CN203551362U - Device for extracting substances in ionized condensed state samples - Google Patents
Device for extracting substances in ionized condensed state samples Download PDFInfo
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- CN203551362U CN203551362U CN201320700075.1U CN201320700075U CN203551362U CN 203551362 U CN203551362 U CN 203551362U CN 201320700075 U CN201320700075 U CN 201320700075U CN 203551362 U CN203551362 U CN 203551362U
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
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- JUPQTSLXMOCDHR-UHFFFAOYSA-N benzene-1,4-diol;bis(4-fluorophenyl)methanone Chemical compound OC1=CC=C(O)C=C1.C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 JUPQTSLXMOCDHR-UHFFFAOYSA-N 0.000 description 4
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- JDLKFOPOAOFWQN-VIFPVBQESA-N Allicin Natural products C=CCS[S@](=O)CC=C JDLKFOPOAOFWQN-VIFPVBQESA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- JDLKFOPOAOFWQN-UHFFFAOYSA-N allicin Chemical compound C=CCSS(=O)CC=C JDLKFOPOAOFWQN-UHFFFAOYSA-N 0.000 description 1
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Abstract
一种萃取电离凝聚态样品内部物质的装置，由初级带电粒子发生器、萃取液输送器、凝聚态样品承载器、凝聚态样品萃取液雾化器、各部分支撑体及其与质谱仪器的联接接口组合而成。通过萃取剂来萃取凝聚态样品，并将萃取液雾化成样品萃取物气溶胶，初级带电粒子发生器产生的带电试剂粒子进入到离子源空间，初级带电试剂粒子与样品萃取物气溶胶在离子源空间中发生碰撞，实现目标分析物分子的离子化，离子化的样品分子通过质谱仪入口进入质谱仪进行分析与检测。本实用新型特别适合在不需要样品粉碎、研磨、匀浆、分离等预处理手段的前提下直接获取固体、胶体、粉末、非均相液态混合物、植物组织、动物组织等凝聚态样品内部物质带电粒子。
A device for extracting the internal substances of ionized condensed matter samples, which consists of a primary charged particle generator, an extract liquid conveyor, a condensed matter sample carrier, a nebulizer for the condensed matter sample extract liquid, various parts of the support body and its connection with a mass spectrometer The interface is composed. The condensed sample is extracted by the extractant, and the extract is atomized into the sample extract aerosol, the charged reagent particles generated by the primary charged particle generator enter the ion source space, and the primary charged reagent particles and the sample extract aerosol are in the ion source Collisions occur in the space to realize the ionization of target analyte molecules, and the ionized sample molecules enter the mass spectrometer through the inlet of the mass spectrometer for analysis and detection. The utility model is particularly suitable for directly obtaining charged substances in condensed samples such as solids, colloids, powders, heterogeneous liquid mixtures, plant tissues, and animal tissues without the need for pretreatment methods such as sample crushing, grinding, homogenization, and separation. particle.
Description
Technical field
The utility model relates to a kind of device that extracts ionization condensed state sample interior material.
Background technology
The original position mass spectrophotometry of condensed state sample all has huge challenge in fields such as analytical chemistry, physical chemistry, biological chemistries, in sample, the interference of large amount of complex base matter all causes very large impact to the speed of existing analysis means, sensitivity, selectivity, even cannot meet the analysis requirement to target substance in complicated substrate.Emerging analytical technique of mass spectrum finds application and develops in natural science applied every field the analysis of complicated substrate nearly ten years, if mass spectrometry is to the detection of trace toxic chemical substance, have its unique advantage to the parsing of life macromolecule form and structure.Mass spectroscopy has that specificity is good, highly sensitive, quick, high flux, feature that consumption sample size is few, and therefore, the exploitation of mass-spectrometric technique and application are the important problems of of current Institute of Science research.
Mass spectrometer only produces response to charged particle, and the ion that neutral molecule is only transformed into certain electric charge could be detected by mass spectrometer.In mass-spectrometric technique exploitation and research, ion gun, as the core component of mass spectrophotometry, has played conclusive effect to the development of mass spectrophotometry.Can not destroy under the prerequisite of target analytes molecule, how the target molecule in complicated substrate sample is efficient, fast, high flux ground ionization, be a difficult problem urgently to be resolved hurrily.
Tradition mass spectrum ionization technique generally needs the sample pretreatment process of complicated and time consumption to the processing of complex sample, complicated substrate sample will pass through the pre-service such as pulverizing, grinding, homogenate, separation, extraction, purifying, and the target analytes purification of samples of the complicated substrate that is removed just can carry out mass spectrophotometry.These sample pretreatment processes loaded down with trivial details, consuming time do not meet undoubtedly now to requirement quick, online, method for high-flux analysis.In addition, the processing of extraction repeatedly and different chemical reagent, to target analysis deposits yields destroy and pollute, particularly destruction and the inactivation of some bioactive macromolecules in preprocessing process is all unavoidable.
Under the pretreated prerequisite without complex sample, the ionization technique of realizing the analysis of object in complicated substrate sample has had development fast, and researcher has been researched and developed a series of ionization source in this direction both at home and abroad.A series of atmospheric pressure ionization technology such as electron spray desorption ionization (DESI), normal pressure substance assistant laser desorpted ionized (APMALDI), electron spray extraction ionization (EESI), surface desorption atmospheric chemical ionization (DAPCI) have obtained abundant scientific payoffs to the direct express-analysis of complex sample.But above-mentioned cited ioning method has shortcoming separately, a deficiency the most significant is exactly, these ionization techniques can only be analyzed the surface of sample, under the prerequisite of not carrying out any sample pretreatment, to the inside of condensed state sample, cannot effectively analyze.Therefore, without complex sample is carried out under pretreated prerequisite, find a kind of soft ionization technology, particularly depend on simple experimental provision and just can realize the quick analytical technique of mass spectrum of complicated condensed state sample interior material is had important practical significance.
Summary of the invention
The purpose of this utility model is just to provide a kind of needs under the prerequisite of the preprocessing means such as sample pulverizing, grinding, homogenate, separation, the device that directly obtains the extraction ionization condensed state sample interior material of the condensed state sample interior material charged particles such as solid, colloid, powder, heterogeneous liquefied mixture, plant tissue, animal tissue, this device connects the quick mass spectrophotometry that can realize condensed state sample interior chemical substance with mass spectrometer.
The device of extraction ionization condensed state sample interior material of the present utility model, comprise that sample extract gasoloid produces passage and elementary charged reagent particle produces passage, sample extract gasoloid produces passage, primary charged particle produces passage and all becomes angle to install with mass spectrometer ion entrance, three is in the same plane, the angle that sample extract gasoloid produces passage and primary charged particle generation passage is 30-120 degree, on the axis of mass spectrometer ion entrance in two passages, itself and sample extract gasoloid produce access port, it is 5-15mm that primary charged particle produces access port horizontal range.
Sample extract gasoloid produces the formation of passage: extract conveyer is connected with condensed state sample carrier by input connecting pipe (quartz capillary or PEEK pipe), the other end of condensed state sample carrier is connected with condensed state sample extraction liquid atomization device by output connecting pipe, condensed state sample is placed in condensed state sample carrier, and condensed state sample extraction liquid atomization device is provided with carrier gas inlet.
Primary charged particle produces passage and consists of primary charged particle generator.
Described extract conveyer is syringe, any one of syringe pump, chromatogram pump etc. or multiple any composition; The mode of carrying liquid is to utilize chromatograph or syringe pump to control extract is injected into the sample interior in condensed state sample carrier with certain flow velocity.Extractant by sample, out obtains condensed state sample extraction liquid by condensed state sample interior extracting substances under fluid pressure.The composition of the extract in extract conveyer and polarity can be artificial selection and control, for condensed state sample of different nature, choose corresponding extract, thereby extract and separate obtains target chemical substances.Condensed state sample carrier also serves as sample extraction device simultaneously, the extract extraction that condensed state sample is injected in the tube chamber of condensed state sample carrier.Condensed state sample extraction liquid is accepted parts by pipeline and is transported in condensed state sample extraction liquid atomization device, and condensed state sample extraction liquid atomization device, by extract atomization, obtains sample extract gasoloid, and sample extract gasoloid enters into ion gun space.
Primary charged particle generator can be to consist of various simple charged particle generators, the form that produces charged particle can be electron spray, corona discharge, plasma etc., primary charged particle generator produces a large amount of elementary charged reagent particles, and enters into ion gun space.
Under the effect of air-flow, electric field, the sample extract gasoloid and the elementary charged reagent particle that enter into ion gun space bump, and elementary charged reagent particle makes electric charge on target analytes molecular band (ionization) by charge transfer to target analytes molecule.Charged target analytes molecule in ion gun space enters mass spectrometer by mass spectrometer entrance and carries out follow-up qualitative framework analysis and quantitative measurment under the booster action of electric field and air-flow.
The device of extraction of the present utility model ionization condensed state sample interior material, application is extensive, has broken through the technical bottleneck that current Ionization Techniques In Mass Spectrometry can only Analysis of Complex matrix condensed state sample surfaces, is deep into the inside chemical substance of analyzing condensed state sample; Extraction ionization condensed state sample interior material device is connected and carries out follow-up qualitative framework analysis and quantitative measurment with direct introducing mass spectrometer, the analysis of complicated substrate condensed state sample is had to high flux, high specificity, highly sensitive feature, can realize the direct express-analysis to complicated substrate condensed state sample, this device is that a kind of applicability is wide, apparatus structure is simple, Ionization Efficiency is high, the mass spectrophotometry ionization apparatus of low cost of manufacture.
Accompanying drawing explanation
Fig. 1 is structural representation of the present utility model;
Fig. 2 is usingd electron spray as primary charged particle generation passage figure;
Fig. 3 is usingd low temperature plasma as primary charged particle generation passage figure;
Fig. 4 is usingd microwave plasma as primary charged particle generation passage figure;
Fig. 5 is usingd dielectric barrier discharge as primary charged particle generation passage figure;
Fig. 6 is usingd corona discharge as primary charged particle generation passage figure;
Fig. 7 is the mass spectrum fingerprint chromatogram of garlic under positive ion mode.
Embodiment
As shown in Figure 1, a kind of device that extracts ionization condensed state sample interior material, comprises extract conveyer 1, input connecting pipe 2, enter airtight plug screw 3, condensed state sample carrier 4, condensed state sample 5, go out airtight plug screw 6, output connecting pipe 7, carrier gas inlet 8, condensed state sample extraction liquid atomization device 9, ion gun space 10, mass spectrometer ion ingress interface 11, electrochondria output connecting pipe 12, primary charged particle generator 13, high voltage interface 14, extract conveyer 1 is connected with condensed state sample carrier 4 by input connecting pipe 2, condensed state sample 5 is filled in the interior tube chamber of condensed state sample carrier 4, input connecting pipe 2 passes into airtight plug screw 3 and extend in the interior tube chamber of condensed state sample carrier 4 and be inserted into the inside of condensed state sample 5, output connecting tube 7 passes out airtight plug screw 6 and is connected with condensed state sample carrier 4, the other end of output connecting tube 7 is connected with condensed state sample extraction liquid atomization device 9, output connecting tube 7 directly imports to sample extraction liquid in condensed state sample extraction liquid atomization device 9, carrier gas is incorporated in condensed state sample extraction liquid atomization device 9 by carrier gas inlet 8, gas is assisted and is made the atomization of sample extraction liquid.
Condensed state sample extraction liquid atomization device 9, primary charged particle generator 13, mass spectrometer ion ingress interface 11 threes under the support of accepting parts with, three is in the same plane, condensed state sample extraction liquid atomization device 9 is 30-120 degree with the angle of primary charged particle generator 13, on the axis of mass spectrometer ion ingress interface 11 in both, itself and sample extract gasoloid produce access port, it is 5-15mm that primary charged particle produces access port horizontal range, dotted portion in the front formation ion gun space 10(extraction of mass spectrometer ion ingress interface 11 ionization condensed state sample interior material device schematic diagram, horizontal range is 5-15mm), the elementary charged reagent particle that the sample extract gasoloid that condensed state sample extraction liquid atomization device 9 produces and primary charged particle generator 13 produce enters into ion gun space 10 under the effect of electric field and air-flow.The sample extract gasoloid and the elementary charged reagent particle that enter into ion gun space 10 bump, and elementary charged reagent particle makes electric charge on target analytes molecular band (ionization) by charge transfer to target analytes molecule.Charged target analytes molecule in ion gun space enters mass spectrometer by mass spectrometer ingress interface 11 and carries out follow-up qualitative framework analysis and quantitative measurment.
The primary charged particle being comprised of electrochondria output connecting pipe 12, primary charged particle generator 13, high voltage interface 14 these three structures is produced to being described in detail of passage below.
It is electron spray generator that primary charged particle shown in Fig. 2 produces passage, and the structure that produces electron spray comprises: extractant ascending pipe 15, high voltage input interface 16, gas spray pipe 17.
It is low-temperature plasma generator that primary charged particle shown in Fig. 3 produces passage, and the structure that produces plasma comprises: ground-electrode 18, gas introduction tube 19, insulation tube 20, electrode 21, high-frequency alternating current input interface 22.
It is microwave excited plasma generator that primary charged particle shown in Fig. 4 produces passage, and the structure that produces plasma comprises: carrier gas ingress pipe 23, work gas ingress pipe 24, metal outer pipe 25, microwave interface 26.
It is that electric discharge is worked as in medium resistance that primary charged particle shown in Fig. 5 produces passage, and the structure that produces charged particle comprises: needlepoint electrode 27, carrier gas pipe 28, endless metal circle 29, alternating voltage input interface 30, ground wire 31.
It is corona discharge that primary charged particle shown in Fig. 6 produces passage, and the structure that produces charged particle comprises: insulating sleeve 33, high voltage input interface 32, discharge metal pin 34.
Embodiment 1:
The fresh garlic sample of take ionizes the device of condensed state sample interior material and the operation steps that the chemical substance in Garlic Tissue is analyzed in mass spectrometer coupling as example illustrates extraction:
1, utilize to support and accept parts (as iron stand, metal fixedly bung flange, quartz capillary, PEEK pipe etc.) and extraction is ionized to condensed state sample interior material device put up;
2, at extract conveyer 1(as syringe, syringe pump, chromatogram pump etc.) in add a certain amount of suitable extract, as cyclohexane, methyl alcohol, water, methanol-water mixed liquor etc., this experiment be take methyl alcohol as extract, it is 0.002-0.010 mL/min that flow velocity is set, and extract conveyer 1 is managed by input connecting pipe 2(PEEK) be connected with condensed state sample carrier 4.Garlic samples is filled in the tube chamber of condensed state sample carrier 4, and utilizes into airtight plug screw 3, goes out that airtight plug screw 6 will be inputted connecting pipe 2, output connecting pipe 7 pins clamping, like this garlic samples with regard to fixing seal in the tube chamber of condensed state sample carrier 4.With N
2as carrier gas, to control nebulizer gas pressure 0.6-1.0 Mpa and import in carrier gas inlet 8 by PEEK pipe, carrier gas enters into condensed state extract atomizer 9.Under carrier gas stream auxiliary, enter into the condensed state sample extraction liquid generation atomization of condensed state sample extraction liquid atomization device 9, form sample extract gasoloid and enter into ion gun space 10.
3, in this experiment, primary charged particle generator 13 is electron spray (structure as shown in Figure 2), and the electron spray carrier gas power of carrying is 0.5 Mpa, take methyl alcohol as primary electrical spraying reagent.Flow velocity with syringe pump with 0.002-0.010 mL/min is pushed into electron spray reagent in electron spray generator, at the high voltage of add+4.5kV of high voltage interface place, produces charged particle (drop) like this at the mouth of pipe place of gas spray pipe.Primary charged particle generator 13 produces a large amount of elementary charged reagent particles, and enters into ion gun space 10.
4, under the effect of air-flow, electric field, the sample extract gasoloid and the elementary charged reagent particle that enter into ion gun space 10 bump, and elementary charged reagent particle makes electric charge on target analytes molecular band (ionization) by charge transfer to target analytes molecule.Charged target analytes molecule in ion gun space 10 enters mass spectrometer (LTQ-MS) by mass spectrometer ion ingress interface 11 and carries out follow-up qualitative framework analysis and quantitative measurment under the booster action of electric field and air-flow.
5, mass spectrum condition: it is positive ion detecting pattern that LTQ-MS is set, 150 ℃ of ion transfer tube temperature, ionization voltage+5 kV, the mass scanning scope of mass spectrometer
m/z50-1000 Da, other mass spectrum parameters are by LTQ-MS system Automatic Optimal.
Under mass spectrum condition after optimization, garlic samples is carried out to direct mass spectrophotometry, obtain the fingerprint chromatogram (Fig. 7) of garlic samples.As shown in Figure 7, extraction ionization condensed state sample interior material device can extract the chemical composition in Garlic Tissue and ionization well, obtains the inner abundant molecular information of garlic samples, as
m/z180 Hes
m/z185 are respectively allicin and NH
4 +and N-a
+in conjunction with signal.
Embodiment 2:
Above experimental result is as primary charged particle, to produce passage with electron spray, introduces respectively below to using plasma, corona discharge and as primary charged particle, produce the practical operation of passage.With reference to embodiment mono-, build sample extract gasoloid and produce passage, according to different primary charged particle producing method (plasma, corona discharge), build multi-form primary charged particle passage.
As shown in Figure 3, using low temperature plasma as primary charged particle passage, the generation of low temperature plasma is mainly by alternating voltage (3 kVpp, 2.5 kHz, 1W), the gas of importing to be stimulated and to become charged gas molecule; As shown in Figure 4, using microwave excited plasma as primary charged particle passage, input certain microwave energy (microwave power is 10W) gas of importing is excited to ionization; As shown in Figure 5, using dielectric barrier discharge as primary charged particle passage, it is to rely on the high-frequency ac voltage being added in endless metal circle that energy is added on the gas molecule of importing that dielectric barrier discharge produces charged gas, makes electric charge on gas molecule band; As shown in Figure 6, using the form of corona discharge as primary charged particle passage, on discharge metal pin, add the DC voltage of 3-5 kV, under high-tension effect, there are electric discharge phenomena in the needle point of discharge metal pin, discharge metal pin contacts with the gaseous sample that sample extract gasoloid produces, sample molecule is ionized, be with electric charge.The charged reagent molecule being produced by primary charged particle passage, enters ion gun space and sample extract gasoloid bumps, and makes electric charge on sample extract molecular band, and enters into mass spectrometer and detect.
Claims (3)
1. one kind extracts the device that ionizes condensed state sample interior material, comprise that sample extract gasoloid produces passage and elementary charged reagent particle produces passage, it is characterized in that: sample extract gasoloid produces passage, primary charged particle produces passage and all becomes angle to install with mass spectrometer ion entrance, three is in the same plane, the angle that sample extract gasoloid produces passage and primary charged particle generation passage is 30-120 degree, on the axis of mass spectrometer ion entrance in two passages, itself and sample extract gasoloid produce access port, it is 5-15mm that primary charged particle produces access port horizontal range, sample extract gasoloid produces the formation of passage: extract conveyer (1) is connected with condensed state sample carrier (4) by input connecting pipe (2), the other end of condensed state sample carrier (4) is connected with condensed state sample extraction liquid atomization device (9) by output connecting pipe (7), condensed state sample (5) is placed in condensed state sample carrier (4), condensed state sample extraction liquid atomization device (9) is provided with carrier gas inlet (8), primary charged particle produces passage and consists of primary charged particle generator.
2. extraction according to claim 1 ionizes the device of condensed state sample interior material, it is characterized in that:
Input connecting pipe (2) passes into airtight plug screw (3) and extend in the interior tube chamber of condensed state sample carrier (4) and be inserted into the inside of condensed state sample (5), and output connecting tube (7) passes out airtight plug screw (6) and is connected with condensed state sample carrier (4).
3. the device of extraction ionization condensed state sample interior material according to claim 1, is characterized in that: described extract conveyer (1) is syringe, any one in syringe pump, chromatogram pump or multiple any composition.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103558076A (en) * | 2013-11-08 | 2014-02-05 | 东华理工大学 | Device for extracting inner substances of ionized condensed state sample |
| CN116930305A (en) * | 2023-08-31 | 2023-10-24 | 江西正谱奕和科技有限公司 | Method and system for detecting pesticide residues in honeysuckle formula particles |
-
2013
- 2013-11-08 CN CN201320700075.1U patent/CN203551362U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103558076A (en) * | 2013-11-08 | 2014-02-05 | 东华理工大学 | Device for extracting inner substances of ionized condensed state sample |
| CN116930305A (en) * | 2023-08-31 | 2023-10-24 | 江西正谱奕和科技有限公司 | Method and system for detecting pesticide residues in honeysuckle formula particles |
| CN116930305B (en) * | 2023-08-31 | 2023-12-19 | 江西正谱奕和科技有限公司 | Method and system for detecting pesticide residues in honeysuckle formula particles |
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