CN103134848A - Qualitative and semi-quantitative analysis method for sample detection by ion mobility spectrometry - Google Patents
Qualitative and semi-quantitative analysis method for sample detection by ion mobility spectrometry Download PDFInfo
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- CN103134848A CN103134848A CN2011103929389A CN201110392938A CN103134848A CN 103134848 A CN103134848 A CN 103134848A CN 2011103929389 A CN2011103929389 A CN 2011103929389A CN 201110392938 A CN201110392938 A CN 201110392938A CN 103134848 A CN103134848 A CN 103134848A
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Abstract
The invention discloses a qualitative and semi-quantitative analysis method for sample detection by an ion mobility spectrometry. An ion mobility spectrometry technology is used as the basic detection technology, and the ion mobility spectrometry in a positive ion mold and a negative ion mold is adopted to establish the qualitative and semi-quantitative analysis method to detect different samples. Self-configuration ion mobility spectrometry analysis software can automatically generate a standard curve, automatically input a standard curve equation and automatically alarm to display the quantity of the samples. According to the qualitative and semi-quantitative analysis method for sample detection by the ion mobility spectrometry, a citric acid fentanyl narcotic sample (FK) is used as an example, a standard curve equation y=1.3451+0.4044x is created in the range of 1-60 ng, and a correlation coefficient r is larger than 0.99. The qualitative and semi-quantitative analysis method is simple, quick and efficient and can be widely used in qualitative and semi-quantitative analysis for the sample detection by the ion mobility spectrometry.
Description
Technical field
The present invention relates to a kind of qualitative, semi-quantitative analysis method for the ion mobility spectrometry test sample.Take Ion mobility spectrometry as basic detection technique, adopt positive and negative ion pattern ion mobility spectrometry to set up qualitative, the semi-quantitative analysis method that ion mobility spectrometry detects different samples specifically.Self-built ion mobility spectrometry analysis software can automatically generate typical curve, automatically import typical curve equation, automatic alarm show sample quantity.This method is easy, quick, efficient, can be widely used in ion mobility spectrometry fast qualitative, semi-quantitative analysis.The method analysis speed is fast, and test operation is simple, need not special specialty background personnel operation.
Background technology
Ion mobility spectrometry (Ion Mobility Spectrometry, IMS) technology is a kind of quick separation detection technique that 20 century 70s occur, and compares with traditional mass spectrum, chromatographic apparatus, have simple in structure, highly sensitive, analysis speed is fast, the characteristics of reliable results.Can detect micro substance in atmospheric environment, be suitable for on-the-spot the use.We IMS of research has been widely used in the fields such as chemical warfare agent, drugs, explosive detection, environmental monitoring, monitoring poisonous gas, fire monitoring, water pollution monitoring and Food Monitoring at present.Ion mobility spectrometry mainly is comprised of sampling device, chamber, ion gate, drift region, detecting device and receiving system.Sample gas produces molecule, ion in chamber ionization.Ion enters the drift region by the ion gate that periodicity is opened under the ordering about of electric field.In the process that the neutral drift gas molecule with adverse current constantly collides, migration rate is different separately in electric field due to these ions, makes different ions be separated, and successively arrives collector detected.Therefore just can determine the existence of evaluating objects material by transit time.
At present mass spectrum, chromatographic apparatus have been widely used in the quantitative test field.Quantitative test instrument majority is the concentration that application peak area or peak height are determined respective substance.And the quantitative test of ion mobility spectrometry due to self reason also could not picture element spectrum, chromatographic apparatus be applied like that.The scope of using detection along with ion mobility spectrometry is more and more wider, and the quantitative demand of analyzing and testing also more and more receives much concern.
Summary of the invention
The purpose of this invention is to provide a kind of qualitative, semi-quantitative analysis new method for the ion mobility spectrometry test sample,
1) in the quantitative concentrations scope that sample to be analyzed is surveyed, get different volumes, more than five, the sample of known variable concentrations enters respectively the ion mobility spectrometry sampling system and detects, the analysis software of ion mobility spectrometry detector is identified variable concentrations sample signal intensity automatically;
The same concentration sample repeats to get more than 3 times its mean value; The mean value of each sample concentration signal intensity and counter sample concentration numerical value are automatically got 10 and are end natural logarithm, as the coordinate of X-axis, Y-axis, generate typical curve respectively, and then match generates the typical curve equation;
2) sample to be analyzed is entered the ion mobility spectrometry sampling system and detect, the analysis software of ion mobility spectrometry detector is identified sample signal intensity automatically;
Corresponding signal peak signal intensity by the equation of match, calculates unknown concentration fentanyl citrate arcotic sample solution concentration; Quantitatively shown by software terminal.
With dripping after the sample dry out solvent on coupongs, be sent to the ion mobility spectrometry detector and analyze, obtain detection signal, carry out the quantitative and semi-quantitative analysis.
The coupongs that contain sample steam by well heater and desolventize, and heating-up temperature 20-50 ℃, the coupongs that then will contain sample are sent to pyrolysis and analyse injector, carry sample molecule by air do carrier gas and are sent to the ion mobility spectrometry detector and analyze.
Utilize positive and negative ion pattern ion mobility spectrometry, prepare five variable concentrations sample solutions (quantitative test concentration is determined in the pre-treatment test) and enter respectively the ion mobility spectrometry sampling system, software is identified variable concentrations sample signal intensity automatically; The same concentration sample repeatedly repeats to get its mean value; The mean value of each sample concentration signal intensity and counter sample concentration numerical value are taken the logarithm automatically, then generate the typical curve equation, are used for the quantitative alarm mode of software terminal.
This semi-quantitative analysis method allows sample to enter detection system by different ion mobility spectrometry sampling systems.Sampling system comprises that high temperature pyrolysis analyses injector or gas sampling system, then carries sample molecule by carrier gas and enters into the ion mobility spectrometry detector and analyze.
Adopt special rational disposal route in the statistical study of data.The same concentration sample will carry out revision test more than three times, and software is at Data processing, and acquiescence is removed signal intensity maximal value and minimum value automatically.All the other repeating datas are got its mean value and are used for the Criterion curve.The error that can avoid like this in detection individual data to occur due to operator's error.
That sample concentration is to the relation between signal intensity according to conventional quantitative test.After this method is got denary logarithm with the data of sample introduction quality and signal intensity, then do linear relationship chart.The automatic Criterion curve linear of software equation automatically imports system interface and can be used for the quantitative detection alarm pattern-recognition of terminal.
Semi-quantitative analysis method of the present invention independently is based upon in the ion mobility spectrometry analysis software, does not affect the qualitative analysis pattern.
This method is used for the quantitative alarm mode of software terminal.Under the experiment condition of optimum, method of the present invention can realize the quantitative alarm mode of two orders of magnitude of ion mobility spectrometry.For enriched sample, ion mobility spectrometry can be diluted to low concentration (in the range of linearity) and complete corresponding quantitative test.
The successful research and development of this detection method will instruct ion mobility spectrometry in the widespread use of analysis field, can carry out fast and accurately semi-quantitative analysis.
Advantage of the present invention is as follows:
1. compare with traditional gas chromatography, mass spectrometry method, ion mobility spectrometry has the following advantages: whole instrument total amount is less than 15kg, and is easy to carry, and instrument can independent operating, can on-the-spotly use; Measuring speed is fast, and per minute can be tested 6 samples; There is no complicated sample pre-treatments test, be highly suitable for line and detect use; The operating cost of instrument is very low, and consumables seldom; The cost performance of instrument is high, and analysis speed is faster more than 10 times than GC-MS etc.Semi-quantitative analysis method with the present invention of these advantages sets up will promote the widespread use of ion mobility spectrometry.
This measuring method easy, quick, be easy to revise.Can build the storehouse after typical curve generates and preserve follow-up use.
3. using based on reality needs, and the powerful data processing software of ion mobility spectrometry has been realized the sxemiquantitative relationship analysis between sample quality and signal intensity.The semi-quantitative analysis of sample that can the accurate instruction every field.
Description of drawings
Fig. 1 is input peak position library information surface chart;
Fig. 2 generates typical curve equation surface chart automatically;
Fig. 3 is input sample message surface chart;
Fig. 4 is analyzing and testing sample 1 test result surface chart;
Fig. 5 is analyzing and testing sample 2 test result surface charts;
Fig. 6 is analyzing and testing sample 3 test result surface charts;
Fig. 7 is analyzing and testing sample 4 test result surface charts;
Fig. 8 is analyzing and testing sample 5 test result surface charts;
Fig. 9 is for generating typical curve surface chart as a result;
Figure 10 is for preserving typical curve text surface chart;
Figure 11 is that the typical curve equation imports system interface figure automatically;
Figure 12 is the alarm software surface chart that user terminal uses.
Embodiment
According to the qualitative analysis, fill in the peak position library information in Fig. 1, the related qualitative analysis alarm mode of this option.
Accessibility Options in the click tools hurdle can show automatic generation typical curve equation surface chart shown in Figure 2.In Fig. 3, input sample ID, sample title and sample appearance time.Sample ID refers to generate in Fig. 2 the line number at linear equation place.Sample goes out the peak position will be determined according to qualitative analysis, such as the FK sample that provides in the present invention goes out the peak at 14.56ms.
Fig. 4-8 are the test ion mobility spectrometry figure (data are 4 repetitions) of the different sample sizes of FK sample (1ng, 5ng, 20ng, 40ng, 60ng).Trial test will be carried out between 0.5-80ng, determines that finally the quantitative scope of FK sample is between 1-60ng.The experiment condition of these spectrograms is: during experiment, the migration tube temperature remains on 100 ℃, 180 ℃ of injector temperature, and carrier gas, to float gas be air, air-flow is respectively 400mL/min, 600mL/min.
As Fig. 4-8 software interface, click " sampling ", can display background signal ion mobility spectrometry figure; Perhaps click " sampling ", insert blank sampling sheet, can detect the coupongs background signal.Click " taking out sample paper ", can take out coupongs.Click " system's cleaning " and open or close, can avoid sample introduction after system have sample residual.
Does background signal have interference after cleaning as the need detection system? need first remove " √ " symbol in the Option Box of " system's cleaning " button back, then click " sampling ", this Secondary Data System is given tacit consent to and is not preserved.Next step still need add " √ " the Symbol Option before continuing experiment.
In Fig. 9, we can see the typical curve surface chart of automatic generation.Right side interface display A, B coefficient and coefficient R.Click lower right corner derived data, enter Figure 10 interface, can preserve information by Update Table, can preserve like this graticule data of generation.After click is completed again, can enter Figure 11 interface.According to No. ID, can find the typical curve equation.Close this interface and can enter terminal interface, in the 1-60ng scope, sample is carried out quantitative alarm mode identification.
In the present invention, the explanation ion mobility spectrometry carries out qualitative analysis as an example of FK (fentanyl citrate arcotic) sample example, determines the sample appearance time.According to Fig. 1-3 interface requirement input relevant information.
During experiment, the migration tube temperature is 100 ℃, 180 ℃ of injector temperature, carrier gas (air) and float gas (air) air-flow and be respectively 400mL/min and 600mL/min.The coupongs that contain sample enter the ion mobility spectrometry detector and analyze after 50 ℃ of steamings of well heater desolventize.
Get respectively 0.5ppm, 1ppm, each 1 μ L of 5ppm with 1 μ L microsyringe, be 0.5ng, 1ng, 5ng; Get respectively 10ppm fentanyl citrate arcotic sample each 2 μ L, 4 μ L, 6 μ L, 8 μ L, i.e. 20ng, 40ng, 60ng, 80ng with 5 μ L microsyringes; At first test is carried out between 0.5-80ng, determines that finally FK sample semi-quantitative analysis scope is between 1-60ng.The coupongs that contain sample enter the ion mobility spectrometry detector and analyze after 50 ℃ of steamings of well heater desolventize.0.5ng and 80ng is not in the quantitative test range of linearity.
The test ion mobility spectrometry figure of the different sample sizes of FK sample (1ng, 5ng, 20ng, 40ng, 60ng) (data are 4 repetitions).What Fig. 9 provided is in the 1-60ng scope, the quantitative relationship curve of ion mobility spectrometry detector to the FK sample.The relational expression of match is y=1.3451+0.4044x.The quantitative effect of linear relation is more satisfactory, and linearly dependent coefficient has reached 0.99, and three groups of measurement data reappearances of same concentration replicate determination are better.
Figure 12 is terminal alarm software interface.The left side alarm lamp, red light show to be found testing sample, directly over toolbar show semi-quantitative analysis numerical value.
As shown in figure 12: 50ppm solution, sampling volume 1 μ L (being 50ng).Software alarm indication 53ng, this tests relative deviation less than 10%.
Therefore, be feasible to the quantitative measurement of FK sample in the above conditions.The sample of higher concentration, being diluted to can quantitative test between 1-60ng.
Claims (8)
1. qualitative, semi-quantitative analysis method that is used for the ion mobility spectrometry test sample is characterized in that:
1) in the quantitative concentrations scope, get different volumes, more than five, the sample of known variable concentrations enters respectively the ion mobility spectrometry sampling system and detects, the analysis software of ion mobility spectrometry detector is identified variable concentrations sample signal intensity automatically;
The same concentration sample repeats to get more than 3 times its mean value; The mean value of each sample concentration signal intensity and counter sample concentration numerical value are automatically got 10 and are end natural logarithm, as the coordinate figure of X-axis, Y-axis, generate typical curve respectively, and then match generates the typical curve equation;
2) sample to be analyzed is entered the ion mobility spectrometry sampling system and detect, the analysis software of ion mobility spectrometry detector is identified sample signal intensity automatically;
Corresponding signal peak signal intensity by the equation of match, calculates unknown concentration fentanyl citrate sample solution concentration; Quantitatively shown by software terminal.
2. method according to claim 1 is characterized in that: ion mobility spectrometry positive and negative ion pattern is qualitative, the semi-quantitative analysis method that propose of available the present invention all.
3. method according to claim 1, it is characterized in that: sample can enter detection system by different ion mobility spectrometry sampling systems; Sampling system comprises that high temperature pyrolysis analyses injector or gaseous sample automatic sampling system, is then that carrier gas is carried sample molecule and entered into the ion mobility spectrometry detection zone and analyze by air.
4. method according to claim 1, it is characterized in that: the same concentration sample will carry out revision test more than three times, and software is at Data processing, and acquiescence is removed signal intensity maximal value and minimum value; But all the other repeating datas are got its mean value and are used for the Criterion curve;
5. method according to claim 1 is characterized in that: after five variable concentrations samples repeated respectively claim 4 step, next step carries out data automatically processed and generates the typical curve schematic diagram, and provides simultaneously the typical curve equation coefficient;
Sample concentration is converted into the sample introduction quality and gets 10 for doing X-axis after end natural logarithm, and signal intensity is got 10 and done Y-axis for after end natural logarithm.
6. method according to claim 1 is characterized in that: the typical curve equation of automatically setting up, the automatic import system of software can be used for the identification of terminal half-quantitative detection alarm mode.
7. method according to claim 1, is characterized in that: will drip on coupongs, and after the coupongs dry out solvent, be sent to the ion mobility spectrometry detector and analyze, and obtain detection signal, and carry out the quantitative and semi-quantitative analysis;
The coupongs that contain sample steam by well heater and desolventize, heating-up temperature SOLUTION PROPERTIES is per sample selected, be typically chosen between 20-50 ℃, the coupongs that then will contain sample are sent to pyrolysis and analyse injector, carry sample molecule by air do carrier gas and are sent to the ion mobility spectrometry detector and analyze.
8. according to claim 1 or 7 described methods, it is characterized in that: example is fentanyl citrate arcotic, sufentanil arcotic, alfentanil arcotic or Remifentanil arcotic.
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| CN104007164A (en) * | 2014-05-29 | 2014-08-27 | 武汉矽感科技有限公司 | Use of ion mobility spectrometer for detecting gibberellins residues in crops and method for detecting gibberellins residues in crops |
| CN108732235A (en) * | 2018-08-14 | 2018-11-02 | 青岛农业大学 | The method that streptococcus lactis cellulose content in chicken is quickly detected based on ion mobility spectrometry |
| CN109030613A (en) * | 2018-08-13 | 2018-12-18 | 中国检验检疫科学研究院 | A kind of methods of 5 kinds of disabling local anesthetics in on-site quick screening cosmetics |
| CN110672708A (en) * | 2019-10-28 | 2020-01-10 | 大连工业大学 | Ethylene detection method based on ion mobility spectrometry technology |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104007164A (en) * | 2014-05-29 | 2014-08-27 | 武汉矽感科技有限公司 | Use of ion mobility spectrometer for detecting gibberellins residues in crops and method for detecting gibberellins residues in crops |
| CN109030613A (en) * | 2018-08-13 | 2018-12-18 | 中国检验检疫科学研究院 | A kind of methods of 5 kinds of disabling local anesthetics in on-site quick screening cosmetics |
| CN108732235A (en) * | 2018-08-14 | 2018-11-02 | 青岛农业大学 | The method that streptococcus lactis cellulose content in chicken is quickly detected based on ion mobility spectrometry |
| CN110672708A (en) * | 2019-10-28 | 2020-01-10 | 大连工业大学 | Ethylene detection method based on ion mobility spectrometry technology |
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Application publication date: 20130605 |