CN103162994A - Ultra-low temperature extraction device and analysis method of smoke aroma components by using ultra-low temperature extraction device - Google Patents
Ultra-low temperature extraction device and analysis method of smoke aroma components by using ultra-low temperature extraction device Download PDFInfo
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- CN103162994A CN103162994A CN2013101056156A CN201310105615A CN103162994A CN 103162994 A CN103162994 A CN 103162994A CN 2013101056156 A CN2013101056156 A CN 2013101056156A CN 201310105615 A CN201310105615 A CN 201310105615A CN 103162994 A CN103162994 A CN 103162994A
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Abstract
The invention discloses an ultra-low temperature extraction device and an analysis method of smoke aroma components by using the ultra-low temperature extraction device combining with a full two-dimensional gas-phase time-of-flight mass spectrometer. Compared with a conventional method, the analysis method is low in price, easy to operate, free from high temperature and high pressure treatment in separation and enrichment processes thus guaranteeing the characteristics of original aroma components in smoke, being capable of being used for collecting and enriching aroma components in particulate matters and gaseous matters of the smoke simultaneously, and being capable of being used for detection by utilizing the full two-dimensional gas-phase time-of-flight mass spectrometer simultaneously, so that the device and the method have the advantages of good degree of separation, high sensitivity and accuracy, and high analysis speed.
Description
Technical field
The invention belongs to the Tobacco Analysis field, be specifically related to a kind of ultralow temperature extraction element and with the method for this device analysis flue gas fragrance component.
Background technology
Tobacco is a kind of directly edible, but by sucking the rear smoke components that produces of burning to certain physiological action of human oral cavity.Generally speaking, people suck from tobacco is the chemical composition that in combustion process, thermal cracking produces and heats up in a steamer through heat the original chemical composition of part tobacco leaf that volatilization enters flue gas, and the flue gas fragrance component that can experience directly affects the sucking quality of cigarette.Composition, the character of grasping fragrance component in flue gas are to improve the basis that tobacco leaf is sucked feature, and therefore, the fragrance component tool of analyzing and studying in flue gas is of great significance.Chinese scholars has been carried out many researchs to the smoke of tobacco composition, the Extraction and enrichment that the analysis of flue gas fragrance component is related generally to flue gas with separate two processes of identifying, Extraction and enrichment technology commonly used is mainly by the absorption of smoking machine cambridge filter or solvent extraction at present, and then adopt as steam distillation, solvent extraction, the while distillation extraction, solid-phase microextraction, the further separation and concentration of the technology such as head space condistillation, recycle at last conventional one dimension capillary column gas chromatography (GC), the Analysis and Identification technology of gas chromatography/mass spectrometry (GC/MS) is carried out qualitative and quantitative analysis to it.But, because smoking machine is expensive, operation is relatively complicated, and utilize cambridge filter only can collect the fragrance component in Smoke Particulate, traditional one dimension chromatographic peak finite capacity of while, lack of resolution, for the such complex sample of flue gas fragrance component, overlap of peaks is serious, affects mass spectrometry and quantitative accuracy.(new technology of GC * GC-TOFMS), comprehensive two dimensional gas chromatography is connected two different capillary columns of polarity by modulator, make resolution and sensitivity greatly improve complete two-dimentional gas phase flight time mass spectrum to have occurred in recent years.The rapid data collection function of this technology and distinctive Data Analysis software have been expanded the separation identification capacity to the flue gas complex sample greatly.
The present invention is directed to the existing deficiency that exists in flue gas fragrance component technology of analyzing improves, specialized designs a kind of ultralow temperature solvent extraction device, fragrance component under the ultralow temperature state in separation and enriched flue gas carries out qualitative and quantitative analysis through the complete two-dimentional gas phase flight time mass spectrum of concentrated recycling.The method simplicity of design is practical, can analyze simultaneously multiple fragrance component in flue gas.
Summary of the invention
the practical problems that the present invention will solve: prior art exists operation relatively complicated, utilize cambridge filter only can collect the fragrance component in Smoke Particulate, traditional one dimension chromatographic peak finite capacity of while, lack of resolution, for the such complex sample of flue gas fragrance component, overlap of peaks is serious, affect mass spectrometry and quantitative accuracy, the present invention is directed to the existing deficiency that exists in flue gas fragrance component technology of analyzing improves, specialized designs a kind of ultralow temperature solvent extraction device, collect the fragrance component in enriched flue gas under the ultralow temperature state, after concentrated in conjunction with complete two-dimentional gas phase flight time mass spectrum qualitative and quantitative analysis.This method simplicity of design is practical, can analyze simultaneously multiple fragrance component in flue gas, have cheap, simple to operate, and in the separation and concentration process without high temperature high pressure process, guarantee original fragrance component feature in flue gas, and simultaneously the fragrance component in Smoke Particulate and gas gas-phase objects is collected enrichment; Utilize simultaneously complete two-dimentional gas phase flight time mass spectrum to detect, degree of separation is better, and sensitivity and accuracy are higher.
The technical solution used in the present invention:
The ultralow temperature extraction element comprises extraction vessel and liquid nitrogen plan, and the extraction solvent is housed in extraction vessel, and liquid nitrogen is housed in liquid nitrogen plan, meets the mouth place and can load onto cigarette, and bleeding point can be bled, and in upper shed place of extraction vessel, operation valve is housed.
the ultralow temperature extraction element is analyzed the method for flue gas fragrance component: be equipped with in extraction vessel and extract solvent (2), fill liquid nitrogen in liquid nitrogen plan, load onto cigarette meeting the mouth place, and light, bleed at bleeding point, by operation valve control and suck speed, thereby control cigarette and burn and suck speed, utilize above-mentioned ultralow temperature solvent extraction plant to carry out separated and collected to the flue gas fragrance component, solution after extraction is thawed at normal temperatures, add the internal standard compound phenethyl acetate in extracting solution, be concentrated at normal temperatures and pressures 1-2 mL with Rotary Evaporators again, utilize at last complete two-dimentional gas phase flight time mass spectrum to carry out qualitative and quantitative analysis to sample.
Extracting solvent is 200-300 mL ether.
Selecting cigarette quantity is that 10-20 props up.
Under normal temperature and pressure, extract is thawed.
Use Rotary Evaporators to concentrate under normal temperature and pressure.
Complete two-dimentional gas phase flight time mass spectrum condition: post 1:DB-1; Post 2:DB-17; Temperature programme: 60 ℃ keep 2 min, then rise to 250 ℃ and keep 10 min with 4 ℃/min; The programmed pressure pattern; Injection port pressure: 30 psi keep 2 min then to rise to 49 psi and keep 10 min with 0.4 psi/min; Sample working time: 57.5 min; Injector temperature: 280 ℃; Sample introduction pattern: do not shunt; Modulation period: 8 s; Duration: 300 ms; Hot spout: 370 ℃; Cold spout flow velocity: 18 L/min; Hot spout pressure: 40 psi; Mass spectrum condition: ion gun: EI, 70 eV; Ion source temperature: 280 ℃; Transmission line temperature: 300 ℃; Mass range: 45-450 m/z; Resolution: 4000 FWHM; Picking rate: 100 Hz.
In the present invention, the Rotary Evaporators that utilizes is provided by HEIDOLPH, and (GC * GC-TOFMS) provided by ZOEX, selected ultralow temperature solvent extraction device is self-control to complete two-dimentional gas phase flight time mass spectrum.
Interior mark compound in the present invention is selected phenethyl acetate.
The technique effect that the present invention reaches:
the present invention analyzes flue gas fragrance component method with other and compares, mainly selected a kind of ultralow temperature solvent extraction device of making by oneself to collect at first simultaneously fragrance component in Smoke Particulate and gas gas-phase objects, (196 ℃) use ether as extracting solvent under the nitrogen ultra low temperature environment, make flue gas constantly by the low-temperature extraction solvent under the effect of suction, thereby make fragrance component dissolution in low temperature in flue gas in extracting solvent, then thaw at normal temperatures and pressures, cooled fragrance component directly is dissolved in extracts in solvent, in conjunction with complete two-dimentional gas phase flight time mass spectrum, fragrance component is carried out Analysis and Identification more at last, multiple fragrance component in disposable Analysis and Identification flue gas.The method does not use smoking machine or cambridge filter to collect enrichment to flue gas fragrance, experimental expenses and operation easier have not only greatly been saved, simultaneously can also collect simultaneously and extract the fragrance component in Smoke Particulate and gas gas-phase objects, solve the shortcoming that cambridge filter can't be collected fragrance component in gas gas-phase objects.In addition, the method combines complete two-dimentional gas phase flight time mass spectrum and carries out qualitative and quantitative analysis, has not only improved the degree of separation of complex sample, accuracy and the reliability of method have been improved simultaneously, and simple to operate, analysis time is short, is suitable for the detection analysis of batch sample.
Repeatability and accuracy to the inventive method are measured
,Adopt identical processing mode respectively same sample to be carried out 3 replicate determinations every day, METHOD FOR CONTINUOUS DETERMINATION 3 days is calculated respectively and is in a few days reached relative standard deviation (RSD) in the daytime, and with the positive and negative matching degree situation of NIST08 standard mass spectral database, result is as shown in table 1.
Can find out from above-mentioned table 1: separate through complete two-dimentional gas phase flight time mass spectrum and identify, altogether Preliminary Identification 54 kinds of fragrance components in the cigarette smoke.By with direct analogy degree and the anti-similarity of standard spectrum storehouse NIST08 retrieval, its positive and negative matching degree is all greater than 80%, wherein the direct analogy degree has 25 kinds of compounds greater than 90%, account for to separate and identify 46.3% of total compound, and anti-similarity has 42 kinds of compounds greater than 90%, account for to separate and identify more than 77.7% of total compound, further illustrate authenticating compound reliability qualitatively.In addition, from stability and the reappearance of method, survey 3 times every day for same sample, METHOD FOR CONTINUOUS DETERMINATION 3 days all lower than 20%, wherein only has 12 kinds of compounds greater than 10% compound at relative standard deviation mean value in a few days, and all the other are all lower than below 10%; Equally, also all lower than 20%, wherein there are 27 kinds lower than 10% compound for the mean value of relative standard deviation in the daytime.So from a few days relative standard deviation and relative standard's standard deviation in the daytime, the stability of the method and reappearance all show better.Can find out from complete two-dimentional gas phase flight time mass spectrum figure, the fragrance component in cigarette smoke has all showed degree of separation preferably in two-dimentional chromatogram, sees accompanying drawing 2.
Description of drawings:
Accompanying drawing 1 is the structural representation of ultralow temperature extraction element of the present invention.
Accompanying drawing 2 adopts method of the present invention to separate the design sketch of volatile aroma in tobacco leaf
Embodiment:
Embodiment 1
The present invention is further described by following instantiation, but does not limit the present invention.
With Cigarette 22 ℃ ± 1 ℃ of temperature, under relative humidity 60% ± 2% condition more than balance 48 h.The 200-300 mL ether extracted liquid of packing in extraction vessel (6) is contained a certain amount of liquid nitrogen in liquid nitrogen container (7), get cigarette 10-20 and prop up and utilize above-mentioned homemade ultralow temperature solvent extraction plant to carry out separated and collected to the flue gas fragrance component.Solution after extraction is thawed at normal temperatures and pressures, add a certain amount of internal standard compound phenethyl acetate in extracting solution, then utilize Rotary Evaporators to be concentrated at normal temperatures and pressures 1-2 mL.Utilize at last complete two-dimentional gas phase flight time mass spectrum to carry out qualitative and quantitative analysis to sample.
Complete two-dimentional gas phase flight time mass spectrum condition: post 1:DB-1; Post 2:DB-17; Temperature programme: 60 ℃ keep 2 min, then rise to 250 ℃ and keep 10 min with 4 ℃/min; The programmed pressure pattern; Injection port pressure: 30 psi keep 2 min then to rise to 49 psi and keep 10 min with 0.4 psi/min; Sample working time: 57.5 min; Injector temperature: 280 ℃; Sample introduction pattern: do not shunt; Modulation period: 8 s; Duration: 300 ms; Hot spout: 370 ℃; Cold spout flow velocity: 18 L/min; Hot spout pressure: 40 psi; Mass spectrum condition: ion gun: EI, 70 eV; Ion source temperature: 280 ℃; Transmission line temperature: 300 ℃; Mass range: 45-450 m/z; Resolution: 4000 FWHM; Picking rate: 100 Hz.
Embodiment 2
Adopt the inventive method to measure the fragrance component of different brands cigarette smoke, wherein sample is mainly derived from the brand cigarette (representing with A, B, C, D respectively) in four kinds of commercially available different places of production, detect 54 kinds of flue gas fragrance components of cigarette by said method, its testing result sees Table 2:
Annotate: above-mentioned data unit is that μ g/ props up, and is three times and measures mean value.
Detecting data by upper table 2 can find out, the flue gas fragrance component content of different brands cigarette is different, and this may cause the different brands cigarette to have different suction fragrance characteristics, to satisfy the hobby of different crowd to smoking.Therefore, the analytical approach of the present invention's foundation can detect the flue gas fragrance component in different-style feature cigarette.
Claims (8)
1. ultralow temperature extraction element, comprise extraction vessel (6) and liquid nitrogen plan (7), it is characterized in that: be equipped with in extraction vessel (6) and extract solvent (2), liquid nitrogen (3) is housed in liquid nitrogen plan (7), connecing mouth (1) locates to load onto cigarette, the interface (5) of bleeding can be bled, and in upper shed place of extraction vessel (6), flue gas flow rate operation valve (4) is housed.
2. ultralow temperature extraction element according to claim 1 is analyzed the method for flue gas fragrance component, it is characterized in that: be equipped with in extraction vessel (6) and extract solvent (2), fill liquid nitrogen (3) in liquid nitrogen plan (7), locate to load onto cigarette connecing mouth (1), and light, bleed at bleeding point (5), by operation valve (4) control and suck speed, the flue gas fragrance component is carried out separated and collected, after being thawed, solution after extraction adds the internal standard compound phenethyl acetate, be concentrated into 1-2 mL with Rotary Evaporators again, utilize at last complete two-dimentional gas phase flight time mass spectrum to carry out qualitative and quantitative analysis to sample.
3. ultralow temperature extraction element according to claim 2 is analyzed the method for flue gas fragrance component, and it is characterized in that: the cooling liquid of ultralow temperature (2) is liquid nitrogen.
4. ultralow temperature extraction element according to claim 2 is analyzed the method for flue gas fragrance component, it is characterized in that: extract solvent (2) and be ether.
5. ultralow temperature extraction element according to claim 2 is analyzed the method for flue gas fragrance component, it is characterized in that: selecting cigarette quantity is that 10-20 props up.
6. ultralow temperature extraction element according to claim 2 is analyzed the method for flue gas fragrance component, it is characterized in that: under normal temperature and pressure, extract is thawed.
7. ultralow temperature extraction element according to claim 2 is analyzed the method for flue gas fragrance component, it is characterized in that: use Rotary Evaporators to concentrate under normal temperature and pressure.
8. ultralow temperature extraction element according to claim 2 is analyzed the method for flue gas fragrance component, and it is characterized in that: detecting instrument is complete two-dimentional gas phase flight time mass spectrum, and its analysis condition is as follows: post 1:DB-1; Post 2:DB-17; Temperature programme: 60 ℃ keep 2 min, then rise to 250 ℃ and keep 10 min with 4 ℃/min; The programmed pressure pattern; Injection port pressure: 30 psi keep 2 min then to rise to 49 psi and keep 10 min with 0.4 psi/min; Sample working time: 57.5 min; Injector temperature: 280 ℃; Sample introduction pattern: do not shunt; Modulation period: 8 s; Duration: 300 ms; Hot spout: 370 ℃; Cold spout flow velocity: 18 L/min; Hot spout pressure: 40 psi; Mass spectrum condition: ion gun: EI, 70 eV; Ion source temperature: 280 ℃; Transmission line temperature: 300 ℃; Mass range: 45-450 m/z; Resolution: 4000 FWHM; Picking rate: 100 Hz.
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| CN104316381A (en) * | 2014-11-05 | 2015-01-28 | 中国科学院生态环境研究中心 | Sample extracting, purifying and concentrating integrated device and sample preprocessing method |
| CN106353419A (en) * | 2016-08-16 | 2017-01-25 | 国家烟草质量监督检验中心 | Method for measuring aroma components in main stream smoke of cigarettes |
| CN109564147A (en) * | 2016-06-03 | 2019-04-02 | 普度研究基金会 | System and method for analyzing the analyte for using adsorbent material to extract from sample |
| CN110133156A (en) * | 2019-06-24 | 2019-08-16 | 中国烟草总公司郑州烟草研究院 | The analysis method of super more target flavor components in a kind of high throughput assay tobacco juice for electronic smoke |
| CN110133155A (en) * | 2019-06-24 | 2019-08-16 | 中国烟草总公司郑州烟草研究院 | A kind of gas chromatography tandem mass spectrometry analysis method of essence spice for cigarette |
| CN110208414A (en) * | 2019-06-24 | 2019-09-06 | 中国烟草总公司郑州烟草研究院 | A kind of analysis method quantitative determining super more target flavor components in tobacco |
| CN110836942A (en) * | 2019-11-29 | 2020-02-25 | 浙江省农业科学院 | Method for analyzing smelly components in fruit and vegetable products |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104316381A (en) * | 2014-11-05 | 2015-01-28 | 中国科学院生态环境研究中心 | Sample extracting, purifying and concentrating integrated device and sample preprocessing method |
| CN104316381B (en) * | 2014-11-05 | 2017-06-20 | 中国科学院生态环境研究中心 | The method of sample extraction, purification and concentration integrated device and sample pre-treatments |
| CN109564147A (en) * | 2016-06-03 | 2019-04-02 | 普度研究基金会 | System and method for analyzing the analyte for using adsorbent material to extract from sample |
| CN109564147B (en) * | 2016-06-03 | 2022-02-18 | 普度研究基金会 | Systems and methods for analyzing analytes extracted from a sample using an adsorbent material |
| CN106353419A (en) * | 2016-08-16 | 2017-01-25 | 国家烟草质量监督检验中心 | Method for measuring aroma components in main stream smoke of cigarettes |
| CN110133156A (en) * | 2019-06-24 | 2019-08-16 | 中国烟草总公司郑州烟草研究院 | The analysis method of super more target flavor components in a kind of high throughput assay tobacco juice for electronic smoke |
| CN110133155A (en) * | 2019-06-24 | 2019-08-16 | 中国烟草总公司郑州烟草研究院 | A kind of gas chromatography tandem mass spectrometry analysis method of essence spice for cigarette |
| CN110208414A (en) * | 2019-06-24 | 2019-09-06 | 中国烟草总公司郑州烟草研究院 | A kind of analysis method quantitative determining super more target flavor components in tobacco |
| CN110836942A (en) * | 2019-11-29 | 2020-02-25 | 浙江省农业科学院 | Method for analyzing smelly components in fruit and vegetable products |
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Application publication date: 20130619 |