CN108519425A - A method of identifying tobacco mildew using High-Field unsymmetric ion migration spectral analysis technology - Google Patents

A method of identifying tobacco mildew using High-Field unsymmetric ion migration spectral analysis technology Download PDF

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Publication number
CN108519425A
CN108519425A CN201810246137.3A CN201810246137A CN108519425A CN 108519425 A CN108519425 A CN 108519425A CN 201810246137 A CN201810246137 A CN 201810246137A CN 108519425 A CN108519425 A CN 108519425A
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CN
China
Prior art keywords
tobacco
faims
ion
mildew
sample
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Pending
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CN201810246137.3A
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Chinese (zh)
Inventor
周沅桢
李�杰
朱明�
龙卫
胡小云
张波
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Hongyun Honghe Tobacco Group Co Ltd
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Hongyun Honghe Tobacco Group Co Ltd
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Priority to CN201810246137.3A priority Critical patent/CN108519425A/en
Publication of CN108519425A publication Critical patent/CN108519425A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/622Ion mobility spectrometry

Abstract

The present invention discloses a kind of method for identifying tobacco mildew using High-Field unsymmetric ion migration spectral analysis technology, this method is applied to tobacco, High-Field field asymmetric ion mobility composes (Field Asymmetric Waveform Ion Mobility Spectrometry, abbreviation FAIMS) it is the gaseous ion isolation technics to grow up on the basis of conventional ion migration spectrum, the present invention is detected to pipe tobacco volatile component using FAIMS detection techniques, by the feature FAIMS spectrum models for establishing the tobacco leaf volatile component that goes mouldy, and utilize sample detection collection of illustrative plates comparison model map identification tobacco mildew.

Description

It is a kind of to identify tobacco mildew using High-Field unsymmetric ion migration spectral analysis technology Method
Technical field
The present invention relates to a kind of methods for identifying tobacco mildew using High-Field unsymmetric ion migration spectral analysis technology.
Background technology
At present in pipe tobacco production process, mainly by manually observing, smelling is judged for tobacco mildew detection and decision procedure, Part cigarette enterprise near-infrared analyzer applied to tobacco mildew judge, part cigarette after near-infrared analyzer Main Basiss go mouldy Study on chemical compositions of leaves changes, and auxiliary identification is carried out according to situation of change, and accuracy rate is not high, and cannot distinguish slight go mouldy and again The difference gone mouldy is spent, cannot recognize that a small amount of tobacco leaf that goes mouldy contained in normal tobacco leaf.
After tobacco mildew, tobacco leaf volatile ingredient will produce variation, will produce special aldehyde radical class and ketone group class compound, cigarette The detection of leaf volatile ingredient can be analyzed by head space+chromatography of gases, and expensive equipment is complicated for operation, and detection and analysis are with high costs, and Analyze speed is slow, and data statistics is complicated, can be only applied to laboratory sample segment detection, still can pass through volatilization without a set of at present The method that property composition detection carries out quick recognition detection to the tobacco leaf that goes mouldy.
Invention content
The object of the present invention is to provide a kind of high use High-Field unsymmetric ion migration spectral analysis technologies of accuracy to identify The method of tobacco mildew.
In order to solve the above-mentioned technical problem, the technical scheme is that:It is a kind of to use High-Field unsymmetric ion migration spectrum The method that analytical technology identifies tobacco mildew is detected using the FAIMS detection techniques tobacco leaf volatile component that goes mouldy, by mould Become the FAIMS spectrum models of tobacco leaf feature volatile component, and mould using sample detection collection of illustrative plates comparison model map identification tobacco leaf Become.
Preferably, FAIMS principles are as follows:Gaseous sample is introduced into ionization area by carrier gas, sample molecule herein by Electric charge transfer or direct ionization ionization, are formed simultaneously negative ions.Ion cluster enters to be applied with to hang down with the gas flow of ions direction of motion The electrode raceway groove of straight rf wave signal, the movement locus of different types of ion cluster wherein is also different, this depends on ion Mobility under high-voltage radio-frequency signal.One lateral direct current compensation voltage is added on rf electric field, the side of offset voltage Back and forth change to intensity, to make the running orbit of each ion cluster that overall offset occur so that there is selection in different ions group Property reach Detection electrode, and then distinguish different test substances.
Preferably, realizing tobacco volatile ingredient analysis to be more preferable, it is 2000ml/min, sample that carrier gas flux, which rationally designs, Product throughput 100ml/min;CV ranging from -6~6V, DF ranging from 0~100%, carrier gas are by activated carbon and molecule well sifted The air of change in production process, selects suitable position to take the pipe tobacco collection of illustrative plates that gas scans as the sample detection collection of illustrative plates.Each collection of illustrative plates Including holotype and negative mode, according to aforesaid operations, tobacco sample detection of going mouldy is carried out using FAIMS, there are one spies of going mouldy for meeting Levy peak, whether judge whether tobacco leaf goes mouldy according to the presence of characteristic peak living containing the tobacco leaf that goes mouldy, and can according to the presence of characteristic peak, Judge the moulding ability of tobacco leaf.
Compared with prior art, the beneficial effects of the invention are as follows:High-Field asymmetric waveform ion mobility spectrometry is mainly used in Gas characteristic constituent analysis, when gas is a kind of gaseous ion isolation technics to grow up on the basis of conventional ion migration spectrum, It is to be based on the characteristics of different ions mobility is in nonlinear change under the conditions of normal pressure high electric field, is carried out at the same time to negative ions Scanning, ion in migration area by asymmetric waveform electric field and offset voltage collective effect, reach detector complete ion isolation with Identification has the characteristics that fast analyze speed, high sensitivity, low cost and without complicated pre-treatment.Based on tobacco volatile ingredient The every demand quickly detected, Selection utilization are based on the exploitation of FAIMS technical principles and are quickly detected to cigarette quality progress air blowing type Instrument.
Description of the drawings
Fig. 1 be the present invention go mouldy tobacco leaf analysis of volatile components test gas path device figure;
Fig. 2 is that the present invention is gone mouldy tobacco leaf volatile component testing result illustration;
Fig. 3 is that the present invention is gone mouldy FAIMS principle schematics in tobacco leaf volatile component.
Specific implementation mode
In the present embodiment, it should be noted that relational terms such as first and second and the like are used merely to one A entity or operation with another entity or operate distinguish, without necessarily requiring or implying these entities or operation it Between there are any actual relationship or orders.Moreover, the terms "include", "comprise" or its any other variant are intended to Cover non-exclusive inclusion, so that the process, method, article or equipment including a series of elements includes not only those Element, but also include other elements that are not explicitly listed, or further include for this process, method, article or setting Standby intrinsic element.
In addition, the connection between component or fixed form if not otherwise specified in this embodiment, connection or solid Determine mode can be fixed by bolt commonly used in the prior art or pin fix or axis pin connection etc. modes, therefore, this It is no longer described in detail in embodiment.
A method of it identifying tobacco mildew using High-Field unsymmetric ion migration spectral analysis technology, is detected using FAIMS The technology tobacco leaf volatile component that goes mouldy is detected, by the FAIMS spectrum models for the tobacco leaf feature volatile component that goes mouldy, and profit With sample detection collection of illustrative plates comparison model map identification tobacco mildew.
As shown in figure 3, FAIMS principles are as follows:Gaseous sample 1 is introduced into ionization area 2 by carrier gas, and sample molecule is herein It is ionized by electric charge transfer or direct ionization, is formed simultaneously negative ions, ion cluster, which enters, to be applied with and the gas flow of ions direction of motion The electrode raceway groove of vertical rf wave signal, the movement locus of different types of ion cluster wherein is also different, this depend on from Mobility of the son under high-voltage radio-frequency signal, a lateral direct current compensation voltage are added on rf electric field 3, offset voltage 4 Direction and intensity back and forth change, to make each ion cluster running orbit occur overall offset so that different ions group has Detection electrode is selectively reached, and then distinguishes different test substances.Ion is in migration area by asymmetric waveform electric field and benefit Voltage collective effect is repaid, detector 5 is reached and completes ion isolation and identification.
To make FAIMS be suitble to detect pipe tobacco volatile component, the design tobacco volatilization of Aided design FAIMS detection techniques is needed Sexual element analyzes process of gas path, specific as shown in Figure 1:Including sample analysis part 6 and instrument clean and standby sections 7, sample Analysis part 6 includes sample gas inlet 60, filter membrane 61, check-valves 62, third flow control 63 and tail gas outlet 64, the sample gas Entrance 60 is connected between filter membrane 61, check-valves 62, third flow control 63 and tail gas outlet 64 by the circulating air flow path 65 of setting It connects;Instrument clean and standby sections 7 include air intake 70, the first asepwirator pump 71, first-class control 72, the first activated carbon/molecule Sieve 73, check-valves 62, FAIMS74, surge tank 75, the second asepwirator pump 76, the second activated carbon/molecular sieve 77 and the second flow control 78, The air intake 70, the first asepwirator pump 71, first-class control 72, the first activated carbon/molecular sieve 73, check-valves 62, FAIMS74, Pass through the circulating air flow path of setting between surge tank 75, the second asepwirator pump 76, the second activated carbon/molecular sieve 77 and the second flow control 78 Connection.
It can be seen from figure 1 that process of gas path figure is divided into two parts, a part of sample analysis flow chart, another part is instrument Cleaning and standby flow chart.During sample analysis, asepwirator pump provides whole flow process gas air source power, is flowed by controlling Amount controller controls the total flow size of entire analytic process, controls the flow of flow controller, can control in cycle gas circuit There is portion gas discharge, and supplemented by way of sample gas sucking as the gas of exhaust gas discharge, this is just to introduce sample gas Provide possibility.And cleaning process after sample analysis and it is standby when instrument can be automatically into cleaning process.
More preferably to realize tobacco volatile ingredient analysis, it is 2000ml/min, sample gas flow that carrier gas flux, which rationally designs, 100ml/min;CV ranging from -6~6V, DF ranging from 0~100%.Carrier gas is the air by activated carbon and molecular sieve purification. In production process, suitable position is selected to take the pipe tobacco collection of illustrative plates that gas scans as the sample detection collection of illustrative plates.Each collection of illustrative plates includes holotype Formula and negative mode, left side is holotype in Fig. 2, and right side is negative mode.
According to aforesaid operations, tobacco sample detection of going mouldy is carried out using FAIMS, there are one characteristic peak (red circles of going mouldy for meeting It is interior), it is living whether containing the tobacco leaf that goes mouldy to judge whether tobacco leaf goes mouldy according to the presence of characteristic peak, and can according to the presence of characteristic peak, Judge the moulding ability of tobacco leaf.
FAIMS detection techniques have begun to be applied to customs inspection, airport security, counterterrorism operations, the drugs side of tracking down and arrest at present Face, and succeeding, but be detected applied to the tobacco leaf that goes mouldy and identification there is no related data and report.
Tobacco mildew detects and decision procedure is mainly by manually observing, judge, or uses near-infrared analyzer, according to chemistry Composition transfer situation carries out auxiliary identification, and accuracy rate is not high, and cannot distinguish the slight difference gone mouldy with severe of going mouldy, Bu Nengshi Do not go out a small amount of tobacco leaf that goes mouldy contained in normal tobacco leaf.Present invention application FAIMS detection techniques go mouldy tobacco leaf volatile component into Row detection by the FAIMS spectrum models for the tobacco leaf feature volatile component that goes mouldy, and utilizes sample detection collection of illustrative plates comparison model figure Spectrum identification tobacco mildew, may be implemented quick, easy, accurate detection, and can distinguish the slight difference gone mouldy with severe of going mouldy, energy Identify a small amount of tobacco leaf that goes mouldy contained in normal tobacco leaf.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any The change or replacement expected without creative work, should be covered by the protection scope of the present invention.

Claims (3)

1. a kind of method for identifying tobacco mildew using High-Field unsymmetric ion migration spectral analysis technology, it is characterised in that:Using The FAIMS detection techniques tobacco leaf volatile component that goes mouldy is detected, and passes through the FAIMS collection of illustrative plates for the tobacco leaf feature volatile component that goes mouldy Model, and utilize sample detection collection of illustrative plates comparison model map identification tobacco mildew.
2. the method according to claim 1 for identifying tobacco mildew using High-Field unsymmetric ion migration spectral analysis technology, It is characterized in that:FAIMS principles are as follows:Gaseous sample is introduced into ionization area by carrier gas, and sample molecule is turned by charge herein It moves or directly ionization ionizes, be formed simultaneously negative ions.Ion cluster, which enters, is applied with vertical with the gas flow of ions direction of motion penetrate The electrode raceway groove of frequency wave signal, the movement locus of different types of ion cluster wherein is also different, this depends on ion in high pressure Mobility under radiofrequency signal.One lateral direct current compensation voltage is added on rf electric field, the direction of offset voltage and strong Degree is reciprocal to be changed, to make the running orbit of each ion cluster that overall offset occur so that different ions group selectively arrives Up to Detection electrode, and then distinguish different test substances.
3. the method according to claim 1 for identifying tobacco mildew using High-Field unsymmetric ion migration spectral analysis technology, It is characterized in that:More preferably to realize tobacco volatile ingredient analysis, it is 2000ml/min, sample gas that carrier gas flux, which rationally designs, Measure 100ml/min;CV ranging from -6~6V, DF ranging from 0~100%, carrier gas are the sky by activated carbon and molecular sieve purification Gas in production process, selects suitable position to take the pipe tobacco collection of illustrative plates that gas scans as the sample detection collection of illustrative plates.Each collection of illustrative plates includes just Pattern and negative mode carry out tobacco sample detection of going mouldy, there are one the characteristic peak that goes mouldy, roots for meeting according to aforesaid operations using FAIMS It is living whether containing the tobacco leaf that goes mouldy according to whether the presence judgement tobacco leaf of characteristic peak goes mouldy, and can judge cigarette according to the presence of characteristic peak The moulding ability of leaf.
CN201810246137.3A 2018-03-23 2018-03-23 A method of identifying tobacco mildew using High-Field unsymmetric ion migration spectral analysis technology Pending CN108519425A (en)

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CN109668992A (en) * 2017-10-13 2019-04-23 贵州中烟工业有限责任公司 A kind of mildew classification of flue-cured tobacco leaves method
CN110118857A (en) * 2019-05-24 2019-08-13 福建中烟工业有限责任公司 Cigarette microorganism introduces the detection method of risk and reduces the method for introducing risk
CN110514614A (en) * 2019-05-05 2019-11-29 贵州中烟工业有限责任公司 One kind being used for throwing material grunge pollution online test method
CN112362720A (en) * 2020-10-29 2021-02-12 河南中烟工业有限责任公司 Detection method for mildew of boxed tobacco leaves
CN114113391A (en) * 2021-11-24 2022-03-01 贵州中烟工业有限责任公司 Method for detecting content of expansion medium

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CN109668992A (en) * 2017-10-13 2019-04-23 贵州中烟工业有限责任公司 A kind of mildew classification of flue-cured tobacco leaves method
CN110514614A (en) * 2019-05-05 2019-11-29 贵州中烟工业有限责任公司 One kind being used for throwing material grunge pollution online test method
CN110118857A (en) * 2019-05-24 2019-08-13 福建中烟工业有限责任公司 Cigarette microorganism introduces the detection method of risk and reduces the method for introducing risk
CN112362720A (en) * 2020-10-29 2021-02-12 河南中烟工业有限责任公司 Detection method for mildew of boxed tobacco leaves
CN114113391A (en) * 2021-11-24 2022-03-01 贵州中烟工业有限责任公司 Method for detecting content of expansion medium
CN114113391B (en) * 2021-11-24 2024-03-26 贵州中烟工业有限责任公司 Method for detecting content of expansion medium

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Application publication date: 20180911