WO2005056186A1 - A modular biochip assembly - Google Patents
A modular biochip assembly Download PDFInfo
- Publication number
- WO2005056186A1 WO2005056186A1 PCT/IE2003/000166 IE0300166W WO2005056186A1 WO 2005056186 A1 WO2005056186 A1 WO 2005056186A1 IE 0300166 W IE0300166 W IE 0300166W WO 2005056186 A1 WO2005056186 A1 WO 2005056186A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- assembly
- biochip
- module
- microchannel
- modules
- Prior art date
Links
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
- B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
- B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
- B01L3/502715—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by interfacing components, e.g. fluidic, electrical, optical or mechanical interfaces
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/56—Labware specially adapted for transferring fluids
- B01L3/563—Joints or fittings ; Separable fluid transfer means to transfer fluids between at least two containers, e.g. connectors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00801—Means to assemble
- B01J2219/0081—Plurality of modules
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L2200/00—Solutions for specific problems relating to chemical or physical laboratory apparatus
- B01L2200/02—Adapting objects or devices to another
- B01L2200/025—Align devices or objects to ensure defined positions relative to each other
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L2200/00—Solutions for specific problems relating to chemical or physical laboratory apparatus
- B01L2200/02—Adapting objects or devices to another
- B01L2200/026—Fluid interfacing between devices or objects, e.g. connectors, inlet details
- B01L2200/027—Fluid interfacing between devices or objects, e.g. connectors, inlet details for microfluidic devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L2200/00—Solutions for specific problems relating to chemical or physical laboratory apparatus
- B01L2200/10—Integrating sample preparation and analysis in single entity, e.g. lab-on-a-chip concept
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L2300/00—Additional constructional details
- B01L2300/08—Geometry, shape and general structure
- B01L2300/0887—Laminated structure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L2400/00—Moving or stopping fluids
- B01L2400/04—Moving fluids with specific forces or mechanical means
- B01L2400/0475—Moving fluids with specific forces or mechanical means specific mechanical means and fluid pressure
- B01L2400/0478—Moving fluids with specific forces or mechanical means specific mechanical means and fluid pressure pistons
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L2400/00—Moving or stopping fluids
- B01L2400/04—Moving fluids with specific forces or mechanical means
- B01L2400/0475—Moving fluids with specific forces or mechanical means specific mechanical means and fluid pressure
- B01L2400/0487—Moving fluids with specific forces or mechanical means specific mechanical means and fluid pressure fluid pressure, pneumatics
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N2035/00178—Special arrangements of analysers
- G01N2035/00326—Analysers with modular structure
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
- G01N2035/1027—General features of the devices
- G01N2035/1034—Transferring microquantities of liquid
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
- G01N35/1065—Multiple transfer devices
Definitions
- the present invention relates to a biochip assembly comprising a plurality of enclosed elongate microchannels, each microchannel having an inlet port adjacent one of its proximal and distal ends, and an outlet port adjacent its other end; a plurality of reservoir wells for use with the microchannels; an enclosed liquid delivery channel assembly having two or more combined inlet and outlet ports, at least one forming an inlet port and at least one other forming an outlet port; and an enclosed sample holder transfer assembly for connecting a port of one module to a port or reservoir well of another module and for connecting two reservoir wells together.
- microfluidics namely the science of handling minute volumes of liquid
- Microfluidic devices offer significant potential advantages over current use instrumentation, particularly in terms of savings in costs and, often more importantly, in both sample and reagent consumption.
- Microfluidics can be employed within the area of cell based assays in order to mimic the continuous flow regime of microcapillaries, as has been described in the above- referenced patent specifications.
- biochip is used to relate to a microfluidic device in which the sample of reagent liquid is transported along the device in order to perform an experiment.
- the device must have an appropriate network of microchannels.
- This definition fails under the assembly of paradigms called “Laboratory on a Chip”. This should be distinguished from a DNA or protein biochip. The latter are based on a completely different technology in which an assembly of DNA fragments or proteins are statically spotted on a substrate. They are described confusingly by the same word “biochip” (or DNA/protein biochip).
- biochips There are various problems at the present moment with biochips, principally arising from the fact that they are relatively complex devices designed by individuals for specific experiments, rather than being universal in use. They are thus essentially specific biochip assemblies, designed and manufactured for a specific requirement, rather than more universal use. Additionally, the robustness of biochip assemblies needs to be improved. Effectively, this means that the construction of the biochip assemblies needs to be simplified.
- biochip assemblies are not easy to integrate with the normal equipment available in laboratories. The user is too often restricted to purchasing an expensive controller for each kind of biochip developed by a particular individual or company. It is essential that such biochip assemblies be usable with a wide range of inter alia optical readers, MALDI mass spectrometers, DNA sequencers and other common laboratory equipment.
- a further problem with current biochip assemblies relates to the transfer of samples to and from the various parts of the biochip assembly.
- the biochip should be capable of operating with conventional manual and automated devices for sample transfer (usually called pipettors).
- a biochip assembly comprising: a plurality of enclosed elongate microchannels, each microchannel having an inlet port adjacent one of its proximal and distal ends; and an outlet port adjacent its other end; a plurality of reservoir wells for use with the microchannels; an enclosed liquid delivery channel assembly having two or more combined inlet and outlet ports, at least one forming an inlet port and at least one other forming an outlet port; and an enclosed sample holder transfer assembly for connecting a port of one part of the biochip assembly to a port or reservoir well of another part and for connecting two reservoir wells together, characterised in that the biochip assembly comprises: a main support frame; a plurality of separate and removable biochip modules, namely an input module forming the enclosed liquid delivery assembly, at least one reservoir well containing a module and a microchannel containing module and in which the enclosed sample holder transfer assembly comprises a pair of support plates; a plurality of rigid tubes mounted on each support plate for engagement with the modules and with transfer conduits for connecting
- the transfer conduits are of a flexible material.
- a reservoir containing module is arranged on either side of the microchannel containing module with the input module adjacent one of the reservoir containing modules. This allows for easy transfer of reagent and sample.
- releasable connection means are provided on the main support frame for securing each of the support plates in spaced-apart relationship with each of the input module and the microchannel containing module and with each rigid tube connecting in liquid sealing manner with the appropriate port.
- each port comprises a compressible seal for engagement with a rigid tube.
- the releasable connection means is adapted to engage the rigid tube with the compressible seal to form a liquid seal. This ensures adequate sealing against air ingress and liquid leaking.
- the cross-sectional area of the microchannel varies along its length.
- the microchannel containing module comprises: sheets of flat plastics material laminated together to form an upper layer having through holes for forming input ports and output ports; an intermediate layer having cut-out through slots forming microchannels; and a base layer.
- microchannel This is a particularly easy way of manufacturing a microchannel. It will also allow any shape of microchannel to be manufactured easily.
- the intermediate layer is of a photo-resist fluoro- polymer material, secured to the other layers by ultraviolet (UV) curing.
- UV ultraviolet
- the intermediate layer is of a photo-resist fluoro-polymer material secured to the top layer by ultraviolet (UV) curing and the bottom layer is a peel-off sheet of polyester film, secured to the intermediate layer by an adhesive.
- UV ultraviolet
- the bottom layer is subsequently peeled off and further experiments carried out. It also could allow the microchannel containing module to be cleaned and re-used.
- Fig. 1 is a diagrammatic layout of an assay assembly using a biochip assembly according to the invention
- Fig. 2 is a perspective view of a biochip assembly according to the invention, in one position of use
- Fig. 3 is a perspective view of a sample holder transfer assembly forming part of the biochip assembly
- Fig. 4 is a perspective view of biochip modules forming part of the biochip assembly of the invention
- Fig. 5 is a perspective view of more of the frame forming part of the invention.
- Fig. 6 is a plan view of the biochip modules of Fig. 4 and the portion of the frame illustrated in Fig. 5, assembled together,
- Fig. 7 is a perspective view of part of a main support frame forming part of the biochip assembly
- Fig. 8 is a sectional view along the lines VIII-VIII of Fig. 2,
- Fig. 9 is a sectional view along the lines IX-IX of Fig. 2,
- Fig. 10 is a perspective view of another microchannel containing module according to the invention.
- Fig. 11 is a plan view of the module of Fig. 10,
- Fig. 12 is a view, similar to Fig. 6, of portion of another biochip assembly according to the invention.
- Fig. 13 is another view, similar to Fig. 6, of portion of a still further biochip assembly according to the invention.
- Fig. 14 is a side view of a microchannel containing module according to the invention.
- Fig. 15 is a typical side sectional view of the microchannel containing module of Fig. 14,
- Fig. 16 is an exploded perspective view of the microchannel containing module of Figs. 14 and 15;
- Fig. 17 is a side view, similar to Fig. 15, of an alternative microchannel containing module according to the invention.
- a biochip assembly 1 within a typical assay assembly with most of the parts shown in outline.
- the assay assembly comprises typically, a liquid delivery unit 2, such as, for example, a nanopump, as described in some of our co-pending patent applications.
- the liquid delivery system 2 would generally be controlled by a controller 3 and computer 4.
- detection and recording equipment indicated generally by the reference numeral 5, which typically would comprise an optical inverted microscope 6, an epifluorescence device 7 and a digital camera 8, all of which are controlled by a suitable computer and recorder 9. All of this has been previously described in the above-referenced patent specifications and does not require any more description.
- the biochip assembly 1 comprises a main support frame 11 comprising a base frame 12 and an upper frame 13, mounting between them is a plurality of separate and removable biochip modules, namely, an input module 15, a pair of reservoir well containing modules 16 and a microchannel containing module
- a sample holder transfer assembly indicated generally by the reference numeral
- the reservoir well containing module 16(a) Since there are two reservoir well containing modules 16 in the embodiment described above, they are distinguished by the letters (a) and (b), the reservoir well containing module 16(a) being between the input module 15 and the microchannel containing module 17 and effectively forming input wells. Similarly, as described below, the reservoir well containing module 16(a) has three sets of wells 33, distinguished again by the letters (a), (b) and (c). Further, the wells 33 in the reservoir well containing modules 16(b) are identified by the reference letters (d), (e) and (f). Referring now to Fig. 3, the sample holder transfer assembly 18 comprises a pair of support plates 20, each plate having a cut-away shelf 21 and mounting a plurality of rigid tubes 22 which project above and below each support plate 20. The tubes 22 are connected by a plurality of flexible transfer conduits 23.
- Figs. 4 to 7 there is illustrated the input module 15, the reservoir containing modules 16(a) and 16(b) and the microchannel containing module 17, all of which will be described in more detail. They are generally mounted within the base frame 12, illustrated in Fig. 5, slotting into holes 25 of the base frame 12.
- the upper frame 13, illustrated in Fig. 7, retains the modules 15, 16(a), 16(b) and 17 tight against the base frame 12.
- the upper frame 13 mounts upstanding posts 30 having slots 31 for reception of the support plates 20 of the sample holder transfer assembly 18. It also mounts releasable connection means 42, again for mounting the sample holder transfer assembly 18, as described in more detail below.
- the input module 15 forms an enclosed liquid distribution system having an input port 30, enclosed distribution channels 31 and output ports 32.
- the reservoir containing modules 16 carries three sets of wells 33. As stated already, the reservoir containing modules 16 and their respective wells 33 are distinguished by the letters (a) and (b): and (a), (b), (c) and (d) (e), (f) respectively.
- the microchannel containing module 17 has a plurality of input ports 35 and output ports 36 connected by microchannels 37. In Fig. 6, they are shown as straight microchannels. The ports 30, 32, 35 and 36 are all exposed, as are the wells 33. However, the microchannels 37 and the channels 31 are enclosed. Their construction will be described in more detail later.
- releasable connection means 42 which comprises a support frame 45 mounting a pivot bar 46 on which is mounted a toggle lever 47 having an arcuate camming surface 48 for engagement with the upper frame 13 and having a slot 49 for reception of the shelf 21 of the support plate 20. It can be readily easily seen how the support plate 20 will be rigidly held on the mainframe 11 exerting a downward pressure.
- Fig. 9 Also illustrated in Fig. 9 are compressible inserts or seals 50 mounted in the output ports 32. Similar compressible seals 50 are provided in the other ports 35 and 36, although not in the input port 30 which will have any suitable construction for connection to the necessary liquid delivery system 2.
- the biochip assembly 1 For completeness, it is necessary to describe briefly how an assay is carried out with the biochip assembly 1 , such as, for example, for a cell adhesion study.
- Different ligands would be provided in each of two sets of the wells 33(a) and 33(b) of the reservoir containing module 16(a), namely the one closest to the input module 15.
- the ligands could, for example, be deposited there by pipetting or any suitable way.
- the number of transfer conduits 23 can be smaller than the microchannels in the microchannel containing module 17.
- the same sample containing suspension cells could be placed in one of the wells 33(a), (b) or (c) of the reservoir well containing module 16(a).
- both the ligands and the sample liquids are placed in different sets of wells 33(a), (b) or (c), of the same reservoir well containing modules 16(a).
- a cell adhesion test in its simplest, can be described, for example, somewhat as follows. Two sample holder transfer assemblies 18 would normally be used simultaneously.
- a syringe pump or other suitable pumping means is connected to the inlet port 30.
- the sample holder transfer assembly 18 is connected between one of the wells, for example, the wells 33(a), containing a ligand which will have been pipetted or placed in it by any suitable means, and the output port 32 of the input module15.
- S_tep_3 is connected between one of the wells, for example, the wells 33(a), containing a ligand which will have been pipetted or placed in it by any suitable means, and the output port 32 of the input module15.
- the ligand is aspirated into the sample holder transfer assembly 18.
- the sample holder transfer assembly 18 is disconnected from the wells 33(a) and is connected to the input port 35 of the microchannel containing module 17.
- Ligand is then delivered into each microchannel 37 to coat the interior thereof.
- microchannel containing module again identified by the reference numeral 17 and in which parts similar to those described, with reference to the previous drawings, are identified by the same reference numerals.
- the microchannels 37 are each arranged to be in a pattern such as can be seen, to increase the length of the microchannel. Other similar patterns may be used.
- FIG. 12 there is illustrated another arrangement in which the various modules are again identified by the same reference numerals.
- input module 15 well containing modules 16(a) and 16(b), and microchannel containing module 17.
- microchannel containing module 15 now contains a splitter for four, rather than eight, microchannels 37, as in the previous embodiment.
- Fig. 13 similarly illustrates again, the various modules, identified by the same reference numerals as before.
- this embodiment as well as having an elongate microchannel 37, there is an additional microchannel 37(a) connected to a microwell 50.
- This is illustrated to show how different microwells and different arrangements of microchannel containing modules 17 may be provided.
- Figs. 11 , 12 and 13 are simply illustrated to show that other arrangements of module are possible which will greatly increase the versatility of the biochip assembly 1.
- a biochip containing module again identified by the reference numeral 15, may be provided from three sheets of plastics material bonded together. Again, parts similar to those described, with reference to the previous drawings, are identified by the same reference numerals.
- This biochip containing module 15 comprises three sheets of flat plastics material laminated together to form an upper layer 60, an intermediate layer 61 and a base layer 62.
- the upper layer 60 has through holes 63 forming the input ports 35 and the output ports 36.
- the intermediate layer 61 has cut-out through slots 64 forming the microchannel 37. These are identified in Fig. 15. It will be appreciated that the upper layer 60 and the base layer 62 seal off the slots 64 to form the enclosed microchannels.
- the biochip modules is made of a mask of SU-8 photo-resist fluoro-polymer. This is used to form the intermediate layers 61 which is then sandwiched between the other two layers 60 and 62, followed by ultraviolet (UV) curing. Similar construction methods may be used to manufacture the input module 15 and the reservoir containing module 16.
- microchannel containing module again identified by the reference numeral 15, and comprising an upper layer 60 and an intermediate layer 61, all manufactured in exactly the same way as described with reference to the embodiment of Figs. 14 to 16 inclusive, and finally, a base layer 65 formed from a peel-off film of polyester film secured thereto by an adhesive.
- microchannel containing modules may be provided in various shapes and sizes to suit the particular type of test required.
- the assembly may simply be removed and disposed of after being used, to aspirate and deliver any one liquid, whether it be a reaction liquid, a cell-based liquid or a ligand. Needless to say, they can be relatively easily cleaned. Further, flushing out, using a system liquid, may also be achieved.
- the length of the microchannels have been greatly foreshortened.
- the microchannels can be lengthened by intertwining the microchannels, as shown, for example, in one embodiment. Indeed, any length of microchannel or indeed, any shape or cross-sectional shape of microchannel may be provided.
- biochip assembly can be easily integrated into other laboratory instruments.
- biochip can be easily fitted into a micro plate reader which adds significant advantages over currently existing systems.
- biochip assembly in accordance with the present invention, is the reduction in reagent or sample consumption. It will also facilitate reduced analysis time and larger transfer rates, due to the diminished distances involved. Further, it will be appreciated that the biochip assembly will facilitate the running of several assays in parallel.
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Clinical Laboratory Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Hematology (AREA)
- Apparatus Associated With Microorganisms And Enzymes (AREA)
- Automatic Analysis And Handling Materials Therefor (AREA)
Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
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AU2003292497A AU2003292497A1 (en) | 2003-12-10 | 2003-12-10 | A modular biochip assembly |
PCT/IE2003/000166 WO2005056186A1 (en) | 2003-12-10 | 2003-12-10 | A modular biochip assembly |
US10/582,295 US20080107565A1 (en) | 2003-12-10 | 2003-12-10 | Modular Biochip Assembly |
EP03768079.0A EP1691924B1 (en) | 2003-12-10 | 2003-12-10 | A modular biochip assembly |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
PCT/IE2003/000166 WO2005056186A1 (en) | 2003-12-10 | 2003-12-10 | A modular biochip assembly |
Publications (1)
Publication Number | Publication Date |
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WO2005056186A1 true WO2005056186A1 (en) | 2005-06-23 |
Family
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/IE2003/000166 WO2005056186A1 (en) | 2003-12-10 | 2003-12-10 | A modular biochip assembly |
Country Status (4)
Country | Link |
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US (1) | US20080107565A1 (en) |
EP (1) | EP1691924B1 (en) |
AU (1) | AU2003292497A1 (en) |
WO (1) | WO2005056186A1 (en) |
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WO2008063070A1 (en) * | 2006-11-23 | 2008-05-29 | Nederlandse Organisatie Voor Toegepast-Natuurwetenschappelijk Onderzoek Tno | Multiple microfluidic connector |
WO2008137008A2 (en) * | 2007-05-04 | 2008-11-13 | Claros Diagnostics, Inc. | Fluidic connectors and microfluidic systems |
DE102007054043A1 (en) * | 2007-11-13 | 2009-05-20 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Micro-analysis module has standard input and output interfaces for assembly of micro-analysis assembly in e.g. medical fluid tests |
WO2009117147A1 (en) * | 2008-03-20 | 2009-09-24 | Corning Incorporated | Modular microfluidic system and method for building a modular microfluidic system |
USD645971S1 (en) | 2010-05-11 | 2011-09-27 | Claros Diagnostics, Inc. | Sample cassette |
US8030057B2 (en) | 2004-01-26 | 2011-10-04 | President And Fellows Of Harvard College | Fluid delivery system and method |
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EP1691924A1 (en) | 2006-08-23 |
US20080107565A1 (en) | 2008-05-08 |
AU2003292497A1 (en) | 2005-06-29 |
EP1691924B1 (en) | 2016-09-14 |
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