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CN106840834A - The enriching apparatus and enrichment method of micro substance in a kind of fluid sample - Google Patents

The enriching apparatus and enrichment method of micro substance in a kind of fluid sample Download PDF

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Publication number
CN106840834A
CN106840834A CN201611229144.XA CN201611229144A CN106840834A CN 106840834 A CN106840834 A CN 106840834A CN 201611229144 A CN201611229144 A CN 201611229144A CN 106840834 A CN106840834 A CN 106840834A
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CN
China
Prior art keywords
field electrode
capillary
fluid sample
micro substance
substrate
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Pending
Application number
CN201611229144.XA
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Chinese (zh)
Inventor
余泉
赵海琛
王晓浩
倪凯
钱翔
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Shenzhen Graduate School Tsinghua University
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Shenzhen Graduate School Tsinghua University
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Priority to CN201611229144.XA priority Critical patent/CN106840834A/en
Publication of CN106840834A publication Critical patent/CN106840834A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N2001/4038Concentrating samples electric methods, e.g. electromigration, electrophoresis, ionisation

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The enriching apparatus and enrichment method of micro substance in a kind of fluid sample, the enriching apparatus include syringe pump, high-field electrode, low-field electrode, capillary and substrate, the syringe pump connects the capillary, for conveying the fluid sample containing micro substance to the capillary, the high-field electrode is located at by the infusion path of the capillary, the low-field electrode is oppositely arranged with the outlet of the capillary, the substrate is placed in the electric field formed between the high-field electrode and the low-field electrode, the fluid sample conveyed in the capillary polarizes under electric field action, small charged drop is formed to depart from the outlet of the capillary and be pooled on the substrate with Sprayable, with the volatilization of charged drop solvent in transition process of spraying, the enrichment of the micro substance is produced on the substrate.The present invention can realize micro substance even compact enrichment in fluid sample.

Description

The enriching apparatus and enrichment method of micro substance in a kind of fluid sample
Technical field
The present invention relates to test and analyze technical field, especially in a kind of fluid sample micro substance enriching apparatus and richness Diversity method.
Background technology
In mass spectral analysis detection, some equipment are only limitted to be analyzed solid sample, for example, parse electron spray (DESI) etc..And the detection for being present in the micro substance in fluid sample just must be rich by the test substance in fluid sample Collection is on substrate, then the determinand that will be enriched with substrate is detected.
For the enrichment of micro substance in fluid sample, conventional mode typically has agent to extract, ion exchange, UF membrane, The modes such as supercritical extract, ionic adsorption, liquid film extraction.And it is higher for the mass spectral analysis of requirement in to(for) test substance, this A little modes are difficult being enriched in the micro determinand even compact in fluid sample on substrate, thus have impact on detection and analysis Effect.
The content of the invention
It is a primary object of the present invention to overcome the deficiencies in the prior art, there is provided the richness of micro substance in a kind of fluid sample Acquisition means and enrichment method, realize the enrichment of micro substance even compact on substrate in fluid sample.
To achieve the above object, the present invention uses following technical scheme:
The enriching apparatus of micro substance in a kind of fluid sample, including syringe pump, high-field electrode, low-field electrode, capillary And substrate, the syringe pump connects the capillary, for conveying the fluid sample containing micro substance, institute to the capillary High-field electrode is stated by the infusion path of the capillary, the low-field electrode is oppositely arranged with the outlet of the capillary, The substrate is placed in the electric field formed between the high-field electrode and the low-field electrode, the liquid conveyed in the capillary Sample polarizes under electric field action, forms small charged drop and departs from the outlet of the capillary and collected with Sprayable Onto the substrate, with the volatilization of charged drop solvent in transition process of spraying, produce on the substrate described The enrichment of micro substance.
Further:
The syringe pump drives the fluid sample containing micro substance and is transported to the capillary with hydraulic pressure or air pressure mode The outlet of pipe.
Preferably, the high-field electrode is enclosed within the capillary with barrel forms.
Preferably, the voltage difference position 3-5kV of the high-field electrode and the low-field electrode.
Preferably, the distance between the high-field electrode and described low-field electrode are in 1-5cm.
Preferably, the distance of low-field electrode described in the substrate distance is no more than 1cm.
Preferably, the substrate is porous adsorbing material.
Preferably, the porous adsorbing material is filter paper, Graphene or nano material.
The enrichment method of micro substance in a kind of fluid sample, is filled using the enrichment of micro substance in the fluid sample Put, wherein the syringe pump conveys the fluid sample containing micro substance to the capillary, the liquid conveyed in the capillary Body sample polarizes under the electric field action between the high-field electrode and the low-field electrode, forms small charged drop and takes off From the capillary outlet and be pooled on the substrate with Sprayable, as the charged drop is in spraying transition process The volatilization of middle solvent, produces the enrichment of the micro substance on the substrate.
Further:
Preferably, the high-field electrode is enclosed within the capillary with barrel forms.
Preferably, the voltage difference position 3-5kV of the high-field electrode and the low-field electrode.
Preferably, the distance between the high-field electrode and described low-field electrode are in 1-5cm.
Preferably, the distance of low-field electrode described in the substrate distance is no more than 1cm.
Beneficial effects of the present invention:
For the enrichment of micro substance in fluid sample, the present invention is proposed in a kind of fluid sample based on electron spray principle The enriching apparatus and enrichment method of micro substance, are provided for effective solution.Using electron spray principle by liquid Body sample is converted into by the spraying of charged drop, and charged drop understands because solvent volatilizees volume during migrating in atmosphere Reduce, be finally scattered in test substance of the fine droplet on substrate with higher concentration, test substance can be enriched with substrate. Because the atomized drop that electron spray is produced is extremely fine, and even compact, therefore it is easily achieved the uniform enrichment on substrate.And And by controlling spray time, it is possible to achieve it is that subsequent analysis are carried to the precise control of enriched fractions content and thickness on substrate The sample form of high-quality has been supplied, analytical effect has directly been improved.Inventor successfully realizes fluid sample using the enriching apparatus Middle micro substance on substrate even compact enrichment, and then treat detection material achieve ideal Detection results.
Present invention advantage compared with prior art has:
(1) present invention can realize the enrichment of micro determinand in fluid sample, expand the application model of parsing electron spray Enclose;
(2) present invention can realize the concentration effect of even compact, improve enrichment quality.
(3) present invention can carry out accurate control by controlling nebulisation time to the thickness of enriched fractions.
(4) enrichment mode simple structure of the present invention, implementation is versatile and flexible, is adapted to promote.
Brief description of the drawings
Fig. 1 is the enriching apparatus structural representation that the embodiment of the present invention is based on micro substance in the fluid sample of electron spray principle Figure.
Fig. 2 is that the electron spray enrichment process principle of the enriching apparatus of micro substance in embodiment of the present invention fluid sample is illustrated Figure.
Specific embodiment
Embodiments of the present invention are elaborated below.It is emphasized that what the description below was merely exemplary, Rather than in order to limit the scope of the present invention and its application.
Refering to Fig. 1 and Fig. 2, in one embodiment, the enriching apparatus of micro substance in a kind of fluid sample, based on EFI Mist principle, the enriching apparatus include syringe pump 1, and high-field electrode 2, low-field electrode 4, capillary 3 and substrate 5, the syringe pump 1 connect The capillary 3 is connect, for conveying the fluid sample containing micro substance to the capillary 3, the high-field electrode 2 is located at institute State by the infusion path of capillary 3, the low-field electrode 4 is oppositely arranged with the outlet of the capillary 3, the substrate 5 is placed in In the electric field formed between the high-field electrode 2 and the low-field electrode 4, the fluid sample 7 conveyed in the capillary 3 is in electricity Polarized under field action, form small charged drop 6 and depart from the outlet of the capillary 3 and be pooled to Sprayable described On substrate 5, with the volatilization of the solvent in transition process of spraying of the charged drop 6, produced on the substrate 5 described micro The enrichment of material.
Enriching apparatus of the invention realize the enrichment mode based on electron spray principle, and the substrate is placed in the height of electron spray In the electric field formed between two electrodes of low pressure, the charged drop that electron spray is produced can fly away and collect on substrate, with powered The quick volatilization of solvent in drop, substrate on residual sample composition, so as to produce the concentration effect of sample.Enriching apparatus profit With the enrichment mode based on electron spray principle, the composition in fluid sample can be enriched on substrate, concentration effect is uniformly caused It is close, and the content of enriched composition can be adjusted by controlling enrichment time.
Refering to Fig. 1 and Fig. 2, in a preferred embodiment, the syringe pump 1 is driven containing micro with hydraulic pressure or air pressure mode The fluid sample of material is simultaneously transported to the outlet of the capillary 3.Fluid sample utilizes syringe pump to the output that capillary 3 is exported The driving forces such as the voltage that 1 hydraulic pressure for producing or air pressure and electric field are produced.
Refering to Fig. 1, in a preferred embodiment, the high-field electrode 2 is enclosed within the capillary 3 with barrel forms.
In the especially preferred embodiments, the voltage difference position 3-5kV of the high-field electrode 2 and the low-field electrode 4, described The distance between high-field electrode 2 and described low-field electrode 4 in 1-5cm, the substrate 5 apart from the low-field electrode 4 distance not More than 1cm.Wherein low-field electrode 4 can be grounded.Configured using combinations thereof, be obtained in that optimal electron spray concentration effect. Wherein, substrate 5 apart from low-field electrode 4 apart from no more than 1cm, with reference to high-field electrode and the voltage difference and electrode spacing of low-field electrode From design, effectively optimize the concentration effect that removes molten time and micro substance of the drop in transition process.
In a preferred embodiment, the substrate 5 is porous adsorbing material.In some specific preferred embodiments, institute It can be the porous adsorbing materials such as filter paper, Graphene or nano material to state porous adsorbing material.
Refering to Fig. 1 and Fig. 2, in another embodiment, the enrichment method of micro substance in a kind of fluid sample, using preceding The enriching apparatus of micro substance in the fluid sample of any embodiment are stated, wherein the syringe pump 1 contains to the conveying of the capillary 3 There is the fluid sample of micro substance, the fluid sample 7 conveyed in the capillary 3 is in the high-field electrode 2 and the low tension Polarized under electric field action between pole 4, form small charged drop 6 and depart from the outlet of the capillary 3 and with shape of spraying Formula is pooled on the substrate 5, with the volatilization of the solvent in transition process of spraying of the charged drop 6, on the substrate 5 Produce the enrichment of the micro substance.
Enrichment method of the invention realizes the enrichment mode based on electron spray principle, and the substrate is placed in the height of electron spray In the electric field formed between two electrodes of low pressure, the charged drop that electron spray is produced can fly away and collect on substrate, with powered The quick volatilization of solvent in drop, substrate on residual sample composition, so as to produce the concentration effect of sample.Enrichment method profit With the enrichment mode based on electron spray principle, the composition in fluid sample can be enriched on substrate, concentration effect is uniformly caused It is close, and the content of enriched composition can be adjusted by controlling enrichment time.
Refering to Fig. 1, in a preferred embodiment, the high-field electrode 2 is enclosed within the capillary 3 with barrel forms.
In the especially preferred embodiments, the voltage difference position 3-5kV of the high-field electrode 2 and the low-field electrode 4, described The distance between high-field electrode 2 and described low-field electrode 4 in 1-5cm, the substrate 5 apart from the low-field electrode 4 distance not More than 1cm.
The feature and principle of the specific embodiment of the invention are further illustrated below in conjunction with accompanying drawing.
Fig. 1 is shown as the enriching apparatus of micro substance in a kind of fluid sample of the invention, the enrichment based on electron spray principle Mode, the device includes syringe pump 1, high-field electrode 2, capillary 3, low-field electrode 4, substrate 5;Substrate 5 is placed in the height of electron spray In the electric field formed between piezoelectricity pole 2 and low-field electrode 4;Syringe pump 1 slowly conveys fluid sample 7 to capillary 3;High-tension electricity Pole 2 is enclosed within capillary 3;The Way out of capillary 3 points to low-field electrode 4.
Fig. 2 is the principle schematic that electron spray enrichment process is carried out using the enriching apparatus shown in Fig. 1, wherein, liquid-like Product 7 can be polarized under electric field action, and electric charge can be moved along direction of an electric field, and charged liquid forms Thailand in the exit of capillary 3 Strangle cone.The charged liquid at taylor cone tip can break through the critical value of surface tension of liquid, from taylor cone tip with fine droplet Form departs from, and is migrated in the air along direction of an electric field, forms spray effect.Charged drop 6 can go molten volatilization in transition process, Volume reduces, and the concentration of the micro determinand of drop internal can also be improved therewith.Final charged drop 6 can collect on the substrate 5, real The enrichment of existing determinand.Electric charge can in atmosphere with can dissipate quickly, the testing sample of final enrichment can be in electroneutral.
Above content is to combine specific/preferred embodiment further description made for the present invention, it is impossible to recognized Fixed specific implementation of the invention is confined to these explanations.For general technical staff of the technical field of the invention, Without departing from the inventive concept of the premise, its implementation method that can also have been described to these makes some replacements or modification, And these are substituted or variant should all be considered as belonging to protection scope of the present invention.

Claims (10)

1. in a kind of fluid sample micro substance enriching apparatus, it is characterised in that including syringe pump, high-field electrode, low tension Pole, capillary and substrate, the syringe pump connect the capillary, for conveying the liquid containing micro substance to the capillary Body sample, the high-field electrode is located at by the infusion path of the capillary, the outlet of the low-field electrode and the capillary It is oppositely arranged, the substrate is placed in the electric field formed between the high-field electrode and the low-field electrode, in the capillary The fluid sample of conveying polarizes under electric field action, forms small charged drop and departs from the outlet of the capillary and to spray Mist form is pooled on the substrate, with the volatilization of charged drop solvent in transition process of spraying, in the substrate The enrichment of the upper generation micro substance.
2. in fluid sample as claimed in claim 1 micro substance enriching apparatus, it is characterised in that the syringe pump is with liquid Pressure or air pressure mode drive the fluid sample containing micro substance and are transported to the outlet of the capillary.
3. in fluid sample as claimed in claim 1 micro substance enriching apparatus, it is characterised in that the high-field electrode with Barrel forms are enclosed within the capillary.
4. in the fluid sample as described in any one of claims 1 to 3 micro substance enriching apparatus, it is characterised in that it is described The voltage difference position 3-5kV of high-field electrode and the low-field electrode, it is preferable that between the high-field electrode and the low-field electrode Distance is in 1-5cm.
5. in fluid sample as claimed in claim 4 micro substance enriching apparatus, it is characterised in that the substrate distance institute The distance for stating low-field electrode is no more than 1cm.
6. in the fluid sample as described in any one of claim 1 to 5 micro substance enriching apparatus, it is characterised in that it is described Substrate is porous adsorbing material.
7. in fluid sample as claimed in claim 6 micro substance enriching apparatus, it is characterised in that the porous adsorption material Expect to be filter paper, Graphene or nano material.
8. in a kind of fluid sample micro substance enrichment method, it is characterised in that using such as any one of claim 1 to 7 institute The enriching apparatus of micro substance in fluid sample are stated, wherein the syringe pump conveys the liquid containing micro substance to the capillary Body sample, under electric field action of the fluid sample conveyed in the capillary between the high-field electrode and the low-field electrode Polarize, form small charged drop and depart from the outlet of the capillary and be pooled on the substrate with Sprayable, with The volatilization of charged drop solvent in transition process of spraying, the enrichment of the micro substance is produced on the substrate.
9. in fluid sample as claimed in claim 8 micro substance enriching apparatus, it is characterised in that the high-field electrode with Barrel forms are enclosed within the capillary.
10. in the fluid sample as described in any one of claim 8 to 9 micro substance enriching apparatus, it is characterised in that it is described The voltage difference position 3-5kV of high-field electrode and the low-field electrode, it is preferable that between the high-field electrode and the low-field electrode Distance is in 1-5cm, it is highly preferred that the distance of low-field electrode described in the substrate distance is no more than 1cm.
CN201611229144.XA 2016-12-27 2016-12-27 The enriching apparatus and enrichment method of micro substance in a kind of fluid sample Pending CN106840834A (en)

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Application Number Priority Date Filing Date Title
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Publication number Priority date Publication date Assignee Title
CN109916914A (en) * 2019-04-10 2019-06-21 清华大学深圳研究生院 A kind of product defects detection method and device
CN111751354A (en) * 2020-07-07 2020-10-09 中节能天融科技有限公司 Electrospray sample injection device and sample injection method based on electric field adsorption

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109916914A (en) * 2019-04-10 2019-06-21 清华大学深圳研究生院 A kind of product defects detection method and device
CN109916914B (en) * 2019-04-10 2021-07-02 清华大学深圳研究生院 Product defect detection method and device
CN111751354A (en) * 2020-07-07 2020-10-09 中节能天融科技有限公司 Electrospray sample injection device and sample injection method based on electric field adsorption

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Application publication date: 20170613

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