EP3615218A1 - Plaque d'analyse maldi-tof a support papier et son utilisation - Google Patents
Plaque d'analyse maldi-tof a support papier et son utilisationInfo
- Publication number
- EP3615218A1 EP3615218A1 EP18723575.9A EP18723575A EP3615218A1 EP 3615218 A1 EP3615218 A1 EP 3615218A1 EP 18723575 A EP18723575 A EP 18723575A EP 3615218 A1 EP3615218 A1 EP 3615218A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- analysis
- sheet
- paper material
- analysis plate
- plate according
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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
- B01L3/502707—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 the manufacture of the container or its components
-
- 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
- B01L3/508—Containers for the purpose of retaining a material to be analysed, e.g. test tubes rigid containers not provided for above
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L9/00—Supporting devices; Holding devices
- B01L9/50—Clamping means, tongs
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0409—Sample holders or containers
- H01J49/0418—Sample holders or containers for laser desorption, e.g. matrix-assisted laser desorption/ionisation [MALDI] plates or surface enhanced laser desorption/ionisation [SELDI] plates
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/26—Mass spectrometers or separator tubes
- H01J49/34—Dynamic spectrometers
- H01J49/40—Time-of-flight spectrometers
-
- 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
- B01L2300/06—Auxiliary integrated devices, integrated components
-
- 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
- B01L2300/0809—Geometry, shape and general structure rectangular shaped
-
- 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
- B01L2300/0809—Geometry, shape and general structure rectangular shaped
- B01L2300/0816—Cards, e.g. flat sample carriers usually with flow in two horizontal directions
-
- 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
- B01L2300/12—Specific details about materials
- B01L2300/126—Paper
-
- 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
- B01L2300/16—Surface properties and coatings
- B01L2300/161—Control and use of surface tension forces, e.g. hydrophobic, hydrophilic
Definitions
- the present invention relates to the field of microbiology. More specifically, the invention relates to the analysis of a biological sample using mass spectrometry, and in particular, matrix-assisted desorption-ionization mass spectrometry and MALDI-TOF time of flight measurement.
- the MALDI-TOF technique has been used for a few years to carry out a rapid identification of micro-organisms, at the level of the species.
- the identification of a microorganism is made from the MALDI-TOF mass spectrum of the most abundant proteins in the microorganism, compared with baseline data allowing (identification of family, gender and most often of the microorganism species).
- the protocol implemented includes the deposition of at least a portion of the colony of the microorganism on a MALDI plate, the addition of a matrix adapted to the MALDI technique, the acquisition of the mass spectrum and the identification of the species by comparison with reference data stored in a database.
- the MALDI technique has also been used to detect the resistance of a microorganism to an antibiotic, and in particular to identify a phenotype responsible for the hydrolysis of beta-lactam antibiotics, because of the secretion of beta-lactamase type enzymes, and in particular of the carbapenemase type.
- the population of microorganism (s) placed within the MALDI matrix is subjected to gentle ionization by laser.
- the laser beam used for the ionization may have any type of wavelength favorable to sublimation or vaporization of the matrix.
- an ultraviolet or even infrared wavelength will be used.
- This ionization may, for example, be carried out with a nitrogen laser emitting a UV ray at 337.1 nm.
- the matrix then absorbs the photonic energy and the restitution of this energy leads to the sublimation of the matrix, the desorption of the molecules present in the population of micro-organism (s) and the appearance of matter in a qualified state of plasma.
- this plasma there is exchange of charges between molecules from the matrix and molecules from microorganisms. For example, protons can be torn from the matrix and transferred to the proteins, peptides and organic compounds present in the analysis zone. This step allows gentle ionization of the molecules present without inducing their destruction.
- the population of microorganism (s) thus releases ions of different sizes. The latter are then accelerated by an electric field and fly freely in a tube under reduced pressure, called flight tube.
- the smaller ions will then "travel" faster than larger ions, allowing them to separate.
- a detector At the end end of the flight tube is located a detector.
- the time of flight (or TOF for "Time Of Flight” in English) put by the ions is used to calculate their mass.
- a mass spectrum is obtained, representing the intensity of the signal corresponding to the number of ionized molecules of the same mass on charge [m / z], in function of the ratio m / z molecules that hit the detector.
- the mass-to-charge ratio [m / z] is expressed in Thomson [Th].
- the MALDI-TOF analysis can be a simple MALDI-TOF analysis, or a MALDI-TOF TOF analysis.
- a MALDI analysis plate has at least one and, in general, several analysis zones.
- the analysis zones form a spot, most often of circular shape.
- the surface of the plate is generally conductive, at least at the level of the analysis zone or zones.
- such an analysis plate is generally formed of a metal, or formed of a polymer such as polypropylene, said polymer being covered with a layer of stainless steel.
- the polymer may contain conductive material such as carbon black.
- Such a plate may be, for example, that marketed by the company Shimadzu, under the reference Fleximass TM DS disposable MALDI targets.
- MALDI plates are commercially available such as BioMérieux VITEK® MS (disposable) and Bruker Daltonics Maldi Biotarget (reusable). Such plates most often comprise from 48 to 96 analysis zones or spots, and at least one or even two or three reference analysis zones, which may be of different size from the analysis zones.
- the analysis plates intended for analysis by MALDI-TOF must have very rigorous geometrical characteristics, in particular thickness characteristics of the analysis plate and flatness of the test face. perfectly mastered. Indeed, the MALDI-TOF analysis relies notably on the comparison of the flight times of the different particles resulting from the ionization. It is easy to see that flight time is affected by the distance to be covered, and therefore by good control of the initial position of the sample.
- EP-2.106.858 discloses an analysis plate whose surface is structured to modify the wetting. This analysis plate is intended to allow analysis by mass spectrometry, but the nature of the analyzer considered for this analysis is not specified. The person skilled in the art would therefore certainly not consider using such a structured analysis plate for a mass spectrometry analysis in which the analysis is based on the measurement of a time of flight of the ionized particles.
- EP-1.814.137 discloses an analysis plate comprising a separate substrate and a measuring element which are in electrical contact.
- EP-2,792,471 discloses a MALDI analysis plate made of a polymeric material with a hydrophobic agent. The analysis plate is further coated with a layer of metallic material.
- EP-2,808,887 discloses an analysis plate for MALDI-TOF analysis which comprises a base plate of metal material covered with a strongly oriented graphite layer, which is assembled to the base plate by a conductive adhesive electricity.
- Some MALDI-TOF analysis plates are reusable. This implies that the analysis plate is cleaned and decontaminated, for example with a solvent, between two uses. It is therefore necessary that the plate supports the cleaning / decontamination process without alteration, which increases the manual procedure for using this type of analysis plate and the time required for the complete process of using the MALDI-TOF, especially in requiring a longer preparation time and more labor intensive.
- Other analysis plates are for single use, for example made of polymer material. Until now, the unit cost of such plates remains high. It appears the need to reduce the cost of manufacturing such analysis plates.
- the invention proposes an analysis plate comprising at least one analysis zone intended to receive a sample to be analyzed by mass spectrometry according to the MALDI-TOF technique, of the type comprising at least one test face on which is delimited at least one analysis zone, and of the type in which the plate comprises a flat support, characterized in that the support comprises at least one sheet of paper material comprising cellulosic fibers, and in that the analysis plate comprises at least one layer of metallic material.
- the layer of metallic material is attached to the sheet of paper material on the side of the test face.
- the layer of metallic material is reported on the sheet of paper material by vacuum metallization of the sheet of paper material.
- the layer of metallic material is reported on the sheet of paper material by transfer metallization.
- the layer of metallic material has a thickness of less than 0.5 micron.
- the layer of metallic material comprises aluminum.
- the sheet of paper material comprises, as fibers, exclusively cellulosic fibers.
- the sheet of paper material comprises cellulosic fibers and synthetic fibers, especially synthetic polymeric fibers.
- the sheet of paper material comprises cellulosic fibers and synthetic fibers, with, by mass, more cellulosic fibers than synthetic fibers.
- the paper material of the sheet of paper material comprises at least one hydrophobic agent.
- the sheet of paper material has a basis weight greater than or equal to 120 grams per square meter, preferably greater than or equal to 150 grams per square meter.
- the sheet of paper material has a basis weight less than or equal to 400 grams per square meter, preferably less than or equal to 300 grams per square meter.
- the support consists exclusively of paper material.
- the support comprises at least one support blade on which is reported the sheet of paper material.
- the support comprises at least one support strip of polymer material on which the sheet of paper material is attached.
- the support comprises two sheets of polymeric material superimposed, and the sheet of paper material is attached to one side of one of the two superimposed blades.
- the blade of polymeric material has a thickness in the range of 0.2 to 2 millimeters.
- the sheet of paper material has a grammage in the range of 60 grams per square meter to 200 grams per square meter.
- the sheet of paper material comprises at least one deformation obtained mechanically along the contour of at least one analysis zone, thus delimiting the at least one analysis zone.
- At least one analysis zone on the sheet of paper material comprises a deformation obtained mechanically over the entire extent of said analysis zone.
- the analysis plate comprises an ink marking defining at least one analysis zone.
- the invention also relates to the use of an assay plate having any of the above characteristics as a sample holder in a method of analyzing the sample by mass spectrometry according to the ALDI-TOF technique. .
- the analysis plate may be used with an adapter that holds the sheet of paper material around it.
- an adapter may comprise a plate, a frame and a clamping mechanism which causes the analysis plate to be clamped between the frame and the plate, the frame cooperating with the periphery of the analysis plate and having an opening that makes it possible to appear. at least one analysis zone of the analysis plate.
- Figure 1 is a schematic perspective view of an analysis plate according to the invention.
- FIGS 2, 3A and 3B schematically illustrate, in cross section, three embodiments of an analysis plate according to the invention, without support blade.
- FIGS 4A and 4B schematically illustrate, in cross section, two embodiments of an analysis plate according to the invention, with respectively one and two blade (s) of support.
- Figure 5A is a top view of a portion of the test face of an analysis plate according to the invention, illustrating more particularly a first embodiment of a marking of a test area.
- Figure 5B is a fragmentary diagrammatic cross-sectional view, broken away, illustrating the embodiment by mechanical deformation of the marking of FIG. 5A.
- Figures 6A and 6B are views similar to those of Figs. 5A and 5B, illustrating an alternative embodiment.
- Figures 7A and 7B are views similar to those of Figs. 5A and 5B, illustrating another alternative embodiment.
- Figure 8 schematically illustrates the production of several analysis plates by cutting a strip.
- FIG. 9A is a schematic exploded perspective view illustrating the use of an analysis plate according to the invention with a adapter, the elements being seen on the side of their lower face, in particular on the side of the support face of the analysis plate.
- Figure 9B is a schematic perspective view illustrating the use of an assay plate according to the invention with the adapter of Fig. 9B; 9A, seen from the side of the test face of the analysis plate.
- Figure 10 is a schematic cross-sectional exploded view of the whole of the Figs. 9B.
- Figure 11 is a schematic cross-sectional view illustrating the assembly of FIG. 9B in use configuration.
- Figures 12A to 12E are schematic views illustrating different structural variants of the analysis plate.
- FIGs. 1 and 2 We have illustrated in Figs. 1 and 2 a first example of an analysis plate 10 made according to the invention.
- the analysis plate 10 has, for example, in a known manner a plane shape in an extension plane.
- the analysis plate 10 has a thickness in the direction perpendicular to its extension plane which is for example less than one-tenth of the smallest dimension of the plate measured in the extension plane, commonly called width.
- the analysis plate 10 thus has a test face 12 and a bearing face 14 which extend parallel to the extension plane.
- the test face 12 is that on which at least one analysis zone is provided, in the illustrated example several analysis zones 16 each for collecting a biological sample to be analyzed.
- the analysis plate 10 thus has 48 analysis zones arranged in four columns of twelve analysis zones.
- it can be expected that it comprises a reduced number of analysis zones, for example one, two, four, five or eight zones of analysis 16.
- the analysis plate 10 may have, in its plane of extension, a smaller dimension of between 10 and 50 millimeters, for example 25 millimeters, and a larger dimension between 50 and 100 millimeters, for example 75 millimeters. millimeters.
- the analysis plate 10 extends in a horizontal plane, and that the test face 12 is an upper face and that the bearing face 14 is a lower face of the analysis plate 10.
- each analysis zone 16 is visually delimited from the remainder of the test face 12 of the analysis plate 10.
- each analysis zone 16 is substantially circular in shape.
- the analysis plate 10 can also comprise reference analysis zones (not shown in the figures), which can be used, for example, for the calibration of the apparatus as part of the MALDI-TOF analysis.
- the analysis plate 10 comprises a plane support 18, which comprises at least one sheet of paper material 20 comprising cellulosic fibers.
- the sheet of paper material 20 therefore has an extension plane corresponding to the plane of extension of the analysis plate 10.
- the paper material is a material which consists of agglomerated fibers, the fibers comprising cellulosic fibers.
- Cellulosic fibers are for example of plant origin.
- the agglomeration of the fibers of the paper material is obtained by the papermaking technique. According to this technique, the fibers are dispersed in an aqueous solution, optionally with the addition of auxiliary materials (fillers, dyes, glue, etc.), thus forming a pulp.
- the paper pulp is deposited in a thin sheet on a perforated table allowing the draining of a large part of the water contained in the paper pulp.
- Various pressing and drying operations of the web allow the agglomeration of the fibers giving the sheet of paper material 20 its cohesion.
- a sheet of paper material 20 may undergo surface treatments for example to deposit, on the surface of the sheet, one or more layers of additive materials for modifying the surface condition of the sheet of paper material.
- the sheet of paper material may also undergo mechanical treatments, including calendering, embossing, etc., also aimed at modifying the surface condition of the sheet of paper material.
- the sheet of paper material 20 may comprise, as fibers, exclusively cellulosic fibers.
- the sheet of paper material 20 comprises, as fibers, only cellulosic fibers, with the exception, however, of the possible presence of fibrous impurities.
- the mass of these fibrous impurities is less than 2% of the mass of paper material. This quantity can be measured according to the TAPPI T401 standard.
- the mass per square meter of the sheet of paper material also called basis weight, is measured according to ISO 536.
- the paper material sheet comprises cellulosic fibers and non-cellulosic fibers, especially glass fibers and / or synthetic polymers.
- Synthetic polymer fibers may in particular comprise polyester, polyethylene or polylactic acid fibers.
- glass microfibers from Lauscha Fiber International for example B-08-F fibers having a diameter of 0.8 microns in borosilicate; synthetic polymer fibers of the company Eastman Cyphrex, for example Cyphrex tm 10001 diameter 2.5 microns and length 2.5 millimeters PET
- Advansa synthetic polymer fibers for example Advansa 328 NSD fibers with a length of 6 mm and with a dtex of 1.7 in polyester or Advansa PLA fibers with a length of 3 mm and a dtex of 1.7 in PLA.
- an analysis plate 10 according to the invention will advantageously be preserved in a moisture-proof package.
- a package comprising an aluminum foil completely enclosing the analysis plate 10 may be formed.
- the analysis plate is packed under a controlled atmosphere, preferably by providing that the atmosphere inside the packaging either the driest possible, and possibly by providing inside the package a desiccant.
- an internal atmosphere is advantageously provided with a relative humidity of less than 5%.
- the relative humidity measurement can be measured using a calibrated hygrometer. The relative humidity can then be calculated from the formulas defined in standard NF X 15-110.
- analysis 10 comprising such a sheet of paper material, in particular by decreasing the time of evacuation for carrying out the analysis.
- the ratio between the mass of non-cellulosic fibers and the total mass of the fibers of the sheet of paper material is less than 50%. This value can be measured for a given paper according to the Tappi 401 method.
- the resistance of the paper material sheet to moisture absorption can also be achieved by other means.
- hydrophobic material for example a paraffin-containing material.
- PVDC Polyvinylidene
- the analysis plate 10 may comprise elements other than the sheet of paper material 20.
- the analysis plate 10 may comprise several sheets of paper material.
- the sheets of paper material are advantageously superimposed on each other, preferably over the entire extent of the analysis plate 10 in its extension plane.
- the different sheets of paper material can be assembled to one another, for example by gluing.
- one will use in this case a one-component polyurethane glue or a two-component polyurethane glue based on solvent (preferably non-aqueous) or without solvent.
- the application of the glue can be done by sprinkling or roller coating. It is possible to use an ultraviolet activatable glue. It is also possible to use a double-sided adhesive film. We will then prefer a film of the smallest possible thickness.
- the sheets of paper materials may be identical or not.
- the paper materials constituting these sheets of paper material, their grammage, and / or their thickness, etc. may be identical or different.
- the sheets of paper materials may have different dimensions, for example at least one different dimension in the extension plane of the analysis plate 10.
- the support 18 of the analysis plate 10 consists exclusively of paper material. This case does not prevent the analysis plate 10 further comprises additional layers or strata as will be described later. However, it is considered in this case that the support 18, which gives most of its mechanical rigidity to the analysis plate, consists exclusively of paper material. In the case of a support consisting exclusively of several sheets of paper material, the presence of an adhesive, especially an adhesive, or other means of assembly between the different sheets of paper material will not prevent the support from being made exclusively of paper material.
- the support 18 of the analysis plate 10 consists of a single sheet of paper material 20, as illustrated in FIGS. 2 and 3A, it preferably has a basis weight greater than or equal to 120 grams per square meter, more preferably greater than or equal to 150 grams per square meter.
- the support 18 of the analysis plate comprises several sheets of paper materials, as illustrated in FIG. 3B, the sum of the grammages of the sheets of paper materials of the support is preferably greater than or equal to 120 g per square meter, more preferably greater than or equal to 150 grams per square meter.
- this basis weight makes it possible to obtain sufficient rigidity for easy handling of the analysis plate in the context of its use in a MALDI-TOF analysis, but especially to thus guarantee a sufficiently flat geometry , including after handling, so as not to disturb the measurements by MALDI-TOF.
- the analysis plate 10 has a basis weight of paper material less than or equal to 400 grams per square meter, preferably less than or equal to 300 grams per square meter, in a sheet or distributed between several sheets. Indeed, it appears that, even in the presence of a single sheet of paper material and / or even in the case where the support of the analysis plate 10 consists exclusively of paper material, such weighting makes it possible to obtain a more than sufficient rigidity of the analysis plate. Beyond such a weight, there is a risk of increasing the susceptibility of the analysis plate 10 to store moisture, which has been seen to be a brake on the use, by requiring an increase in the emptying time of the analysis chamber in a MALDI-TOF analysis apparatus.
- the sheet of paper material 20 used in the analysis plate 10 according to the invention preferably has a thickness which may be between 100 and 450 microns, measured according to the standard NF EN ISO 534.
- the cumulative thickness of the sheets of paper materials, after their assembly to form the analysis plate is preferably between 100 and 1000 microns, measured according to standard NF EN ISO 534.
- the sheet of paper material 20 has, at least on its face turned towards the test face 12 of the analysis plate 10, a low roughness.
- this roughness measured according to the Bendtsen method defined in the ISO 8791-2: 2013 standard, may have a value of less than 750 milliliters per minute, preferably less than 500 milliliters per minute.
- the support 18 may comprise at least one support blade 22 on which the sheet of paper material 20 is attached.
- the support 18 thus comprises at least two elements, namely the support blade 22 and the sheet of paper material 20, as illustrated for example in FIG. 4A.
- the support blade 22 preferably has a planar shape extending parallel to the plane of extension of the analysis plate 10.
- the support blade 22 has a thickness in the direction perpendicular to its extension plane which is for example less than one-tenth of the smallest dimension of the plate measured in the extension plane.
- the carrier blade 22 is arranged below the sheet of paper material 20 or the plurality of sheets of paper material.
- the support blade 22 preferably has a lower face which forms the bearing face 14 of the analysis plate 10.
- the support blade 22 is for example made of polymer material, for example polypropylene or polypropylene-based material.
- the support blade is a black 800 Priplak® Classic polypropylene sheet, 800 micron thick.
- Such a support plate can be laminated with a plate of the same type using a Super-Lok® 364 glue from the company National Starch.
- Particles and / or fibers or other additives may be embedded in the polymeric material, especially electrically conductive particles and / or fibers, especially metal and / or metal-based particles and / or fibers and / or particles and / or or carbon fibers.
- the support blade 22 may be derived from a strip of material obtained by extrusion.
- the support blade 22 can thus be obtained in very long strip, packaged in roll or plate, so in a presentation similar to paper material obtained at the output of a paper machine.
- the sheet of paper material 20 and the support blade 22 can be assembled to one another, for example by gluing.
- the application of the adhesive can be done by sprinkling or by roller coating or by direct etching. It is possible to use an ultraviolet activatable glue. It is also possible to use a double-sided adhesive film. We will then prefer a film of the smallest possible thickness.
- the support 18 may comprise a plurality of support blades, in particular two superposed polymer material support blades, and the sheet of paper material 20 is attached to one face of the two superposed blades.
- the support blade 22 of polymeric material, or the plurality of support blades has, for example, a thickness in the range of 0.2 to 2 millimeters.
- the sheet of paper material 20 may have a basis weight less than that envisaged in the case where the support 18 consists exclusively of paper material.
- the sheet of paper material may have a basis weight in the range of 60 grams per square meter to 200 grams per square meter.
- the analysis plate 10 comprises at least one layer of metallic material.
- a stratum is understood to be an element or part of an element of the analysis plate 10 which extends in the extension plane of the analysis plate 10.
- the metallic materials include metals and their alloys.
- the layer 24 of metallic material is attached to the sheet of paper material 20.
- the layer 24 of metallic material may be attached directly to the sheet of paper material 20, with only the interposition of a possible layer of adhesive material such as a glue or an adhesive film, without the interposition of another support layer. as shown in FIG. 2.
- a possible layer of adhesive material such as a glue or an adhesive film
- a layer of metallic material may be attached to the sheet of paper material 20, on the side of the test face 12.
- the stratum 24 of metallic material may for example be an aluminum stratum, or an aluminum alloy. However, other metallic materials can be envisaged, for example silver or silver alloys.
- a layer 24 of metallic material may be attached to the sheet of paper material 20 by vacuum metallization of the sheet of paper material 20.
- the layer 24 of metallic material may form the surface of the test surface 12 of the analysis plate 10.
- the vacuum metallization technique is a thin film deposition technique widely used in the paper industry.
- the metal to be deposited is evaporated from a source of solid metal by heating at a high temperature in a vacuum deposition chamber in which a substrate, for example a strip of paper material, is introduced in a continuous manner.
- the particles resulting from the evaporation are deposited directly on the paper material on which they condense in the solid state.
- Such a Vacuum metallization is typically achieved in a vacuum metallizer.
- such a layer 24 of metallic material may be attached to the sheet of paper material 20 by transfer metallization.
- An exemplary embodiment of a transfer metallization is described in detail in the document FR-2,406,523 to which the skilled person can relate. Note that in this case, as illustrated in Figs. 3A and 3B, the analysis plate 10 can comprise, starting from the test face 12:
- a resin layer for example an acrylic or epoxy-acrylic resin 26;
- a layer of adhesive 28 for example a one-component polyurethane adhesive in a solvent phase
- An example of an embodiment of an analysis plate 10 according to the invention, in the variant of FIG. 3A, is constructed in the following manner.
- a sheet of paper material 20 made of cellulose fibers is obtained using a Foudrinier type paper machine.
- the paper preferably comprises at least one hydrophobic agent which is mixed with the pulp before the formation of the sheet.
- the hydrophobic agent that has been used is an aqueous emulsion of Alkyl Ketene Dimer (AKD).
- This sheet of paper is coated on both sides with a pigment solution (not visible in the drawings), for example a solution of calcium carbonate and Kaolin, by the coating technique air knife. Removal is about 10 g / m 2 per side.
- This sheet of paper material has a basis weight of 250 g / m 2 .
- metallization is applied by transfer metallization according to the teaching of FR-2,406,523.
- a laminate complex consisting of a PET base film (polyethylene) is formed terephthalate), a release layer (release), an acrylic resin layer 26 of about 2 microns and a deposit of aluminum alloy 24 (10 to 100 nanometers thick, preferably 15 to 50 nanometers, preferably about 20 nanometers), deposited under vacuum on the resin layer 26 to form the layer of metal material 24.
- This metal layer can be measured by commercial equipment for measuring thickness, especially those using radiometric methods ( X-ray fluorescence or backscattering p) allowing access to measurement resolutions between 100 nanometers and some Angstroms.
- This complex is assembled, with the layer of metallic material 24 turned towards the sheet of paper, using a layer of one-component solvent glue 28, against the upper face of the paper sheet 20.
- the glue 28 can to be one of those mentioned above.
- the amount of glue used can be for example 3 to 12 grams per square meter.
- the base film is detached in order to leave the adhesive layer 28, the metallization 24 and the resin layer 26 on the paper.
- the surface of the test face 12 of the analysis plate 10 is formed by the non-electrically conductive resin layer 26 which covers the metal material layer 24 .
- such an analysis plate 10 may comprise, as indicated above, other sheets of paper material and / or possibly one or more support blades.
- FIG. 3B an alternative embodiment which comprises all the elements of the embodiment of FIG. 3A, except that the sheet of paper material 20 has a basis weight of 80 g / m 2 , and which comprises an additional sheet of paper material 20 'assembled against the underside of the sheet of paper material 20, so the face opposite to the one on which is reported the layer 24 of metallic material.
- the assembly can be done by gluing with a layer of glue 28 '.
- the glue 28 ' can be one of those mentioned above.
- the sheet of additional paper material 20 ' has for example a basis weight of 170 g / m 2 .
- a PET film previously coated with a nano-chromium chloride-based release layer is coated with an epoxy / acrylic resin which is dried.
- This coated face is introduced into a metallizer in order to receive an aluminum deposit of about 20 nanometers.
- the metallized side is coated with a single-component solvent-based polyurethane glue by a coating in direct etching. It is dried before being pressed against a paper Satimat® 90 g / m 2 of the company Arjowiggins. The next day, the PET film is peeled from the surface of the paper leaving the visible metal deposit on the paper.
- This assembly is then bonded to a support assembly comprising at least a support blade, for example using a Super-Lok® 364 adhesive from the company National Starch.
- the support assembly comprises two support blades each of which is formed of a Priplak® Classic polypropylene black plate 800, 800 microns thick.
- the two support blades are for example glued with a Super-Lok® 364 glue from the company National Starch.
- an analysis plate 10 comprising a layer of metallic material, in particular of aluminum or of aluminum alloy, attached to an upper face of a sheet of paper material 20, such as illustrated in Figs. 3A or 3B, can form a perfectly satisfactory analysis plate 10 making it possible to obtain analysis results with the same reliability as a reference plate.
- a layer of metallic material in particular aluminum or aluminum alloys, having a thickness of less than 0.5 micron, or even less than 0.1 micron, or less than 0 , 05 micron.
- This layer of thin metal material may be the only electrically conductive layer of the analysis plate 10, including the possible presence, above the layer of metal material 24, of a layer of non-conductive material , in this case the resin layer 26.
- a layer 24 of metallic material, and more particularly aluminum or aluminum alloy preferably has a thickness greater than 0.01 micron. Such a thickness makes it possible in particular for the stratum not to be degraded during the evacuation of the analysis chamber.
- an analysis plate consisting exclusively of a sheet of paper by Powercoat HD 230 Arjowiggins company, which is an extremely smooth coated paper whose thickness is 222 microns and the grammage 219 g / m 2 , has not satisfied, with only a few peaks detected but with a spectrum without quality.
- Other tests with test plates not including a layer of metallic material reported on the test surface were unsatisfactory, including with a sheet of paper material having a basis weight of 300 g / m 2 .
- each analysis zone 16 of the test face 12 is at least visually marked on the test face 12.
- an analysis zone may be delimited on the test face by the presence of a mechanical deformation of the analysis plate 10, in particular by mechanical deformation of the sheet of paper material 20.
- the sheet of paper material 20 is mechanically deformed according to the contour of the analysis zone, in this case specific case according to a part of the contour of the analysis zone.
- the analysis zone 16 is a circular zone whose contour is delimited in part by a groove 29.
- the groove 29 is here in two parts, each in the shape of an arc of a circle, and the two parts face each other This groove 29 can be obtained by depressing the test face 12 in the direction of the thickness of the analysis plate 10, with plastic deformation of the sheet of paper material 20, thus obtaining a permanent mechanical deformation.
- the sheet of paper material is mechanically deformed over the entire extent of the analysis zone, in the form of a flat-bottomed bowl.
- the sheet of paper material is mechanically deformed over the entire extent of the analysis zone 16, and also around the analysis zone 16 to leave a raised bead 30 which extends into the illustrated example in a circle along the contour of the analysis zone 16.
- the analysis zone 16 is thus hollow with respect to the top of the bead 30, forming a bowl as in the previous example.
- the sheet of paper material 20 is surmounted by a layer 24 of metallic material forming the test face 12, and this layer of metal material 24 is also deformed to form the groove 29 or the bowl to Flat bottom or bead 30.
- the layer 24 of metallic material is obtained by transfer metallization, including with the possible additional presence of one or more support blades 22 as mentioned above.
- the depth of the permanent mechanical deformation is for example between 10 and 300 microns.
- the mechanical deformation which delimits the analysis zone 16 not only delimits it visually, but also allows to form a barrier to the propagation of the sample, and / or the reagent or reagents, and / or the matrix during the deposition on the analysis plate 10.
- this mechanical deformation can easily be performed according to conventional embossing techniques used in the paper industry.
- embossing can be carried out online, for example when the support is still in the form of a continuous strip.
- the analysis plate may comprise an ink marking. Such marking is preferably affixed to the test face 12.
- the marking may have, for example, a geometry similar to the mechanical deformation illustrated in the examples of FIGS. 5A, 6A or 7A.
- the marking can be carried out on the test surface 12, preferably over the entire extent of the analysis zone 16, with an ink having, once dried, a wetting angle for the sample and / or matrix which is different from the wetting angle of the surface of the constituent material of the test face 12, for the sample and / or the matrix.
- the wetting angle between the ink and the sample and / or the matrix is lower than the wetting angle between the surface of the constituent material of the test face 12 and the sample and / or the matrix, for example with AGFA Orgacon TM EL-P3145 ink sold by AGFA GEVAERT NV or its affiliates.
- the surface of the ink when it is dry, is more hydrophilic than the surface of the test surface 12.
- the ink makes it easier to deposit the sample and or the liquid-phase matrix, but the difference in wetting angle between the ink and the surface of the material constituting the test face 12 forms a barrier which will prevent, or at least limit, the extension of the deposit, confining the latter inside the analysis zone 16 marked by the ink.
- the ink is deposited not on the analysis zone 16, but around it, and it is then possible for example to provide that the wetting angle between the ink and the sample and or the matrix is larger than the wetting angle between the surface of the constituent material of the test face 12 and the sample and / or the matrix.
- this is done with the DuPont TM 5064H ink sold by EI from Pont de Nemours and Company or its affiliates, which has a higher wetting angle with water or formic acid than the surface of the metallized transfer paper carrier.
- This ink is conductive of electricity.
- the values below are wetting angles in degrees as a function of time measured with a Dynamic Absorption Tester device from Testing Machines, Inc. (TMI) using the TAPPI 558 method.
- the marking can be performed on the test surface 12, preferably over the entire extent of the analysis zone 16, with an electrically conductive ink.
- the ink-jet marking may be carried out by any known technique, in particular any technique used in the printing industry such as, for example, electrophotography printing, inkjet printing, screen printing, flexographic printing or an offset printing.
- the analysis zone 16 is a smooth surface, having, for example, a roughness comparable to, or even inferior to, that of the sheet of paper material 20.
- the surface of the analysis zone 16 is structured.
- this structuring will be obtained by mechanical deformation of the surface, and in particular by mechanical deformation of the sheet of paper material 20.
- This structuring can thus form, on the surface of the analysis zone 16, hollows and reliefs according to a regular or irregular geometry.
- the relative depth between the hollows and the reliefs of the surface of the structured analysis zone may for example be between 10 and 300 microns.
- the geometry and the relative depth of the depressions and reliefs of the surface of the structured analysis zone 16 can be scalable over the extent of an analysis zone 16, for example by variation of shape, size, step and / or depth of the hollows or reliefs.
- the structuring is formed of concentric circular lines 52, recessed or raised relative to the surface of the analysis zone 16.
- the circular lines are for example equidistant from each other, but they could have an evolutionary spacing, not constant.
- the circular lines 52 are for example distributed over the entire extent of the analysis zone 16.
- the circular lines are for example concentric with a circular contour 54 of the analysis zone 16.
- the structuring is formed of radial lines 56 coming from the same central point of the analysis zone 16, recessed or in relief with respect to the surface of the analysis zone 16.
- the radial lines are, for example, discarded angularly from each other at a constant angle, but they could have an evolutive, non-constant spacing.
- the lines Radial lines are, for example, distributed over the entire extent of the analysis zone 16.
- the radial lines are for example derived from the center of a circular contour 54 of the analysis zone 16.
- the patterning is formed of concentric circular lines 52 as described in FIG. 12A, and radial lines 56, as described in FIG. 12B.
- the structuring is formed of lines, recessed or raised relative to the surface of the analysis zone 16, forming a grid 54.
- the grid 58 may be a square grid formed of two perpendicular series of parallel straight lines, but one can also consider two non-perpendicular series of parallel straight lines, or more than two series of parallel lines, each series each having a different orientation. Within a series of parallel lines, the lines are for example equidistant from each other, but they could have an evolutionary spacing, not constant.
- the grid 58 extends for example over the entire extent of the analysis zone 16. However, the grid may be limited to only a part of the analysis zone 16, for example to a peripheral crown, of the zone Analysis 16.
- the patterning is formed of a multitude of repeated geometric elements, forming a repeating pattern 60, recessed or raised with respect to the surface of the analysis zone 16.
- the structuring is formed of a checkerboard repeating pattern 60, recessed or raised relative to the surface of the analysis zone 16.
- the pattern 60, 62 extends for example over any the extent of the analysis zone 16.
- the pattern could be limited to only a part of the analysis zone 16, for example to a peripheral crown of the analysis zone 16.
- an analysis plate 10 makes it possible to produce the analysis plate 10 using materials and techniques commonly used in the paper industry, making it possible to obtain a plate of analysis at very low cost, both from the point of view of the cost of the materials used and, more importantly, from the point of view of the cost of the manufacturing processes implemented.
- an analysis plate 10 according to the invention can be carried out, as illustrated in FIG. 8, by cutting individual analysis plates 10 starting from a strip of material 32 produced at very low cost.
- This strip of material 32 may comprise all of the sheet (s) of paper material 20, blade (s) support 22, layer 24 of metallic material, etc., envisaged for the production of the analysis plate 10 according to FIG. invention, pre-assembled in a laminated complex capable of being obtained in strip line of great length.
- mechanical deformation marking operations or ink deposition marking operations can use the corresponding techniques used in the printing industry, again implemented online for long length belts.
- analysis plates made according to the teachings of the invention make it possible to obtain, in a standard apparatus, a characterization of the samples in accordance with what is generally obtained with the pre-existing analysis plates. .
- MS spectra were also comparable, having the same resolution, the same number of peaks and the same dynamic range. All the peptides and proteins tested with the different matrix were detected on an analysis plate according to the invention, in a smooth version, with the same quality as on the reference target. The tests were carried out on 22 bacterial species and on yeasts, with masses between 2000 and 20000 Daltons, and with peptides and proteins whose mass was between 300 and 46000 Daltons.
- a plate according to the invention is therefore advantageously used as a sample support in a method of analysis of the sample by mass spectrometry according to the MALDI-TOF technique.
- the inventors For use in standard equipment for mass spectrometry according to the MALDI-TOF technique, the inventors have designed an adapter 34 which makes it possible to use the analysis plates 10 according to the invention, in particular the analysis plates according to the invention.
- Figs. 3A and 3B described above which have a reduced thickness compared to conventional analysis plates.
- the adapter 34 holds the analysis plate 10 by its periphery and makes it possible to position this sheet of paper material 20 in the analysis chamber of the apparatus so that the test face 12 of the analysis plate 10 is located at an equivalent position, in the direction perpendicular to its extension plane, to that of a conventional analysis plate, despite the difference in thickness between the two.
- the adapter 34 comprises a plate 36 and a frame 38.
- the plate 36 has a flat shape, and its dimensions are equal to that of the analysis plate 10 in the plane of extension of the plate.
- the plate 36 has an upper face 40 intended to receive the bearing face 14 of the analysis plate 10, and a lower face 41.
- the frame 38 is in the form of a profile which extends in a plane parallel to the plane of extension of the analysis plate 10, around the perimeter of the analysis plate 10.
- upper face 42 and a lower face 44 In the lower face 44, a clearance 45 is arranged which has the exact contour of the analysis plate 10.
- the depth of the clearance 45, in the direction perpendicular to the plane of extension of the analysis plate 10, is preferably greater than the thickness of the Analysis plate 10. In the example illustrated, this depth substantially corresponds to the sum of the thickness of the analysis plate 10 with the thickness of the plate 36, which can then also be received, at least in part in the clearance 45.
- the frame 38 delimits, in its upper face 42, an opening 46 whose dimensions in the extension plane are sufficient to reveal the entirety of the analysis zones 16 of the analysis plate 10 through this opening 46 when the analysis plate 10 is engaged in the clearance 45 of the lower face 44 of the frame 38, the test face 12 upwards.
- the opening 46 has, in the plane of extension of the plate 10, smaller dimensions than that of the plate 10 so that the bottom of the clearance 45 of the frame 38 forms a stop surface 48 against which press around the test surface 12 of the analysis plate 10.
- the adapter 34 also comprises a clamping mechanism which causes the clamping of the analysis plate 10 between the frame 38 and the plate 36.
- the clamping mechanism is a mechanism Magnet comprising a series of magnets 50.
- the magnets 50 are carried by the frame 38, so that the plate 36 is made at least partly of ferromagnetic material, for example of ferromagnetic metal and / or comprises also corresponding magnets arranged with their inverted magnetic polarity.
- the opposite arrangement could be provided.
- Other clamping mechanisms could be envisaged, for example with clamps or screws.
- the magnetic mechanism has the advantage of a very easy implementation and provides a clamping force sufficient to maintain the plate 10 without damaging it, especially in avoiding excessive tightening and adapting to a variable range of paper thickness without modification of the adapter.
- the depth of the clearance 45 of the frame 38 and the thickness of the plate 36 thus determine, according to whether one or the other rests against the reception face of the analysis chamber, the position of the test face 12 of the analysis plate 10 in the analysis chamber, in a direction perpendicular to the plane of extension of the plate 10. Also, the depth of the clearance 45 of the frame 38 and the thickness of the plate 36 are calculated so that the test face 12 of the analysis plate 10 is arranged, in a direction perpendicular to the plane of extension of the plate 10, at a desired altitude for the proper functioning of the apparatus.
- an adapter 34 makes it possible to avoid any damage to the analysis plate 10 during its handling, in particular when it is introduced into the mass spectrometry equipment. It is indeed possible to handle only the adapter 34, which can be made of plastic material and / or metal. This avoids in particular the risk of folding the analysis plate 10 when it is thin, for example with a support 18 consisting only of one or more sheets of paper materials 20, 20 ', without the presence of a blade additional support.
- the same apparatus can be used indifferently with a conventional analysis plate or with an analysis plate according to the invention without requiring registration of the mass peaks.
- the invention is not limited to the examples described and shown because various modifications can be made without departing from its scope.
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- Chemical Kinetics & Catalysis (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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FR1753705A FR3065652B1 (fr) | 2017-04-27 | 2017-04-27 | Plaque d'analyse maldi-tof a support papier et son utilisation |
PCT/FR2018/051056 WO2018197814A1 (fr) | 2017-04-27 | 2018-04-26 | Plaque d'analyse maldi-tof a support papier et son utilisation |
Publications (1)
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EP3615218A1 true EP3615218A1 (fr) | 2020-03-04 |
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EP18723575.9A Pending EP3615218A1 (fr) | 2017-04-27 | 2018-04-26 | Plaque d'analyse maldi-tof a support papier et son utilisation |
Country Status (5)
Country | Link |
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US (1) | US20200114346A1 (fr) |
EP (1) | EP3615218A1 (fr) |
CN (1) | CN110997146A (fr) |
FR (1) | FR3065652B1 (fr) |
WO (1) | WO2018197814A1 (fr) |
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FR3105024B1 (fr) * | 2019-12-20 | 2022-04-15 | Commissariat Energie Atomique | Dispositif à actionnement pneumatique à substrats à base de papier |
FR3105025A1 (fr) * | 2019-12-20 | 2021-06-25 | Commissariat à l'Energie Atomique et aux Energies Alternatives | Dispositif micro-fluidique réalisé par embossage d’un substrat à base de papier |
FR3105026B1 (fr) | 2019-12-20 | 2022-07-08 | Commissariat Energie Atomique | Dispositif micro-fluidique à substrats à base de papier |
FR3117897A1 (fr) | 2020-12-21 | 2022-06-24 | Commissariat à l'Energie Atomique et aux Energies Alternatives | Procédé de récupération d'un échantillon capturé dans une membrane hydrophile et dispositif destiné à mettre en œuvre le procédé |
Family Cites Families (12)
Publication number | Priority date | Publication date | Assignee | Title |
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DE2747241C2 (de) | 1977-10-21 | 1986-03-20 | Helmuth 2058 Lauenburg Schmoock | Verfahren zur Herstellung einer Schichtstoffkombination |
DE3821582A1 (de) * | 1988-06-25 | 1990-02-15 | Hoechst Ag | Folie fuer die transfermetallisierung |
AU774336B2 (en) * | 1999-04-27 | 2004-06-24 | Ciphergen Biosystems, Inc. | Probes for a gas phase ion spectrometer |
WO2003071263A1 (fr) * | 2002-02-19 | 2003-08-28 | Genome Institute Of Singapore, National University Of Singapore | Dispositif de focalisation isoelectrique |
US7019288B2 (en) * | 2003-09-30 | 2006-03-28 | Sequenom, Inc. | Methods of making substrates for mass spectrometry analysis and related devices |
US6825478B1 (en) * | 2003-10-10 | 2004-11-30 | Perseptive Biosystems, Inc. | MALDI plate with removable magnetic insert |
US20070001114A1 (en) * | 2005-06-29 | 2007-01-04 | Goodley Paul C | Apparatus and method for ion capture and production |
EP1814137A3 (fr) | 2006-01-27 | 2008-04-23 | Sony DADC Austria AG | Assemblage de porte-echantillons pour de la spectrometrie de masse |
EP2106858B1 (fr) | 2008-03-31 | 2011-11-02 | Sony DADC Austria AG | Substrat et plaque cible |
US20140008115A1 (en) * | 2011-03-28 | 2014-01-09 | Toray Advanced Film Co., Ltd. | Conductive laminate and touch panel |
EP2792471B1 (fr) | 2013-04-16 | 2018-01-31 | Stratec Consumables GmbH | Pièces en polymère |
JP2014232055A (ja) | 2013-05-29 | 2014-12-11 | 株式会社島津製作所 | Maldi質量分析用測定基板 |
-
2017
- 2017-04-27 FR FR1753705A patent/FR3065652B1/fr active Active
-
2018
- 2018-04-26 WO PCT/FR2018/051056 patent/WO2018197814A1/fr unknown
- 2018-04-26 US US16/603,687 patent/US20200114346A1/en active Pending
- 2018-04-26 EP EP18723575.9A patent/EP3615218A1/fr active Pending
- 2018-04-26 CN CN201880027902.0A patent/CN110997146A/zh active Pending
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WO2018197814A1 (fr) | 2018-11-01 |
FR3065652B1 (fr) | 2021-07-23 |
US20200114346A1 (en) | 2020-04-16 |
FR3065652A1 (fr) | 2018-11-02 |
CN110997146A (zh) | 2020-04-10 |
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