CN102297791A - Method for processing sampling slice specially used for ion mobility spectrometry - Google Patents
Method for processing sampling slice specially used for ion mobility spectrometry Download PDFInfo
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- CN102297791A CN102297791A CN2010102069465A CN201010206946A CN102297791A CN 102297791 A CN102297791 A CN 102297791A CN 2010102069465 A CN2010102069465 A CN 2010102069465A CN 201010206946 A CN201010206946 A CN 201010206946A CN 102297791 A CN102297791 A CN 102297791A
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Abstract
The invention discloses a method for processing a sampling slice specially used for an ion mobility spectrometry, the invention is characterized in that the sampling slice is immersed in a solution containing a chemical additive and then volatilized to obtain. The invention optimizes a simple and feasible pre-processing method of purified sampling slice; simultaneously, a chemical additive can be directly added on the clean sampling slice which optimizes the sampling background of ion mobility spectrometry, the chemical additive signal is not only capable of covering the original reagent quasi-molecular ions (RIP), but forming the detection signal peak of a new chemical additive, as well as enhancing the signal strength of the sample detection simultaneously, when the sampling slice is used for analyzing various samples, the chemical additive has a plurality of effects: (1) optimizing the detection sample peak of the ion mobility spectrometry; (2) raising the strength of the signal peak of sample detection so that the detection sensitivity can be raised; (3) combining the samples which has no response and can be directly analyzed in the ion mobility spectrometry such as melamine with the chemical additive on the sampling slice to form a novel product for acquiring a detection signal.
Description
Technical field
The present invention relates on the sampling thin slice of ion mobility spectrometry directly to add chemical addition agent optimizing the method that ion mobility spectrometry detects, specifically a kind of novelty, easy, unique method that chemical addition agent is added on the ion mobility spectrometry sampling thin slice.This method utilizes ion mobility spectrometry fast detecting instrument as detection means based on ion mobility spectrometry sampling and analytical technology.The data that experimental study provides are that important impetus is played in development and the application of chemical addition agent in the ion mobility spectrometry analyzing and testing.
Background technology
The analyzing and testing of ion mobility spectrometry is not only that the sample that detection signal is arranged is analyzed at present, adds chemical addition agent after deliberation in the check and analysis process, can optimize original detection signal peak on the one hand, improves detection sensitivity; Can follow the chemical addition agent combination that adds by adding chemical addition agent, make the material that in ion mobility spectrometry, does not have detection signal on the other hand, form new product, and in ion mobility spectrometry, obtain detection signal.In the addition manner of the chemical addition agent report at home and abroad, use often, add to the form of gas in the gas circuit of ion mobility spectrometry as acetone, amine and other organic volatile material of a class that equates.
It is braided material that the teflon high temperature cloth adopts high-quality import glass fibre, carry out plain weave, twill, satin weave or adopt other weave to be woven into high glass fiber cloth base material, again through the technology of uniqueness, fully flood repeatedly, apply high-quality Teflon resin, produce the multiple super wide high temperature resistant varnished cloth of all thickness.Teflon high temperature cloth principal feature: 1. dimensionally stable, the intensity height, lengthening coefficient is less than 5 ‰.2. temperature tolerance is good, continuous working temperature-70-300 ℃.3. skin-friction coefficient is little, good insulating.4. resistance to bond is good, is easy to clean the various oil stains that adhere to its surface, and stain or other attachment be good corrosion resistance 5., and anti-various strong acid and strong base corrosion are not burnt, and are ageing-resistant.6. different weaving manners have formed the different high temperature cloth of gas penetration potential, and sample is had absorption.
Niacinamide character: white crystalline powder.Odorless or odorless almost, bitter.Easily molten in water or ethanol, in glycerine, dissolve.Fusing point 128-131 ℃.PH value is 5.5～7.5.Soluble in water, ethanol and glycerine.Be used for the treatment of pellagra and for want of caused illness of niacinamide such as stomatitis, glossitis etc.Also be used as the intermediate of medicine.Can be by filtering by the styrene type strong basic ion exchange resin after nicotinic acid and the ammonia effect, the logical more saturated filtrate of ammonia and making.
Phthalic ester (Phthalic Acid Esters is called for short PAEs, the another name phthalate ester) is the important organic compound material of a class.Be generally water white oily liquids, be insoluble in water, be soluble in methyl alcohol, ethanol.Common have repefral (DMP), diethyl phthalate (DEP), n-butyl phthalate (DBP), di-n-octyl phthalate (DOP), diisooctyl phthalate (DEHP) and a butyl benzyl phthalate (BBP).PAEs increases the plasticity of product and the intensity of raising product mainly as the plastifier in polybag and the plastic products, also can be used as farm chemical carrier, the raw materials for production of pest repellant, cosmetics, fragrance product, lubricant and defoamer.In recent years, along with the use of commercial production and plastic products, phthalic ester constantly enters environment, is prevalent in the environmental samples such as soil, water body, biology, air and atmospheric falling dust thing.
Summary of the invention
The purpose of this invention is to provide a kind of disposal route that ion mobility spectrometry detects the special-purpose sampling of the ion mobility spectrometry thin slice of performance, this method novelty, easy, unique optimized.Test method is simple, feasible, all is improved for analyzing sample sensitivity of the same race and detection limit.
Add chemical addition agent, can optimize original detection signal peak on the one hand, improve detection sensitivity; Can make the material that in ion mobility spectrometry, does not have detection signal with the chemical addition agent combination that adds on the other hand, form new product, and in ion mobility spectrometry, obtain detection signal.But the method for adding chemical addition agent at present awaits to study new addition manner, to simplify instruments design and experimentation.The present invention utilizes ion mobility spectrometry fast detecting instrument as analysis means based on the ionic migration spectrometer technology, has optimized the method that a kind of thin slice of sampling purifies pre-treating method and directly add chemical addition agent on the sampling thin slice.
The purifying treatment method of sampling thin slice is: (1) at first will sample thin slice with the clean surperficial booty of cleanser, behind the ultrasonic 5-10min of cleanser water, wash down with clean clear water; (2) and then with organic solvent ultrasonic cleaning 5-10min, it is water insoluble but be dissolved in the chaff interference of organic phase to wash the surface off; (3) use pure water ultrasonic cleaning 5-10min at last, put on the clean glass surface ware with tweezers.In the process of the test, require to use glassware, avoid bringing unnecessary undesired signal.Such sampling thin slice is put into (100-180 ℃, 0.5-1.5h) dry for standby in the drying box.
Organic solvent in the pre-treatment of described sampling thin slice is meant methyl alcohol, ethanol, methylene chloride or the acetone of noiseless background detection signal in ion mobility spectrometry.
The sampling thin slice of above-mentioned processing can directly add chemical addition agent according to following method.With the ionic migration spectrometer is detecting instrument, and the chemical addition agent that the present invention mentioned is applicable to the detecting pattern of ion mobility spectrometry.Specify that the consumption of some chemical addition agent will be adjusted according to the character and the concentration of concrete test sample in the method.
Be specially: the disposal route of the special-purpose sampling of a kind of ion mobility spectrometry thin slice after the sampling thin slice soaked in containing the solution of chemical addition agent, volatilizes solvent and gets final product.
Described sampling thin slice is the high temperature resistant sampling cloth of teflon, sampling paper, metal sampling thin slice, poly-tetrafluoro sampling sheet or glass wool cloth.According to the difference of different ion mobility spectrometry detector injection port structures, the wafer processes of will sampling becomes difformity; The sampling lamina dimensions is processed into wide 1.5-2.5cm, long 10cm-5m; This sampling sheet thickness is mainly 0.08-0.9mm.
Described chemical addition agent is niacinamide, hartshorn salt, ammonium bicarbonate, n-butyl phthalate (DBP), repefral, diethyl phthalate, dipropyl phthalate, diamyl phthalate, dihexylphthalate, dibutyl phthalate (DHP), dioctyl phthalate, dinonyl phthalate or didecyl phthalate.
Described niacinamide, hartshorn salt or the ammonium bicarbonate concentration in solution is 10-20g/L; N-butyl phthalate (DBP), repefral, diethyl phthalate, dipropyl phthalate, diamyl phthalate, dihexylphthalate, dibutyl phthalate (DHP), dioctyl phthalate, dinonyl phthalate or the volume by volume concentration of didecyl phthalate in solution are 1 ‰-1%.Bake out temperature 70-105 ℃ of adopting of described solvent flashing process, time 0.5-1.5h, solvent do not volatilize can influence the ion mobility spectrometry detection signal; The solvent that described obtain solution adopted is water, methyl alcohol, dichloromethane ethanol or acetone.Described immersion process adopts sonicated.
Advantage of the present invention is as follows:
Compare with traditional interpolation chemical addition agent method, the method for directly adding chemical addition agent on the sampling thin slice has the following advantages: 1. reduced the step of single sample ion mobility spectrometry analyzing and testing, needn't test manual interpolation chemical addition agent one by one; Shortened the time that the on-the-spot on-line analysis of sample detects, the robotization of analytical approach has been played a role.2. original chemical addition agent is that heating makes it to become gas and enters detection system, and such additive losses is very fast, and need observe it constantly and use up the time.3. to adopt high-quality import glass fibre be braided material to the teflon high temperature cloth, and its special nature decision purifies that to get rid of pre-treatment step that signal disturbs simple and can large batch ofly handle simultaneously; 4. more consumables mainly are the required organic solvent methyl alcohol of pre-treatment, ethanol, methylene chloride or acetone in the disposal route; Dilution when 5. chemical addition agent uses reduces a large amount of damaging influences of using former medicine that environment is caused.6. chemical addition agent has been optimized the peak type, more helps sample and detects.
Description of drawings
Fig. 1 is for detecting the migration spectrogram of sampling cloth (not adding chemical addition agent) with ion mobility spectrometry;
Fig. 2 is the migration spectrogram that detects sampling cloth (niacinamide-containing additive) with ion mobility spectrometry;
Fig. 3 is the ion mobility spectrometry figure with ion mobility spectrometry test sample lidocaine, niacinamide-containing on the cloth of wherein sampling;
Fig. 4 is the ion mobility spectrometry figure with ion mobility spectrometry test sample cocaine, niacinamide-containing on the cloth of wherein sampling;
Fig. 5 is the ion mobility spectrometry figure with ion mobility spectrometry test sample ephedrine, niacinamide-containing on the cloth of wherein sampling.
Fig. 6 contains n-butyl phthalate (DBP) for the ion mobility spectrometry figure with ion mobility spectrometry test sample melamine on the cloth of wherein sampling.
Embodiment
Described ionic migration spectrometer: with the ionization source is radioactivity
63The Ni source, ultraviolet light ionization source and discharge ionization source.Described ionic migration spectrometer mainly comprises sampling device, ionization source, reaction zone, ion gate, migration area, signal reception and detection system and gas circuit drying system.Sampling device mainly comprises hot parser, high temperature sampling cloth and carrier gas transfer pipeline.Wherein hot parser mainly is made up of injection port, heating rod or heating tape, temperature controller, and the sampling thin slice is teflon high temperature cloth, sheet metal, poly-tetrafluoro thin slice, and the carrier gas transfer pipeline is made up of four fluorine tube or metal tube and flowmeter.
Fig. 1-6 has provided some experiment spectrograms the present invention has been given and explanation.The experiment condition of these spectrograms is: the migration tube temperature remains on 100 ℃ during experiment, and the injector temperature remains on 180 ℃.
Embodiment 1
In order on the sampling thin slice, directly to add chemical addition agent to optimize the ion mobility spectrometry detection signal, the sampling thin slice requires to carry out simple purified treatment, the present invention, is used for sample analysis with the sampling thin slice that adds chemical addition agent then and detects as analysis means with ion mobility spectrometry.
Sampling cloth purified treatment is simple, feasible in this method, and its process is: (1) at first will sample thin slice with the clean surperficial booty of cleanser, behind the ultrasonic 5-10min of cleanser water, wash down with clean clear water; (2) and then with methyl alcohol or ethanol ultrasonic cleaning 5-10min, it is water insoluble but be dissolved in the chaff interference of organic phase to wash the surface off; (3) use pure water ultrasonic cleaning 5-10min at last, put on the clean glass surface ware with tweezers.Such sampling thin slice, it is promptly available to be put in the baking oven (100-180 ℃, 0.5-1.5h) oven dry.
Accurately take by weighing the 10g niacinamide and be dissolved in the 500mL pure water, the 5 meters long ultrasonic 10min of sampling cloth takes out back 100-105 ℃ of oven dry (about 0.5-1 hour) in baking oven and gets final product.Twine into a volume, the outside In Aluminium Foil Packing is standby.Little of cloth of sampling is proportionally approximately converted the proportioning of solvent, can handle equally.When using it for the ion mobility spectrometry detection, the niacinamide signal peak is covered reagent ion peak (RIP), and does not influence the detection of other samples simultaneously.
Fig. 1 has provided the migration spectrogram of a positive ion mode ion mobility spectrometry detectable quasi-molecular ions (RIP), and as can be seen from the figure, the reagent ion peak (RIP) of this instrument appears at about 6.8ms.Under the positive ion mode in the testing process RIP back usually follow the analysis of little signal peak Interference Detection sample.
Fig. 2 has provided the sampling thin slice ion mobility spectrometry figure of ion mobility spectrometry detection niacinamide-containing adjuvant, and the niacinamide consumption of test method appointment can be covered RIP and occur, and the characteristic peak of niacinamide appears at 8.6ms.
Above-mentioned two figure are to direct interpolation niacinamide adjuvant on the sampling thin slice as directed, both can enhancing signal intensity, can beautify background signal again, and the analysis that helps sample detects.
Utilize the process of ionic migration spectrometer test sample as follows: 1. lidocaine is a kind of medicament spraying agent, finishes sample collecting by the homemade air-extractor in laboratory.When the lidocaine spray was sprayed onto in the air, the air-extractor band the sampling cloth of niacinamide-containing adjuvant and is collected sample 10-30S.The cloth of sampling then inserts the ion mobility spectrometry injection port, and 180 ℃ of pyrolysis are analysed the sample gas that obtains and brought into the ionized region of ion mobility spectrometry by carrier gas, and the flow of carrier gas is about 300sccm; Sample is ionized to positive and negative ion at ionized region, and the ion gate by periodically opening enters the drift region that is made of uniform electric field, obtains in the drift region separating and detects.The mobility constant of different compounds is variant, the speed difference that moves in the drift region, and they arrive the asynchronism(-nization) of detecting device.Measure time and peak intensity that ion arrives detector, just can confirm classes of compounds.2. cocaine and the ephedrine methanol solution of getting 10 μ L, 50ppm respectively are added drop-wise on the sampling thin slice that contains adjuvant, volatilize methyl alcohol and insert the ion mobility spectrometry injection port then, and all the other processes are with above-mentioned step.
What Fig. 3 provided is the migration spectrogram that detects lidocaine with the ion mobility spectrometry detector.As shown in Figure 3, the characteristic peak of lidocaine (a) is represented the different niacinamide adjuvants constantly of continuous acquisition and the unlike signal intensity of lidocaine characteristic peak respectively with (b) about 11.4ms.
What Fig. 4 provided is the migration spectrogram that detects cocaine with the ion mobility spectrometry detector.As shown in Figure 4, the characteristic peak of cocaine is about 12.9ms.
What Fig. 5 provided is the migration spectrogram that detects ephedrine with the ion mobility spectrometry detector.As shown in Figure 5, the characteristic peak of ephedrine is about 9.2ms.
Embodiment 2
Difference from Example 1 is: accurately measure n-butyl phthalate (DBP) 1mL, be dissolved in the 100mL methyl alcohol.The sampling thin slice is put into wherein ultrasonic 10min, is that available In Aluminium Foil Packing is standby at 70-80 ℃ of oven dry methyl alcohol then.Add the sampling thin slice of chemical addition agent like this, can be directly used in the sample analysis of melamine.
Fig. 6 has provided the ion mobility spectrometry figure with ion mobility spectrometry test sample melamine.The direct test sample melamine of ion mobility spectrometry no signal under experiment condition.(a) figure has provided the signal peak that adds the DBP adjuvant on the sampling thin slice, and its characteristic peak is about 15.6ms, and (b) figure has provided and added the DBP adjuvant on the sampling thin slice, thereby induces the melamine peak, and its appearance time is about 18.7ms.
Claims (10)
1. the disposal route of the special-purpose sampling of an ion mobility spectrometry thin slice is characterized in that: after the thin slice of will sampling soaks in containing the solution of chemical addition agent, volatilize solvent and get final product.
2. method according to claim 1 is characterized in that: described sampling thin slice is the high temperature resistant sampling cloth of teflon, sampling paper, metal sampling thin slice, poly-tetrafluoro sampling sheet or glass wool cloth.
3. method according to claim 2 is characterized in that: according to the difference of different ion mobility spectrometry detector injection port structures, the wafer processes of will sampling becomes difformity; The sampling lamina dimensions is processed into wide 1.5-2.5cm, long 10cm-5m; This sampling sheet thickness is mainly 0.08-0.9mm.
4. method according to claim 1 is characterized in that: described chemical addition agent is niacinamide, hartshorn salt, ammonium bicarbonate, n-butyl phthalate (DBP), repefral, diethyl phthalate, dipropyl phthalate, diamyl phthalate, dihexylphthalate, dibutyl phthalate (DHP), dioctyl phthalate, dinonyl phthalate or didecyl phthalate.
5. method according to claim 4 is characterized in that: described niacinamide, hartshorn salt or the ammonium bicarbonate concentration in solution is 10-20g/L; N-butyl phthalate (DBP), repefral, diethyl phthalate, dipropyl phthalate, diamyl phthalate, dihexylphthalate, dibutyl phthalate (DHP), dioctyl phthalate, dinonyl phthalate or the volume by volume concentration of didecyl phthalate in solution are 1 ‰-1%.
6. method according to claim 1 is characterized in that: bake out temperature 70-105 ℃ of adopting of described solvent flashing process, and time 0.5-1.5h does to guarantee solvent evaporates, and solvent does not volatilize can influence the ion mobility spectrometry detection signal.
7. method according to claim 1 is characterized in that: the solvent that described obtain solution adopted is water, methyl alcohol, ethanol, methylene chloride or acetone.
8. method according to claim 1 is characterized in that: described immersion process adopts sonicated.
9. method according to claim 1, it is characterized in that: described sampling thin slice needed pre-treatment before soaking, concrete grammar is: (1) at first will sample thin slice with the clean surperficial booty of cleanser, behind the ultrasonic 5-10min of cleanser water, wash down cleanser water with clean clear water; (2) and then with organic solvent ultrasonic cleaning 5-10min, it is water insoluble but be dissolved in the chaff interference of organic phase to wash the surface off; (3) use pure water ultrasonic cleaning 5-10min at last, put on the clean glass surface ware with tweezers; In the process of the test, require to use glassware, avoid bringing unnecessary undesired signal; Such sampling thin slice is put in the baking oven, and afterwards In Aluminium Foil Packing is standby for 100-180 ℃ of oven dry, cooling.
10. method according to claim 8 is characterized in that: the organic solvent in the pre-treatment of described sampling thin slice is meant methyl alcohol, ethanol, methylene chloride or the acetone of noiseless background detection signal in ion mobility spectrometry.
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Cited By (8)
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| CN102866044A (en) * | 2012-09-12 | 2013-01-09 | 奥瑞金包装股份有限公司 | Board-type material ion migration detection pretreatment device and method |
| CN103884771A (en) * | 2012-12-21 | 2014-06-25 | 中国科学院大连化学物理研究所 | Accurate method for detecting propofol anesthetic in blood |
| CN104297013A (en) * | 2014-10-22 | 2015-01-21 | 公安部第一研究所 | Purification treatment method of ionic migration spectrum sampling strip |
| WO2015014294A1 (en) * | 2013-08-01 | 2015-02-05 | 同方威视技术股份有限公司 | Method used for rapid testing of highly volatile substances of very high concern in textiles |
| CN106198703A (en) * | 2015-05-06 | 2016-12-07 | 中国科学院大连化学物理研究所 | A kind of sampling paper pre-treating method for ion mobility spectrometry |
| CN106950072A (en) * | 2017-02-27 | 2017-07-14 | 深圳中物安防科技有限公司 | A kind of special sampling paper of drugs and preparation method thereof |
| CN109632437A (en) * | 2018-12-14 | 2019-04-16 | 北京化工大学 | A kind of sample-pretreating method of the on-site test based on ion mobility spectrometry |
| CN110646501A (en) * | 2019-10-31 | 2020-01-03 | 大连大学 | Method for detecting environmental hormone dimethyl phthalate |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102866044A (en) * | 2012-09-12 | 2013-01-09 | 奥瑞金包装股份有限公司 | Board-type material ion migration detection pretreatment device and method |
| CN102866044B (en) * | 2012-09-12 | 2015-04-29 | 奥瑞金包装股份有限公司 | Board-type material ion migration detection pretreatment device and method |
| CN103884771A (en) * | 2012-12-21 | 2014-06-25 | 中国科学院大连化学物理研究所 | Accurate method for detecting propofol anesthetic in blood |
| WO2015014294A1 (en) * | 2013-08-01 | 2015-02-05 | 同方威视技术股份有限公司 | Method used for rapid testing of highly volatile substances of very high concern in textiles |
| CN104297013A (en) * | 2014-10-22 | 2015-01-21 | 公安部第一研究所 | Purification treatment method of ionic migration spectrum sampling strip |
| CN106198703A (en) * | 2015-05-06 | 2016-12-07 | 中国科学院大连化学物理研究所 | A kind of sampling paper pre-treating method for ion mobility spectrometry |
| CN106950072A (en) * | 2017-02-27 | 2017-07-14 | 深圳中物安防科技有限公司 | A kind of special sampling paper of drugs and preparation method thereof |
| CN109632437A (en) * | 2018-12-14 | 2019-04-16 | 北京化工大学 | A kind of sample-pretreating method of the on-site test based on ion mobility spectrometry |
| CN109632437B (en) * | 2018-12-14 | 2020-07-24 | 北京化工大学 | Sample pretreatment method based on-site detection of ion mobility spectrometry |
| CN110646501A (en) * | 2019-10-31 | 2020-01-03 | 大连大学 | Method for detecting environmental hormone dimethyl phthalate |
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Application publication date: 20111228 |