CN106093267B - A kind of method of infrared auxiliary hydration reaction on-line headspaces chromatography mass spectrometric determination tobacco water extract - Google Patents
A kind of method of infrared auxiliary hydration reaction on-line headspaces chromatography mass spectrometric determination tobacco water extract Download PDFInfo
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Abstract
The invention discloses a kind of method of infrared auxiliary hydration reaction on-line headspaces chromatography mass spectrometric determination tobacco water extract, comprise the following steps：(1) sealing bottleneck, headspace sample bottle inner bottom part are placed in drier after the test tube equipped with tobacco water extract is placed in headspace sample bottle；(2) infrared lamps headspace sample bottle to tobacco water extract reclaimed water steam is absorbed by drier completely, then carries out static headspace-GC-MS measure, is calculated by areas of peak normalization method, obtain the percentage contents of each component.The detection method that the present invention establishes, it is simple to operate, accurately, it is sensitive, with application value, can be effective for the analysis of the fragrant sample of cause containing moisture such as essence and flavoring agent, especially suitable for the solid sample containing moisture and wherein containing the fluid sample of component or the headspace sampling of solid sample that can be reacted with drier.
Description
Technical field
The invention belongs to chemical analysis field, relate to a kind of analysis method of tobacco water extract, and in particular to one kind
Head space-GC-MS of infrared auxiliary hydration reaction on-line determination tobacco water extract.
Background technology
The fragrance of tobacco is a variety of coefficient results of fragrance component with specific fragrance characteristic, different tobacco types
Kind or type identical kind under different ecological environments and cultivation condition, composition, content and the ratio of its fragrance component
Example is not quite similar, therefore shows different Type of aroma.Pass through qualitative and quantitative analysis, it will be appreciated that they are to cigarette product style
Influence, can provide technical basis and reference information for cigarette composition designer and meat flavor formulating technology personnel again.
Traditional tobacco flavor component extracting method has ultrasonic extraction, steam distillation extraction method, soxhlet extraction etc.,
But these methods have extraction time length, and extraction efficiency is low, and operating procedure is numerous and diverse, exposure chance is more, easily causes volatility
The loss of composition, the shortcomings of the distortion of sample message.In recent years, although SPE and solid phase micro-extraction technique have been used for tobacco
The assay of middle volatile ingredient, but the extracting head coat type of its extraction equipment is few, it is expensive, and service life is short,
It is used for multiple times and the problem of cross pollution is also present.Therefore quick, accurate and high sensitivity sample-pretreating method need to be established to use
The volatile ingredient in tobacco is detected in analysis.
Headspace technique is simple by its device in recent years, and cost is low, gas sampling, and chromatographic system is polluted less, and analyzes
Speed is fast, and the analysis detection of flavor component in tobacco is increasingly being applied to the features such as high sensitivity.Further, since tobaccoization
Study point more complicated, analyze the volatile ingredient in detection tobacco using headspace technique, separated volatile ingredient, be pure
Change and be enriched with, can both reduce interference component, turn avoid the pollution to follow-up chromatographic detection system, be easy, quick, sensitive
Spend high sample pre-treatments new technology.
The method of measure tobacco head space composition mainly has Static Headspace and Dynamic headspace method GC-MS etc. at present.
Static head space gas chromatography mass spectrography is that the headroom of the liquid or solid analyte in the closed container for reached balance takes
Gaseous sample, and a kind of more special analytical technology analyzed gaseous sample is combined with gaschromatographic mass spectrometry.Head space
The major advantage of gaseous state sampling makes the sample matrices composition of complexity together by band when being that of avoiding direct liquid or solid sampling
Enter the possibility of analytical instrument system, so as to eliminate by bringing into for matrix composition and to the analysis of volatile composition in sample
Caused influence and interference.But in current headspace sampling device, due to often some moisture in sample, with adding
Heat, pressurize, the moisture in sample also enters in gas-chromatography.Because damage of the water to gas chromatographic column is larger, and influence chromatogram
Peak, therefore the moisture how removed in sample is the key point of headspace analysis.
The content of the invention
Overcome the shortcomings of the prior art, provided for the head space on-line analysis detection of tobacco water extract volatile ingredient
A kind of simple, quick, highly sensitive analysis method.
A kind of method of the online HS GC mass spectrometric determination tobacco water extract of infrared auxiliary hydration reaction, including
Following steps：
(1) sealing bottleneck, headspace sample bottle inner bottom part after the test tube equipped with tobacco water extract is placed in headspace sample bottle
It is placed in drier；
(2) infrared lamps headspace sample bottle to tobacco water extract reclaimed water steam is absorbed completely, then carries out head space-gas
Phase chromatographic mass spectrometry determines, and is calculated by areas of peak normalization method, obtains the percentage contents of each component.
Infra-red radiation is the electromagnetic wave between visible ray and microwave, its wave-length coverage about 0.76 μm to 1000 μm it
Between, frequency is from 4 × 1014Hz to 3 × 1011Hz.It has advantages below：1) safety and environmental protection, compared with microwave, infra-red radiation pair
The harm of human body is minimum, the problem of leakage without consideration.2) efficient energy-saving, infra-red radiation heat are with electromagnetic wave transmission
, therefore during infrared heating, it is not necessary to any medium, heat loss is small, while will not also produce ring around any waste pollution
Border.3) firing rate is fast, and the energy of infra-red radiation is directly proportional to the power of radiation temperature 4.It can provide higher than Convective Heating by tens
Heat flow density again.It is a kind of preferable thermal source because infra-red radiation has high heat leak power and security, extensively should
The fields such as extraction and agricultural byproducts processing used in natural products.The present invention mainly makes tobacco water extraction using the heating of infrared auxiliary
Moisture rapid evaporation in thing, hydration reaction life occurs with drier (anhydrous sodium sulfate, anhydrous magnesium sulfate, anhydrous calcium chloride etc.)
Into hydrate, and then realize the purpose of water removal.It need to be extracted when carrying out headspace analysis inventive process avoids traditional water extract
A series of cumbersome handling processes such as take, be dehydrated, filtering, while avoiding drier and directly contacted with sample.
Preferably, the infrared lamp is placed in the bottom of headspace sample bottle.
Further preferably, the infrared lamp is apart from headspace sample bottom of bottle 1~3cm of portion.
More there is choosing, the infrared lamp is apart from headspace sample bottom of bottle portion 2cm.
Preferably, the power of the infrared lamp is 250~300W, and infrared lamp irradiation time is 10~60min.
Most preferably, the present invention investigated infrared lamp distance (2,4,6,8,10cm), infrared lamp power (100,150,175,
250th, 275W), heat time (10min, 20min, 30min, 40min, 50min, 60min) these key influence factors, see
The vapor volatilized in headspace sample bottle is examined, hydration reaction is carried out as standard using vapor and anhydrous magnesium sulfate completely, finally
Preferable condition is apart from ml headspace bottle bottom 2cm, in 275W infrared lamps 60min.
The present invention uses infrared heating mode, has the following advantages that：
(1) identical sample size needs 90min (being placed in column oven) using traditional heating, is volatilized in headspace sample bottle
The vapor gone out carries out hydration reaction completely with anhydrous magnesium sulfate；And use infrared heating mode, it is only necessary to 60min, greatly contract
The short water removal time.Because the absorption spectrum of water is in the range of 2.5 are in infra-red radiation between μ -25 μm, when infrared
When the wavelength of radiation is consistent with the absorbing wavelength of heating object, the material makes it easy to absorb infrared ray, molecular motion aggravation.
(2) in addition, using HS GC-mass spectral analysis is carried out after traditional heating, its total ion current figure is as schemed
Shown in 3 (A), total peak area is 2.32 × 108, and its total peak area of infrared heating is 8.05 × 108, intensity greatly reinforces, infrared
The reachable sample interior of radiation, makes its content temperature rise rapidly, acceleration is extracted the peripherad diffusion of composition, so as to shorten
Extraction time, improve extraction efficiency.
(3) traditional heating altogether it is qualitative go out 19 kinds of compounds (being shown in Table 1), mainly include a kind of alcohol compound, 4 kinds of aldehydes
Compound, 2 kinds of acid compounds, 2 kinds of ketone compounds, a kind of hydrocarbon compound, 8 kinds of heterocycle compounds, a kind of ester type compound.
From the point of view of percentage composition, heterocycle compound content highest accounts for 72.65%, and aldehyde compound, which takes second place, accounts for 18.78%, alcohols chemical combination
Thing, ketone compounds, ester type compound, alkenes compounds and acid compounds account for 6.54% respectively, 1.32%, 0.36%,
0.23%th, 0.11%.
Total ion current such as Fig. 3 of the infrared online HS GC mass spectrometric determination tobacco water extract of auxiliary hydration reaction
(B) shown in, altogether it is qualitative go out 30 kinds of volatile components (being shown in Table 2), main to include 2 kinds of alcohol compounds, 6 kinds of aldehyde compounds, 3 kinds
Acid compounds, 3 kinds of ketone compounds, a kind of hydrocarbon compound, 13 kinds of heterocycle compounds, 2 kinds of ester type compounds.From percentage
From the point of view of content, heterocycle compound content highest accounts for 60.17%, and acid compounds, which take second place, accounts for 19.89%, aldehyde compound, alcohol
Class compound, ketone compounds, ester type compound and alkenes compounds account for 12.91% respectively, 4.42%, 1.59%,
0.76%th, 0.25%, phenolic compound accounts for 0.80%.From the point of view of single compound, mainly there are nicotine (50.06%), acetic acid
(17.7%), some important aroma components such as 5 methyl furfural (4.07%), phytol (2.25%).
The offal water extract traditional heating qualitative, quantitative table of table 1
| Retention time | Compound name | Matching degree | Molecular formula | No. CAS | Percentage composition (%) |
| 9.31 | Furans | 95.8 | C4H4O | 110-00-9 | 1.92 |
| 16.44 | 2- methylfurans | 98.4 | C5H6O | 534-22-5 | 0.87 |
| 24.11 | 2 methyl butyraldehyde | 91.9 | C5H10O | 96-17-3 | 17.46 |
| 26.71 | 2,5- dimethyl-furans | 85.4 | C6H8O | 625-86-5 | 0.23 |
| 32.43 | 2- methylpyrroles | 86.1 | C5H7N | 636-41-9 | 0.25 |
| 39.83 | 2- methyltetrahydrofuran -3- ketone | 81.7 | C5H8O2 | 3188-00-9 | 0.18 |
| 43.51 | 3- furfurals | 98.6 | C5H4O2 | 498-60-2 | 0.57 |
| 46.86 | 3 Methylbutanoic acid | 84.2 | C5H10O2 | 503-74-2 | 0.05 |
| 47.46 | 2-Methyl Butyric Acid | 90 | C5H10O2 | 116-53-0 | 0.06 |
| 51.20 | 2- acetyl furans | 96.9 | C6H6O2 | 1192-62-7 | 0.04 |
| 55.42 | Benzaldehyde | 97.1 | C7H6O | 100-52-7 | 0.33 |
| 55.67 | Butyrolactone | 90.2 | C4H6O2 | 96-48-0 | 0.36 |
| 56.73 | 5 methyl furfural | 95.6 | C6H6O2 | 620-02-0 | 0.43 |
| 66.52 | Butadiene | 93.3 | C4H6 | 106-99-0 | 0.23 |
| 69.44 | 3- acetylpyridines | 88.8 | C7H7NO | 350-03-8 | 0.27 |
| 82.70 | Nicotine | 98.4 | C10H14N2 | 54-11-5 | 65.01 |
| 84.32 | Damascene ketone | 88 | C13H18O | 23726-93-4 | 1.14 |
| 87.91 | Myosmine | 90.7 | C9H10N2 | 532-12-7 | 4.07 |
| 100.41 | Phytol | 93.3 | C20H40O | 102608-53-7 | 6.54 |
Preferably, headspace analysis condition is：
Equilibrium temperature is 160 DEG C, and equilibration time is arranged to 30min, and transmission line temperature is 160 DEG C, and extraction time is
0.2min, sample injection time 0.5min, GC circulation time 120min.
Preferably, chromatographic condition is：Capillary chromatographic column DB-324,260 DEG C (60m × 1.8 μm of 320 μ m)；Injection port
Temperature：250℃；Temperature programming：Initial temperature is set to 40 DEG C, keeps 10min, rises to 150 DEG C with 2 DEG C/min, keeps 0min, so
260 DEG C are risen to 3 DEG C/min again afterwards, keeps 10min；Carrier gas：Helium (purity 99.999%)；Flow rate of carrier gas：1mL/min；Enter
Sample loading mode：Split sampling, split ratio 5:1, the μ L of sampling volume 1.
Mass Spectrometry Conditions are：Ion gun：Electron impact ion source (EI sources)；Electron energy：70eV；Transmission line temperature：260
℃；Ion source temperature：230℃；Detection pattern：Full ion scan monitoring, mass scan range are 50~450amu, sweep speed
It is 3scans/s.
Compared with existing analysis method, the HS GC mass spectrum for the on-line determination tobacco water extract that the present invention establishes
Method has advantages below：
(1) present invention uses thermal source of the infra-red radiation as hydration reaction, has firing rate fast, homogeneous heating, saves
Efficiently, the characteristics of safe and harmless, it is a kind of preferable thermal source.
(2) present invention is applied to the headspace sampling of the sample containing moisture, and its is simple in construction, easy to operate, avoids numerous
Trivial preprocessing process, on-line analysis detection quickly can be carried out to the sample containing moisture.
(3) detection method that the present invention establishes, not only increases the sensitivity of sample analysis, and make to eventually enter into chromatogram
The sample of post does not contain moisture, avoids chromatographic column and reduces service life because being influenceed by moisture.
(4) detection method that the present invention establishes, it is simple to operate, it is accurately, sensitive, there is application value, can be effective
For the analysis of the fragrant sample of cause containing moisture such as essence and flavoring agent, contain especially suitable for the solid sample containing moisture and wherein
There are the fluid sample of component or the headspace sampling of solid sample that can be reacted with drier.
Brief description of the drawings
Fig. 1 is the inventive method principle schematic.
Fig. 2 is that the offal water of heating means of the present invention extracts total ion current figure.
Fig. 3 is that conventional heating methods and the offal water of heating means of the present invention extract total ion current figure comparison diagram.
Embodiment
By following embodiments, the present invention is described further, but embodiment is not to technical solution of the present invention
Limit.
Embodiment 1
1. instrument and reagent
Instrument：The electronic analytical balances of AL 204 (plum Teller-support benefit instrument Shanghai Co., Ltd)；Head space auto injection fills
Put (Agilent Technologies 7697A, USA)；Gas chromatograph-mass spectrometer (GC-MS) (Agilent Technologies
7890A-5975C,USA)；Ml headspace bottle (20ml, Agilent Technologies)；Seal cap (polytetrafluoroethylene (PTFE), Agilent
Technologies,USA)；Infrared lamp (Haining City Qiyi Illumination Appliances Co., Ltd, Zhejiang, China)；Offal water extract sample
(offer of Li Qun thin slices factory)；Anhydrous magnesium sulfate (analyzes pure, Shishewei Chemical Co., Ltd., Shanghai).
2. the HS GC mass spectrography of infrared auxiliary hydration reaction on-line determination tobacco water extract
Comprise the following steps that：
Ⅰ：Preparation of samples：3g anhydrous magnesium sulfate samples accurately are weighed, 20ml headspace sample bottle bottom of bottle is positioned over, accurately pipettes
Then test tube is put in headspace sample bottle by 100 μ l offals water extracts in 2ml test tubes with tweezers, with containing polytetrafluoroethylene (PTFE)/
The aluminium cap of organosilicon dottle pin is sealed.
Ⅱ：Infrared auxiliary hydration reaction：Infrared lamp is set apart from ml headspace bottle bottom 2cm, in 275W infrared light irradiation
Certain time (10min, 20min, 30min, 40min, 50min, 60min), observe the vapor feelings in headspace sample in Fig. 1
Condition, the vapor for finding to volatilize in headspace sample bottle during 60min carry out hydration reaction i.e. vapor completely with anhydrous magnesium sulfate
Absorbed completely.
Ⅲ：Headspace analysis condition：Head space balance of plant temperature is 160 DEG C, and equilibration time is arranged to 30min, transmission line temperature
Spend for 160 DEG C, extraction time 0.2min, sample injection time 0.5min, GC circulation time 120min.
3. gas chromatography-mass spectrography analysis condition
Chromatographic condition：DB-324,260 DEG C of capillary chromatographic column (60m × 1.8 μm of 320 μ m)；Injector temperature：250
℃；Temperature programming：Initial temperature is set to 40 DEG C, keeps 10min, rises to 150 DEG C with 2 DEG C/min, 0min is kept, then again with 3
DEG C/min rises to 260 DEG C, keep 10min；Carrier gas：Helium (purity 99.999%)；Flow rate of carrier gas：1mL/min；Input mode：
Split sampling, split ratio 5:1, the μ L of sampling volume 1.
Mass Spectrometry Conditions：Ion gun：Electron impact ion source (EI sources)；Electron energy：70eV；Transmission line temperature：260℃；
Ion source temperature：230℃；Detection pattern：Full ion scan monitoring, mass scan range is 50~450amu, and sweep speed is
3scans/s。
4. the Qualitative and quantitative analysis of volatile ingredient
Qualitative analysis is set to 20 by automatic mass spectrum deconvolution qualitative systems, deconvolution parameter peak width, resolution ratio, sensitivity
And the requirement of chromatographic peak profile is set to medium, matching attribute minimum value is arranged to 80, signals assigned selection NIST11, in combination with
Document auxiliary is qualitative.Quantitative analysis is calculated by areas of peak normalization method, obtained by chem workstation data handling system
The percentage contents of each component.
5. tabacco water extracts the qualitative, quantitative result of volatile ingredient
Total ion current such as Fig. 2 of the infrared online HS GC mass spectrometric determination tobacco water extract of auxiliary hydration reaction
It is shown, altogether it is qualitative go out 30 kinds of volatile components (being shown in Table 2), mainly include 2 kinds of alcohol compounds, 6 kinds of aldehyde compounds, 3 kinds of acid
Class compound, 3 kinds of ketone compounds, a kind of hydrocarbon compound, 13 kinds of heterocycle compounds, 2 kinds of ester type compounds.Contain from percentage
From the point of view of amount, heterocycle compound content highest accounts for 60.17%, and acid compounds, which take second place, accounts for 19.89%, aldehyde compound, alcohols
Compound, ketone compounds, ester type compound and alkenes compounds account for 12.91% respectively, 4.42%, 1.59%, 0.76%,
0.25%, phenolic compound accounts for 0.80%.From the point of view of single compound, mainly have nicotine (50.06%), acetic acid (17.7%),
Some important aroma components such as 5 methyl furfural (4.07%), phytol (2.25%).
The offal water extract qualitative, quantitative table of table 2
6. method again investigate by property
In order to investigate the precision of this method, three are carried out to the volatile compound in offal water extract under these conditions
Secondary replicate analysis measure.Three kinds of main compound nicotine, acetic acid, the relative standard deviation (RSD) of phytol are respectively 3.39%,
4.65% and 5.77%, the RSD values of three kinds of compounds are respectively less than 10%, show that this method has good precision.
To sum up, the HS GC mass spectrography of infrared auxiliary hydration reaction on-line determination tobacco water extract is using energy-conservation
Efficiently, thermal source of the safe and harmless infra-red radiation as hydration reaction, avoid traditional water extract extracted, dehydrated,
A series of cumbersome handling processes such as filtering, while avoid drier and directly contacted with sample, it is a kind of simple, quick, accurate
Really, highly sensitive analysis method, there is application value, can be effective for the cause perfume (or spice) sample containing moisture such as essence and flavoring agent
The headspace analysis of product.
Claims (3)
1. a kind of method of the online HS GC mass spectrometric determination tobacco water extract of infrared auxiliary hydration reaction, its feature
It is, comprises the following steps：
(1) sealing bottleneck, headspace sample bottle inner bottom part are placed in after the test tube equipped with tobacco water extract is placed in headspace sample bottle
Drier, headspace analysis condition are：
Equilibrium temperature is 160 DEG C, equilibration time 30min, and transmission line temperature is 160 DEG C, extraction time 0.2min, during sample introduction
Between be 0.5min, GC circulation times are 120min；
(2) infrared lamps headspace sample bottle to tobacco water extract reclaimed water steam is absorbed by drier completely, then carry out head space-
Gaschromatographic mass spectrometry determines, and is calculated by areas of peak normalization method, obtains the percentage contents of each component；
The infrared lamp is placed in the bottom of headspace sample bottle, and the infrared lamp is described red apart from headspace sample bottom of bottle 1~3cm of portion
The power of outer lamp is 250~300W, and infrared lamp irradiation time is 10~60min.
2. method according to claim 1, it is characterised in that
Chromatographic condition is：Capillary chromatographic column DB-324,260 DEG C；Injector temperature：250℃；Temperature programming：Initial temperature is set
For 40 DEG C, 10min is kept, 150 DEG C is risen to 2 DEG C/min, keeps 0min, then rise to 260 DEG C again with 3 DEG C/min, keep
10min；Carrier gas：Helium；Flow rate of carrier gas：1mL/min；Input mode：Split sampling, split ratio 5:1, the μ L of sampling volume 1；
Mass Spectrometry Conditions are：Ion gun：Electron impact ion source；Electron energy：70eV；Transmission line temperature：260℃；Ion gun temperature
Degree：230℃；Detection pattern：Full ion scan monitoring, mass scan range is 50~450amu, sweep speed 3scans/s.
3. method according to claim 1, it is characterised in that the drier is anhydrous sodium sulfate, anhydrous magnesium sulfate or nothing
Water calcium chloride.
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| CN106474764B (en) * | 2016-11-24 | 2018-09-18 | 福州大学 | A kind of device and method of the headspace solid-phase microextraction removed water |
| CN107543879A (en) * | 2017-08-11 | 2018-01-05 | 安徽中烟工业有限责任公司 | The assay method of solid content in a kind of papermaking-method reconstituted tobaccos tobacco water extract |
| CN108828090A (en) * | 2018-04-28 | 2018-11-16 | 江苏中烟工业有限责任公司 | The detection method of dorinone in a kind of tobacco |
| CN108680694B (en) * | 2018-05-29 | 2020-12-08 | 云南中烟工业有限责任公司 | Method for measuring volatile chemical components in flue gas by using infrared mirror reverberatory furnace-headspace gas chromatography-mass spectrometry |
| CN114047273B (en) * | 2021-11-16 | 2024-10-29 | 云南中烟工业有限责任公司 | Method for measuring moisture content in cigarette bursting beads |
| CN115372529A (en) * | 2022-07-29 | 2022-11-22 | 上海化工院检测有限公司 | Headspace sample injection bottle for photolysis reaction research and use method |
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| US20050064076A1 (en) * | 2003-09-22 | 2005-03-24 | Fmc Technologies, Inc. | Method of measuring volatile components of foods |
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| US5191211A (en) * | 1992-03-23 | 1993-03-02 | Bridgestone/Firestone, Inc. | Thermal desorption method for separating volatile additives from vulcanizable rubber |
| CN105445402A (en) * | 2016-01-07 | 2016-03-30 | 云南中烟工业有限责任公司 | Headspace bottle for removing water in sample |
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