.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102041174A (en) * | 2011-01-07 | 2011-05-04 | 江苏中烟工业有限责任公司 | Preparation method of moss-scented tobacco flavor and application of moss-scented cigarette flavor in cigarette flavoring |
| CN104178522A (en) * | 2014-08-19 | 2014-12-03 | 云南中烟工业有限责任公司 | Evernia furfuracea fermented extract and preparation method and application thereof |
| CN104991007A (en) * | 2015-07-10 | 2015-10-21 | 云南中烟工业有限责任公司 | Method for exactly characterizing and evaluating sweet aroma characteristics in cigarette aroma |
| CN105738530A (en) * | 2016-04-29 | 2016-07-06 | 江苏中烟工业有限责任公司 | Method for optioning aroma component in natural moss perfume spice |
-
2017
- 2017-04-06 CN CN201710218861.0A patent/CN106908550B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102041174A (en) * | 2011-01-07 | 2011-05-04 | 江苏中烟工业有限责任公司 | Preparation method of moss-scented tobacco flavor and application of moss-scented cigarette flavor in cigarette flavoring |
| CN104178522A (en) * | 2014-08-19 | 2014-12-03 | 云南中烟工业有限责任公司 | Evernia furfuracea fermented extract and preparation method and application thereof |
| CN104991007A (en) * | 2015-07-10 | 2015-10-21 | 云南中烟工业有限责任公司 | Method for exactly characterizing and evaluating sweet aroma characteristics in cigarette aroma |
| CN105738530A (en) * | 2016-04-29 | 2016-07-06 | 江苏中烟工业有限责任公司 | Method for optioning aroma component in natural moss perfume spice |
Non-Patent Citations (2)
| Title |
|---|
| NATALIA YU. TRETYAKOVA ET AL.: "Degradative Pathways for Aqueous Chlorination of Orcinol", 《ENVIRON. SCI. TECHNOL.》 * |
| 于学龙 等: "长松萝中酚类化学成分研究", 《中国中药杂志》 * |
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