CN101067621A - Production of micro-solid phase extraction chip based on micro-processing method and using method - Google Patents
Production of micro-solid phase extraction chip based on micro-processing method and using method Download PDFInfo
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- CN101067621A CN101067621A CN 200710041619 CN200710041619A CN101067621A CN 101067621 A CN101067621 A CN 101067621A CN 200710041619 CN200710041619 CN 200710041619 CN 200710041619 A CN200710041619 A CN 200710041619A CN 101067621 A CN101067621 A CN 101067621A
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Abstract
The invention relates to a miniature solid phase extract chip which is manufactured based on the micro processing method and its application method. The chip includes at least a cap rock and a pipeline level, the states pipeline level forms at least a section of solid phases extracts padding packing pipeline and a section through the micro processing filters pipeline, among, the solid phase extract padding packing pipeline through dam type structure or the stockade structure partially separates from the neighboring pipeline, but keeps the partial gas phases and the liquid phase connectivity with the neighboring pipeline, the filter pipeline partially is the pore structure which forms by the light initiation polymer; simultaneously at the back of the pipeline level corresponds the solid phase extract padding packing pipeline region process has the miniature heating electrode and the temperature induction electrode, which is used to heating control temperature. The invention may apply to the analytical chemistry and the biochemistry domain micro sample fast extract.
Description
Technical field
The present invention relates to a kind of micro-solid phase extraction chip and using method, relate to a kind of micro-solid phase extraction chip and using method of making based on micro-processing method or rather, described chip can be applicable to analytical chemistry and bioanalysis detection range.
Background technology
(Solid-Phase Extraction SPE) is one of present most popular sample pretreatment technology to Solid-Phase Extraction.It is to be based upon on traditional liquid-liquid extraction (LLE) basis, and interactional similar HPLC, the stationary phase ABC among the GC that mixes mechanism and widespread use at present of bound substances grows up gradually, is mainly used in separation, the purifying and concentrated of sample.(LLE) compares with liquid-liquid extraction, SPE have easy and simple to handle fast, advantage such as consumption of organic solvent is few, environmental pollution is little.The SPE technology is subjected to widespread use [Simpson in fields such as medicine, food, environmental protection, commodity inspection, cosmetics, agriculturals at present, N.J.K. " Solid-Phase Extraction Principles; Techniques and Applications, " MarcelDekker:New York; 2000].
Conventional SPE device is made of SPE pillar and auxiliary usually, often relate to numerous parts such as column jecket, sintering pad, filler, vacuum system, vacuum pump, blow-dry device, inertia source of the gas, high volume sampler and surge flask, be difficult to realize microminiaturized and integrated, and be not suitable for the processing of micro-example, thereby limited the robotization and the portability of The whole analytical process.The solid-phase microextraction that grow up the nineties in 20th century (Solid Phase Microextraction, SPME) though technology has had good improvement in the microminiaturization of device and the simplicity method of operation, but aspect integrated, still have bigger limitation, be difficult to the detection of bulk processing of front end sample and rear end integrated.
Adapt to the microminiaturization of present analysis instrument, integrated development trend, in recent years based on micro-total analysis system (the Micro Total Analysis Systems of micro-fluid chip platform, μ-TAS) emerge rapidly, and beginning is used at the biological and chemical analysis field.Solid-Phase Extraction research based on micro-fluid chip also has relevant report, 1998, [Figeys such as Figeys, D., Aebersold, R. " Nanoflow solvent gradientdelivery from a microfabricated device for protein identifications by electrosprayionization mass spectrometry, " Anal.Chem., 1998,70 (18): 3721-3727.] in chip external, fill post C
18The kapillary of silica gel has realized first that as the Solid-Phase Extraction microtrabeculae Solid-Phase Extraction combines with micro-fluid chip; Recently, [Oleschuk such as Oleschuk, R.D., Shultz-Lockyear, L.L., Ning, Y., Harrison, D.J. " Trapping of bead-based reagents within microfluidic systems:on-chip solid-phase extraction and electrochromatography; " Anal.Chem., 2000,72 (3): 585-590.] by micro-processing technology, in chip channel, be processed to form a microlaser cavity, fill filler, made the single micro-fluid chip of integrated Solid-Phase Extraction function.Compare with traditional SPE device, microfluid SPE chip has following advantage: (1) improves sample processing throughput; (2) significantly reduce the consumption of solvent and the generation of refuse; (3) recovery height, favorable reproducibility; (4) be easy to realize integrated and robotization.Though existing microfluid SPE chip has successfully been realized combining of solid phase extraction techniques and micro-fluid chip,, limit promoting the use of of this new technology aspect front and back end integrated, also doing inadequately.
Summary of the invention
The micro-solid phase extraction chip and the using method that the purpose of this invention is to provide functions such as a kind of integrated filtration, pyrolysis absorption, described micro-solid phase extraction chip is fill pipe and a heating microelectrode of processing filter pipe, solid phase extraction filler by micro-processing method on monolithic chip, improve the speed of Solid-Phase Extraction process and the integrated level of The whole analytical process, reduce the consumption of organic reagent.This chip is easy to integrated and realizes robotization, can be used for making up micro-full analytical system.
A kind of micro-solid phase extraction chip provided by the invention is characterized in that described chip comprises at least one cap rock and a pipe layers; Be processed with on the cap rock and the corresponding aperture in each little pond of pipe layers.Wherein pipe layers comprises fill pipe and one section filter pipe of at least one section solid phase extraction filler; Partly separate by dam type or fence structure and adjacent channel at solid phase extraction filler fill pipe two ends, and the restriction solid phase extraction filler is in the fill pipe zone, but keep the connectedness of this zone and adjacent channel part gas phase or liquid phase; Filler particles shape solid phase extraction filler in the fill pipe of solid phase extraction filler is used to carry out selective extraction; The microcellular structure that the filter pipe part is formed by the light initiation polymerization thing constitutes, and is used for filtered sample liquid particulate contamination or biomacromolecule impurity; The corresponding solid phase extraction filler fill pipe of die bottom surface zone is processed with miniature heating electrode and temperature sense electrode, can the material of fill pipe part be heated and temperature control, is used for the organic extraction composition of direct heat desorption volatility and half volatile.In addition, described pipe layers is characterised in that and comprises at least one activating reagent pond, a sample cell, a drip washing liquid pool, extraction stuffing filling pond, a waste liquid pool and a sample collection pond; Sample cell, activating reagent pond and drip washing liquid pool converge by three laterals and form extraction chip trunk line, and wherein connecting sample cell is filter pipe with the lateral that extracts the chip trunk line; Extraction stuffing is filled the pond and is linked to each other with solid phase extraction filler fill pipe on being positioned at extraction chip trunk line by a lateral, is used for filling solid phase extraction filler to fill pipe; Waste liquid pool links to each other with extraction chip trunk line rear end by two laterals with the sample collection pond.The back side of pipe layers is processed with miniature heating electrode and humidity inductive electrode corresponding to the solid phase extraction filler conduit region.
Particularly, when implementing sample extraction, at first fill and add the extraction stuffing that is the suspending liquid state in the pond 8 at extraction stuffing, by air pressure or electroosmotic flow type of drive extraction stuffing 12 is inserted in the solid phase extraction filler fill pipe 3, in activating reagent pond 5, sample cell 6 and drip washing liquid pool 7, add activator, sample liquid and leacheate respectively then, and implement Solid-Phase Extraction according to the order that activation, sample introduction, drip washing, wash-out are collected.Organic extraction composition for volatility or half volatile can save wash-out collection step, directly carry out pyrolysis absorption by the heating microelectrode 13 and 14 heating of temperature sense microelectrode at the back side, make it to break away from combining of solid phase extraction filler and enter checkout equipments such as rear end gas chromatography, analyze by interface with sample collection pond 10.For the extract of difficulty volatilization, can it be eluted from solid phase extraction filler by the wash-out operation, will collect composition then and import checkout equipments such as rear end liquid chromatography or electrophoretic separation, analyze.
The present invention compares with existing solid-phase extraction chip, and integrated on-line filtration and pyrolysis adsorption function have improved the integrated level of solid-phase extraction chip, have improved the feasibility of whole extraction process robotization.
Description of drawings
Fig. 1 is a solid-phase extraction chip structural representation of the present invention.
Fig. 2 is a solid-phase extraction chip pipe layers planar structure synoptic diagram of the present invention.
Fig. 3 is the partial enlarged drawing in Fig. 2 solid phase extraction filler fill pipe zone 3.
Fig. 4 is the back side, a chip corresponding solid phase extraction filler fill pipe zone microelectrode partial enlarged drawing.
Embodiment
Further specify substantive distinguishing features of the present invention and obvious improvement below in conjunction with accompanying drawing.
Fig. 1 is a solid-phase extraction chip structural representation of the present invention, and this chip comprises a cap rock 1 and a pipe layers 2.Wherein pipe layers is processed with as shown in Figure 2 microchannel and little pool structure by little manufacturing process, and cap rock is processed with and the corresponding aperture in each little pond of pipe layers.
Fig. 2 is a solid-phase extraction chip pipe layers planar structure synoptic diagram of the present invention, comprises at least one section solid phase extraction filler fill pipe 3, filter pipe 4 and a series of little pond: activating reagent pond 5, sample cell 6, drip washing liquid pool 7, extraction stuffing are filled pond 8, a waste liquid pool 9 and a sample collection pond 10.Wherein filter pipe 4 is made of the polyacrylamide with pore characteristics, and its making is by acrylamide that charges into the doping light trigger in pipeline and methylene diacrylamide mixed liquor, and pipeline local irradiation ultraviolet light generation polymerization is realized.The different needs of the big molecular impurity of liquid filtering biological, cell or dust granule per sample, the blending ratio of adjusting acrylamide and methylene diacrylamide is different, and the aperture of polyacrylamide can change between 5nm～1 μ m in the filter pipe 4.
Fig. 3 is Fig. 2 solid phase extraction filler fill pipe zone 3 partial enlarged drawings, separate with the pipeline other parts by dam type or fence structure 11 at solid phase extraction filler fill pipe two ends, restriction solid phase extraction filler 12 is in the fill pipe part, but keeps the connectedness of fill pipe part and adjacent channel part gas phase and liquid phase.
Fig. 4 is the back side, a chip corresponding solid phase extraction filler fill pipe zone microelectrode partial enlarged drawing, comprises miniature heating electrode 13 and temperature sense electrode 14, is used for filler fill pipe zone is heated, and carries out the direct heat desorption.
When implementing sample extraction, at first fill and add extraction stuffing suspending liquid in the pond 8 at extraction stuffing, apply draught head or voltage difference by filling between pond 8 and the waste liquid pool 9 at extraction stuffing, with air pressure driving or electroosmotic flow type of drive extraction stuffing 12 is inserted in the solid phase extraction filler fill pipe 3, because the particle diameter of extraction stuffing 12 is greater than the space of dam type or fence structure 11, extraction stuffing 12 will be limited in fill pipe 3 zones.In activating reagent pond 5, sample cell 6 and drip washing liquid pool 7, add activator, sample liquid and leacheate respectively then, and implement Solid-Phase Extraction: (A) between activating reagent pond 5 and waste liquid pool 9, apply draught head or voltage difference with the order that activation, sample introduction, drip washing, wash-out are collected, drive activator stream through solid phase extraction filler fill pipe zone 3, the activation filler; (B) between sample cell 6 and waste liquid pool 9, apply draught head or voltage difference, drive sample liquid flow, carry out selective binding through solid phase extraction filler fill pipe zone 3; (C) between drip washing liquid pool 7 and waste liquid pool 9, apply draught head or voltage difference, drive the leacheate solid phase extraction filler fill pipe zone 3 of flowing through, carry out drip washing, remove impurity.But the organic extraction composition for volatility or half volatile saves wash-out and collects step this moment, can directly carry out pyrolysis absorption by the heating microelectrode 13 and 14 heating of temperature sense microelectrode at the pipe layers back side this moment, make it to break away from combining of solid phase extraction filler and enter checkout equipments such as rear end gas chromatography, analyze by interface with sample collection pond 10.For the extract of difficulty volatilization, carry out wash-out and collect by apply draught head or voltage difference between drip washing liquid pool 7 and collecting pit 10 this moment, will collect composition then and import checkout equipments such as rear end liquid chromatography or electrophoretic separation, analyzes.
Claims (7)
1, a kind of micro-solid phase extraction chip of making based on micro-processing method is characterized in that:
1. described miniature solid phase chip is made of a cap rock (1) and a pipe layers (2), is processed with on the cap rock (1) and each little pond respective apertures of pipe layers (2);
2. described pipe layers is made of one section solid phase extraction filler fill pipe (3), filter pipe (4) and little pond; Described little pond comprises an activating reagent pond (5), a sample cell (6), a drip washing liquid pool (7), extraction stuffing filling pond (8), a waste liquid pool (9) and a sample collection pond (10), sample cell, activating reagent pond and drip washing liquid pool converge by three laterals and form extraction chip trunk line, and wherein connecting sample cell is filter pipe (4) with the lateral that extracts the chip trunk line; Extraction stuffing fill the pond by a lateral be positioned at the solid phase extraction filler fill pipe (3) that extracts on the chip trunk line and link to each other; Waste liquid pool links to each other with extraction chip trunk line rear end by two laterals with the sample collection pond.
2, by the described micro-solid phase extraction chip of claim 1, it is characterized in that the back side of described pipe layers (2), be processed with miniature heating electrode (13) and temperature sense electrode (14) corresponding to solid phase extraction filler fill pipe (3) zone.
3, by the described micro-solid phase extraction chip of claim 1, it is characterized in that the two ends of solid phase extraction filler fill pipe (3) are separated with adjacent channel by dam type or fence structure, but still keep and the gas phase of adjacent channel or the connectedness of liquid phase.
4, by the described micro-solid phase extraction chip of claim 1, it is characterized in that filter pipe (4) tool at pore characteristics, micropore size is between 5nm～1 μ m.
5, by the described micro-solid phase extraction chip of claim 4, the mixing ratio realization of the micropore size that it is characterized in that described filter pipe (4) by regulating in the mixed liquor of forming by third rare acid amides and methylene diacrylamide both.
6, use be is characterized in that by the method for each described micro-solid phase extraction chip among the claim 1-5:
(1) at first fills adding extraction stuffing suspending liquid in the pond (8) at extraction stuffing, apply draught head or voltage difference by filling between pond (8) and the waste liquid pool (9) at extraction stuffing, with air pressure driving or electroosmotic flow type of drive extraction stuffing (12) is inserted in the solid phase extraction filler fill pipe (3), because the particle diameter of extraction stuffing (12) is greater than the space of dam type or fence structure (11), extraction stuffing (12) will be limited in fill pipe (3) zone;
(2) in activating reagent pond (5), sample cell (6) and drip washing liquid pool (7), add activator, sample liquid and leacheate then respectively, and implement Solid-Phase Extraction with the order that activation, sample introduction, drip washing, wash-out are collected:
(a) between activating reagent pond (5) and waste liquid pool (9), apply draught head or voltage difference, drive activator stream, the activation filler through solid phase extraction filler fill pipe zone (3);
(b) between sample cell (6) and waste liquid pool (9), apply draught head or voltage difference, drive sample liquid flow, carry out selective binding through solid phase extraction filler fill pipe zone (3);
(c) between drip washing liquid pool (7) and waste liquid pool (9), apply draught head or voltage difference, drive the leacheate solid phase extraction filler fill pipe zone (3) of flowing through, carry out drip washing, remove impurity, enter road, back checkout equipment and analyze.
7, press the using method of the described micro-solid phase extraction chip of claim 6, it is characterized in that having wash-out to collect step for the organic extraction composition of volatility or half volatile, directly carry out pyrolysis absorption by the heating microelectrode (13) and temperature sense microelectrode (14) heating at the pipe layers back side, make it to break away from combining of solid phase extraction filler and enter checkout equipments such as rear end gas chromatography, analyze by interface with sample collection pond (10); For the extract of difficulty volatilization, carry out wash-out and collect by apply draught head or voltage difference between drip washing liquid pool (7) and collecting pit (10) this moment, will collect composition then and import checkout equipments such as rear end liquid chromatography or electrophoretic separation, analyzes.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101999078A (en) * | 2008-04-11 | 2011-03-30 | 柯尼卡美能达精密光学株式会社 | Microchip and method for manufacturing microchip |
| EP2950076A1 (en) | 2014-05-26 | 2015-12-02 | CSEM Centre Suisse d'Electronique et de Microtechnique SA - Recherche et Développement | Portable system for automated preparation of liquid and/or solid samples |
| CN106841377A (en) * | 2016-12-30 | 2017-06-13 | 上海华质生物技术有限公司 | Micro-fluidic multichannel on-line preconcentration MALDI TOF detection means and method |
| CN106841376A (en) * | 2016-12-30 | 2017-06-13 | 上海华质生物技术有限公司 | A kind of micro-fluidic on-line preconcentration MALDI TOF detection means and method |
| CN107036874A (en) * | 2017-05-25 | 2017-08-11 | 华东理工大学 | The encapsulation type enrichment and separation device detected for online solid phase spectra |
| CN107271254A (en) * | 2016-03-31 | 2017-10-20 | 瑞皮斯坎系统公司 | Substances of interest is detected using gas Chemical properties of solid phas |
| CN113945653A (en) * | 2021-09-27 | 2022-01-18 | 深圳职业技术学院 | Chip type living body solid phase micro-extraction device system and method for nano-drug pharmacokinetics precise analysis by using same |
| CN114308153A (en) * | 2021-12-17 | 2022-04-12 | 华南农业大学 | Solid-phase extraction micro-fluidic chip for detecting nafil substances and system for detecting nafil substances |
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| CN1763545A (en) * | 2005-09-22 | 2006-04-26 | 复旦大学 | Microfluidic solid-phase extraction chip for sample pre-processing and preparation method thereof |
| CN1740779A (en) * | 2005-09-22 | 2006-03-01 | 复旦大学 | Analyzing system and analysing method based on integrated micro-flow control chip |
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2007
- 2007-06-05 CN CN2007100416197A patent/CN101067621B/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101999078A (en) * | 2008-04-11 | 2011-03-30 | 柯尼卡美能达精密光学株式会社 | Microchip and method for manufacturing microchip |
| EP2950076A1 (en) | 2014-05-26 | 2015-12-02 | CSEM Centre Suisse d'Electronique et de Microtechnique SA - Recherche et Développement | Portable system for automated preparation of liquid and/or solid samples |
| CN107271254A (en) * | 2016-03-31 | 2017-10-20 | 瑞皮斯坎系统公司 | Substances of interest is detected using gas Chemical properties of solid phas |
| CN106841377A (en) * | 2016-12-30 | 2017-06-13 | 上海华质生物技术有限公司 | Micro-fluidic multichannel on-line preconcentration MALDI TOF detection means and method |
| CN106841376A (en) * | 2016-12-30 | 2017-06-13 | 上海华质生物技术有限公司 | A kind of micro-fluidic on-line preconcentration MALDI TOF detection means and method |
| CN107036874A (en) * | 2017-05-25 | 2017-08-11 | 华东理工大学 | The encapsulation type enrichment and separation device detected for online solid phase spectra |
| CN107036874B (en) * | 2017-05-25 | 2021-03-16 | 华东理工大学 | A encapsulation type enrichment separator for online solid-phase spectral detection |
| CN113945653A (en) * | 2021-09-27 | 2022-01-18 | 深圳职业技术学院 | Chip type living body solid phase micro-extraction device system and method for nano-drug pharmacokinetics precise analysis by using same |
| CN113945653B (en) * | 2021-09-27 | 2023-08-18 | 深圳职业技术学院 | Chip type living body solid phase microextraction device system and analysis method thereof |
| CN114308153A (en) * | 2021-12-17 | 2022-04-12 | 华南农业大学 | Solid-phase extraction micro-fluidic chip for detecting nafil substances and system for detecting nafil substances |
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