WO2014177675A9 - Plaques pour échantillon destinées à une spectrométrie de masse à désorption-ionisation laser assistée par matrice - Google Patents

Plaques pour échantillon destinées à une spectrométrie de masse à désorption-ionisation laser assistée par matrice Download PDF

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Publication number
WO2014177675A9
WO2014177675A9 PCT/EP2014/058953 EP2014058953W WO2014177675A9 WO 2014177675 A9 WO2014177675 A9 WO 2014177675A9 EP 2014058953 W EP2014058953 W EP 2014058953W WO 2014177675 A9 WO2014177675 A9 WO 2014177675A9
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sample
sample plate
mass spectrometry
ldi
laser desorption
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PCT/EP2014/058953
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English (en)
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WO2014177675A3 (fr
WO2014177675A2 (fr
Inventor
Niels-Christian Reichardt
Javier CALVO MARTÍNEZ
Juan ECHEVARRIA RUIZ
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Asociación Centro De Investigación Cooperativa En Biomateriales
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Publication of WO2014177675A2 publication Critical patent/WO2014177675A2/fr
Publication of WO2014177675A9 publication Critical patent/WO2014177675A9/fr
Publication of WO2014177675A3 publication Critical patent/WO2014177675A3/fr

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    • 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

Definitions

  • the present invention relates to sample plates for mass
  • MALDI-ToF MS matrix assisted laser desorption/ionization time of flight mass spectrometry
  • an organic matrix for example, 2 , 6-dihydroxy benzoic acid
  • MALDI is typically a two-step process. Rapid heating by
  • nanosecond pulsed laser irradiation leads to matrix ablation and evaporation which carries the analytes into the gaseous phase.
  • Analyte ion formation can follow several different pathways and often a distinction between matrix ion formation (primary path) and analyte ion formation in the plume (secondary path) can be made. 1,2 Only a very small fraction of desorbed analytes are ionized and ionization yields (in positive mode) depend on various factors such as fluence, analyte basicity, temperature, matrix type etc.
  • MALDI-ToF MS has proved invaluable for the analysis of large molecules and for proteomics, the analysis of small molecules for metabolomics , drug discovery and tissue imaging is hampered by the spectral interference of matrix-derived species of masses below 700Da.
  • MALDI- ToF MS for co-crystallization and solubility of analyte and matrix have motivated the search for alternatives based on soft laser desorption ionization.
  • SALDI-MS surface assisted laser desorption ionization mass spectrometry
  • WO 2004/113924 relates to a method of capturing peptide from gels onto surfaces formed from polycarbonate or polyester that can then be studied using mass spectroscopy.
  • WO 2006/083151 relates to sample plates formed from etched and coated substrates.
  • Stainless steel is the only form of steel mentioned.
  • WO 2007/133724 describes chips for use in mass spectroscopy with self-assembled monolayers and capture agents for binding to analyte.
  • the substrate on which the layers are assembled can be metallic; the only metals specified are gold and silver.
  • US 2004/024545 relates to LDI sample plates coated with a thin layer of carbon.
  • the underlying substrate can be metallic, but only conventional stainless steel and gold coated steel plates are described.
  • US 2004/0038423 relates to coated stainless steel MALDI plates.
  • GB 2378755 relates to a support for holding conventional
  • GB 2381068 discloses laser etched and coated MALDI plates relating to conventional stainless steel as the substrate.
  • the present invention is based on the finding that sample plates for surface enhanced laser desorption ionization (LDI) mass spectrometry having sample surfaces formed from weathering steel, and in particular plates of cut and polished weathering steel sheets, can be employed as sample plates for the sensitive analysis of a wide range of analytes by surface enhanced laser desorption mass spectrometry.
  • LIDI laser desorption ionization
  • Weathering steels commonly referred to by the trade name COR-TEN®, are low-alloy steels that, due to doping with nickel, chromium, phosphorous, silicon and calcium, are protected against corrosion through the formation of a nanostructured iron oxide and/or hydroxide mesh or other nanostructure such as a plurality of iron oxide and/or iron hydroxide nanowires, nanotubes, nanorods and/or nanofibers.
  • weathering steels include copper, manganese, vanadium,
  • Weathering steel is commercially available, of comparatively low cost and, for the present uses and methods, shows good stability with respect to storage, and additionally stability under storage at ambient conditions, low cost of production (including the possibility of having single use slides), and low levels of background ions.
  • the present invention provides a sample plate for surface enhanced laser desorption ionization (LDI) mass spectroscopy which comprises a sample surface formed from a weathering steel.
  • LDM laser desorption ionization
  • the sample plates of the present invention may be used in different forms of laser desorption ionization (LDI) mass spectrometry, including surface assisted laser desorption ionization (SALDI) mass spectrometry or surface enhanced laser desorption ionization (SELDI) mass spectrometry.
  • LDDI laser desorption ionization
  • SALDI surface assisted laser desorption ionization
  • SELDI surface enhanced laser desorption ionization
  • the sample plate is cut from a sheet of weathering steel.
  • the sample surface of the slide has a passivated layer as obtainable by removing an outer iron oxide layer on the sample surface of the weathering steel and then exposing the resultant surface to humid atmospheric conditions to promote slow formation of rust crystals on the surface. This enables sample plates to be produced easily and at low production costs .
  • the sample plates enable laser desorption ionization (LDI) mass spectrometry to be carried out which are capable of detecting analyte species present in nanomole quantities, and more preferably detecting analyte species present in picomole quantities, and even more preferably detecting analyte species present in femtomole quantities.
  • LIDI laser desorption ionization
  • the present invention provides a method of making a sample plate for laser desorption ionization (LDI) mass spectrometry, the method comprising:
  • the present invention provides a sample plate obtainable by a methods described herein.
  • the present invention provides the use of a sample plate of the present invention in the detection of an analyte using laser desorption ionization (LDI) mass
  • the present invention provides a method of detecting an analyte using laser desorption ionization (LDI) mass spectrometry, the method comprising: depositing the analyte onto the sample surface of a sample plate of the present invention;
  • LBI laser desorption ionization
  • sample plates are sufficiently inexpensive to be single use plates, they are also sufficiently easy to re-use for example by washing the sample surface, e.g. with eOH, hexanes, and/or water.
  • sample plates made of weathering steel can be expected in small molecule analysis in drug discovery and academic research, tissue imaging by MS, as single use sample plates in kits for the quantification of metabolites, food ingredients (example lactose) or the glycoanalysis of
  • glycoproteins by isotopic dilution.
  • FIG. 1 SALDI- S of synthetic bi-antennary glycan equipped with aminopentyl linker 1.
  • Figure 2. A Comparison of different surfaces in LDI-MS detection of biantennary glycan 1.
  • Figure 8 Direct lactose quantification in diluted crude milk sample by isotopic dilution.
  • Figure 10 Glycan analysis on a hydrophobic weathering steel plate .
  • Figure 11 TEM images at various magnifications showing the effect of slides prepared using treatment Tl, stored in the lab at ambient conditions.
  • Figure 12. SEM images of COR-TEN steel after storage at room temperature for 48 h and then after subsequent 1 h immersion in deionised water at various magnifications.
  • Figure 13. XPS analysis of slides shown in Figure 14, Upper image: polished slide stored at room temperature and XPS analysis of COR-TEN steel after storage at room temperature. Lower image: image and XPS spectra of slide stored at room temperature and subsequent immersion in deionized water for 1 h
  • FIG. 1 Matrix-free LDI mass spectra collected from mouse brain tissue sections on a polished weathering steel slide. The tissue sections had not been processed after mounted in the target.
  • FIG. 1 Matrix-free LDI mass spectra collected from mouse brain tissue sections on a OTS coated weathering steel slide. The tissue sections had not been processed after mounted in the target .
  • FIG 20 LDI-MS spectra of IgG glycans (up), and IgG glycans in the presence of a labeled glycan standard (down) using a OTS- coated slide.
  • Figure 21 LDI-MS spectra of the mixture of 8 glycan standards using a OTS-coated slide.
  • Figure 22 A mixture of 8 glycan standards analyzed by LDI-MS in weathering steel slides after polishing and washing (middle) , after TMO coating (up) and by MALDI-MS using DHB matrix (down) .
  • weathering steel is understood in the art and describes a group of steel alloys that, owing to their alloy content, exhibit increased resistance to atmospheric corrosion through the formation of a corrosion resistant oxide patina. Weathering steels are also often referred to as atmospheric corrosion resistant steels, self-protecting steels, self-passivating steels, and weather resistant steels.
  • Weathering steels are low alloy steels. Commonly used alloying elements include nickel, copper, chromium, phosphorous, silicon and calcium, although other alloying elements, including
  • manganese, vanadium, molybdenum, sulphur and rare earth elements may also be used.
  • Preferred alloying combinations may include Cu-Cr and Cu-Cr-P- (Ni ) .
  • the weathering steel is a weathering steel comprising one or more of the following alloying elements in the composition percentage range given: carbon (0 - 0.2%), silicon (0 - 1%), manganese
  • the weathering steel is a weathering steel comprising one or more of the following alloying elements in the composition percentage range given in parentheses: carbon (0.12 - 0.19%), silicon (0.25 - 0.75%), manganese (0 - 1.5%), phosphorus (0 -
  • the weathering steel is a weathering steel comprising one or more of the following alloying elements in the composition percentage range given in parentheses: carbon (0.12 - 0.19%), silicon (0.25
  • the weathering steel comprises at least 0.2%, preferably at least 0.3%, chromium, and in some preferred embodiments the percentage chromium content is in the range 0.3 - 1.5%, preferably 0.3 - 1.25%. In some embodiments, the weathering steel comprises at least 0.1%, preferably at least 0.2%, copper, and in some preferred embodiment the percentage copper content is in the percentage range 0.1 - 0.6%, preferably 0.25 - 0.55%. In some embodiments, the weathering steel
  • weathering steels suitable for use according to the present invention include, but are not limited to, COR-TEN A® and COR-TEN B@; EN 10155 grade weathering steels available from COR-TEN®, and other COR-TEN® weathering steels,
  • 09CuP, 09CuPCrNi-A, and 09CuPCrNi-B (commercially available from YUSHENG IRON AND STEEL CO., LIMITED), and ferrite-perlite and ferrite-bannite weathering steels.
  • the present inventors have found that the surface formed in this passivation process desorbs and ionizes adsorbed analytes under irradiation with a laser at 355nm very efficiently without the addition of any organic matrix compound. No use for matrix-free desorption ionization employing this material as a sample plate has been reported before. Studies have shown that the rust on some weathering steels can be divided into two different layers, an outer layer with a- and ⁇ -FeOOH phases and an protective inner layer with enriched Cu and P content, which is and a nanometric mesh of FeOOH.
  • this protective inner layer is primarily composed of nanometric Cr-goethite crystals "containing surface-adsorbed and/or inter- granular CrO x 3 ⁇ 2x complex anions" 28 within Fe(0,OH) 6 network leads to a distortion of the rust structure. 29
  • the heterogeneously-inserted surface chromium leads to the formation of very fine crystals rust with a consistent size distribution due to the increase in nucleation sites and a decrease of the critical radius of nucleation r*.
  • sample plates of the present invention may be used for laser desorption ionization (LDI) mass spectrometry and are capable of detecting molecular species with mass/charge (m/z) ratios below 700, more preferably below 600, more preferably below 500, more preferably below 400, with signal to noise ratios greater than 5
  • LIDI laser desorption ionization
  • the sample plates of the present invention may be used for laser desorption ionization (LDI) mass spectrometry is capable of detecting molecular species with mass/charge (m/z) ratios below 700, more preferably below 600, more preferably below 500, more preferably below 400, with signal to noise ratios greater than 25.
  • LIDI laser desorption ionization
  • the sample plates of the present invention may be used for laser desorption ionization (LDI) mass spectrometry is capable of detecting molecular species with mass/charge (m/z) ratios below 700, more preferably below 600, more preferably below 500, more preferably below 400, with signal to noise ratios greater than 50.
  • LIDI laser desorption ionization
  • the sample plates of the present invention may be used for laser desorption ionization (LDI) mass spectrometry is capable of detecting molecular species with mass/charge (m/z) ratios below 700, more preferably below 600, more preferably below 500, more preferably below 400, with signal to noise ratios greater than 100.
  • LIDI laser desorption ionization
  • the sample plates of the present invention may be used for laser desorption ionization (LDI) mass spectrometry is capable of detecting molecular species with mass/charge (m/z) ratios below 700, more preferably below 600, more preferably below 500, more preferably below 400, with signal to noise ratios greater than 100. More preferably, the sample plates of the present invention may be used for laser desorption ionization (LDI) mass spectrometry is capable of detecting molecular species with mass/charge (m/z) ratios below 700, more preferably below 600, more preferably below 500, more preferably below 400, with signal to noise ratios greater than 200.
  • LBI laser desorption ionization
  • a sample plate of suitable size for example, 2.75 x 7.5 cm and 1 mm thickness, is laser cut from a sheet of weathering steel, for example COR-TEN A ⁇ or COR-TEN B®.
  • the outer oxide layer of the sample surface is then removed from the sample plate using abrasion, for example using a suitable rotating metal brush or sandpaper. Passivation of ' the surface to form the fine nanostructured iron oxide/hydroxide surface advantageous for use in the methods of the present invention may then occur either through storage at, for example, room temperature, or be
  • the sample surface may be immersed in water for between 30 minutes and 24 hours, and more preferably for between 30 minutes and 2 hours. This may be followed by a drying step, conveniently at 18-25 °C. Exposing the sample surface to humid atmospheric conditions to promote slow formation of rust crystals on the surface. By way of example, the passivating step may last between one week and one year. If desired, the surface may then be derivatised, for example, through the application of a hydrophobic layer such as a layer of octadecylsilane or
  • trimethoxy (octadecyl ) silane
  • the surface of the plate may be derivatised, for example, through the application of a tetraethylorthosilicate film.
  • the film can then be further derivatized for example by immersion in a silane to promote silanization, the silane is preferably an alkyl silane for example, but not limited to, methyl silane.
  • Silanization can be affected in a solvent for example an organic solvent,
  • silanization can be performed for example at room temperature. Silanization can be performed for example from 1 to 48 hours, preferably about 24 hours. After the silanization the resulting slide can be rinsed for example with an organic solvent, preferably dichloromethane. The slide may then be dried prior to loading the analyte for example under an argon flow. It may be preferable to store the slide in a desiccator until used.
  • Microarrays are now a commonly used format for most high- throughput screening applications in genomics, proteomics and glycomics and the ability to analyse them by more than a single readout method is desirable to broaden their applications.
  • the present invention provides a method of making a microarray on a surface of a sample plate according to the present invention, the method comprising:
  • linker molecules comprise a hydrophobic group capable of non-covalently binding to the support layer and a reactive functional group
  • binding agents comprise a functional group capable of reacting in situ on the microarray with the reactive functional group of the linker molecules to covalently link the binding agents to the linker molecules immobilized on the sample plate, thereby forming the microarray.
  • the present invention further provides a microarray supported on a sample plate according to the present invention as obtainable by this method or any other method described in US 14/203611.
  • PCT/EP2014/056737 which is herein incorporated by reference in its entirety, describes methods and materials for the
  • PCT/EP201 /056737 provides a kit for identifying a glycan in a sample, the kit comprising:
  • a tagged standard comprising one or more isotopically-labelled glycans
  • the present invention provides a kit as described in PCT/EP2014/056737 further comprising a sample plate formed of weathering steel as described herein according to any described embodiment of the present invention.
  • the sample plate comprises a hydrophobic layer, for example, an organic silane, e.g. an alkyl silane such as
  • OTS octadecylsilane
  • alkoxy silane such as
  • TMO trimethoxy (octadecyl) silane
  • the passivation process may be accelerated by immersing the slides in deionised water, tap water and artificial sea water, wiping them clean with a lint free cloth.
  • a larger batch of samples plates (100 slides) of 2.5x7.5 cm size and 1 mm thickness were laser cut from Corten® steel sheets and the outer iron oxide layer removed by oil-free polishing with a rotating metal brush.
  • the slides were kept in a humidity chamber during months prior to use in LDI experiments to promote slow passivation of the exposed metal surfaces but without visible rust formation.
  • Figure 2A shows that the weathering steel sample plate exhibited the highest S/N ratio of all surfaces tested with a nearly 4.5 fold gain in sensitivity over the standard sample plates at considerably lower fluence.
  • Figure 2B shows that the even at femtomole quantities, the same standard can be detected with good signal to noise ratio on the weathering steel sample plate that had been immersed in water for 1 hour and dried before analysis.
  • the sensitivity of the weathering steel plates according to the present invention compares extremely favourably with scratched and polished stainless steel plates, as can be seen in Figure 2A. This sensitivity allows analytes present in only very small quantities to be detected, as is demonstrated in Figure 2B.
  • the plate for this experiment plate had not been immersed in water prior to analysis, and was made from polished plain weathering steel.
  • Figure 4 shows mass spectra of example compounds after deposition of 1 ⁇ of a 4mM aqueous solution which amounts to picomole quantities of analytes onto the weathering steel sample plates.
  • the selection included the drugs lamivudine (m/z 229.1), a reverse-transcriptase inhibitor used for the treatment of
  • Lactose is an important constituent of cows milk and the
  • Figure 9 shows a comparison of the lipid profile of a human breast milk sample (Sigma Aldrich) compared to a sample of bovine milk.
  • the magnification shows a shift of to higher masses for the most abundant triglycerides in human milk sample compared to bovine milk ( Figure 9, bottom spectra), with TG ( 16 : 0/18 : 1/18 : 1 ) being the most abundant.
  • N-glycans are an important post-translational modification of therapeutic antibodies and proteins, which can strongly influence Fc-receptor binding in antibody-dependant cell mediated
  • ADCC cytotoxicity
  • SALDI-MS in combination with isotopically tagged glycans could provide the quantitative mass spectrometric methods required for the rapid, and inexpensive glycoanalysis of iriAbs and other therapeutic glycoproteins with minimal sample preparation.
  • N-glycans released by treatment with peptide N-glycosidase F from a human serum IgG sample were analyzed on a weathering steel plate which had been coated with octadecylsilane (OTS) to form a hydrophobic layer.
  • OTS octadecylsilane
  • OTS coated slides for LDI-MS glycan analysis OTS coated slides for LDI-MS glycan analysis .
  • a sample of glycans released from human IgG by PNGaseF treatment was loaded directly in the OTS-coated slide (200 pmol of total glycan content) and analyzed by LDI-MS.
  • the glycan sample was spiked with an amount of labeled glycan standard G2F.
  • the mixture of natural glycans and the standard was loaded in the slide and analyzed by LDI-MS ( Figure 20) .
  • a mixture of 8 labeled N-glycan standards was prepared in d H 2 0 as a 50 ⁇ solution of each glycan.
  • the mixture was loaded in the OTS-coated slide (0.5 ⁇ , 25 pmol of each glycan) and analyzed by LDI-MS ( Figure 21) . Polished slides and TMO (trimethoxy octadecyl silane) coated slides for LDI-MS glycan analysis .
  • Polished slides washing Polished Corten slides were thoroughly cleaned by immersion and sonication in hexane and isopropanol (10 minutes each) avoiding any paper rubbing. After this procedure, the clean slides were dried under an argon flow and stored in a desiccator until used.
  • TEOS Tetraethyl orthosilicate
  • tetraethylorthosilicate solution (1:1) containing 1 % of acetic acid for 30 seconds followed by one minute in water. After this time the slides are dried under an argon flow. The TEOS - water cycle is then repeated 3 times until the desired film properties are obtained. Finally, the coated substrates are cured for 1 hour at 80 °C and then stored in a desiccator until used.
  • TMO Trimethoxy (octadecyl) silane silanization conditions
  • Detection of a mixture of 8 glycan standards using a TMO-coated weathering steel slide is shown in Figure 22.
  • the signal to noise ratio is comparable to that of the polished weathering steel slides.
  • Both the TMO-coated and polished weathering steel slides exhibit a similar signal to noise ratio than that observed using standard MALDI techniques with a DHB matrix.
  • Figure 23 demonstrates that TMO-coated weathering steel slides can be used to detect 8 glycan standards in high resolution without using mass deflection.
  • the ability to analyse samples without mass deflection enables the detection of compounds present in only small amounts or compounds that readily decompose upon ionisation.
  • non-targeted mass spectrometry studies such as tissue imaging, metabolomics or where little background ions are expected are preferably carried out without mass deflection, for example by employing SALDI-MS.
  • Figures 11, 12, 14 and 15 show SEM images at varying
  • FIG. 11 shows XPS analyses of a COR-TEN A® surface after passivation at room temperature and of a COR-TEN A® surface which has undergone accelerated passivation through immersion in water for one hour followed by storage at room temperature for 48 hours.
  • the spectra shows the elemental composition at different sputtering times which relates directly to surface depth.
  • Upper XPS spectra shows very low iron oxide level confined to the outer layer while the lower spectra of the oxidised surface shows a thick iron oxide layer protruding far into the material.
  • Figure 16 shows spectra of glycan 1 on a weathering steel plate passivated through immersion in water for one hour followed by storage at room temperature for 48 hours. Ions for iron oxide background peaks can be observed when deflector is turned off.
  • Polished and OTS-coated slides (0.8 um roughness) .
  • the surface topology of both surfaces was analysed by scanning electron microscopy (SE ) while depth dependant changes in the elemental surface composition due to corrosion were studied by X-ray photoelectron spectroscopy (XPS) .
  • SE scanning electron microscopy
  • XPS X-ray photoelectron spectroscopy
  • the inventors then evaluated the difference in LDI-MS imaging observed with the polished vs OTS-coated weathering steel slides.
  • a new batch of 1 mm thickness weathering steel slides was polished with a rotating metal brush obtaining a mirror-like surface (0.07 ⁇ surface roughness) .
  • a number of the polished slides were coated with octadecylsilane (OTS) to form a
  • Plain weathering steel slides and OTS-treated hydrophobic 1mm thick slides were tested for LDI imaging of mouse brain sections.
  • a single mouse brain was cut by a cryostat microtome into 4 urn and 20 ⁇ thick sections and thaw mounted onto weathering steel slides.
  • the brain sections were fixed to the slides and were dried after removal from the freezer and stored under vacuum.
  • the 4 ⁇ sections were used for direct LDI of the dry tissue ( Figure 17, polished slides; Figure 18, OTS-coated slides) .
  • Both slides provide mass data over a wide range of masses.
  • the hydrophobic slides provide particular clear LDI images. Without wishing to be bound by theory, it is thought that the increased quality of the images relates to improved sensitivity which may also affect the S/N ratio. A possible explanation of this is that the UV-Vis absorbance of the hydrophobic slides is higher than the polished slides (100% vs 70% at 355 nm) .
  • passivation process can be used as a low-cost and reusable sample plate with good to excellent sensitivity for the detection of a broad range of analytes by surface assisted and matrix-free laser desorption ionisation mass spectrometry.
  • silane chemistry e.g. OTS
  • standard protocols can easily change the surface using silane chemistry (e.g. OTS) employing standard protocols
  • sample plates with specifications required for use in MS analysis flatness, purity
  • LDI surfaces which have been or are currently commercialised and which require the use of clean room facilities for carrying out sophisticated multi-step surface modifications.
  • Possible applications for sample plates made of weathering steel can be expected in small molecule analysis in drug discovery and academic research, tissue imaging by MS, as single use sample plates in kits for the quantification of metabolites, food ingredients (example lactose) or the
  • glycoanalysis of glycoproteins by isotopic dilution Further covalent and non-covalent functionalisation of sample plates, e.g. with affinity probes can provide a surface for the

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Abstract

La présente invention concerne des plaques pour échantillon destinées à une spectrométrie de masse à désorption-ionisation laser (LDI) assistée par matrice ayant des surfaces pour échantillon constituées d'acier résistant aux intempéries. En particulier, des plaques de feuilles d'acier résistant aux intempéries découpées et polies peuvent être employées en tant que plaques pour échantillon en vue de l'analyse sensible d'une large plage d'analytes par spectrométrie de masse à désorption-ionisation laser assistée par matrice. Les aciers résistant aux intempéries sont des aciers faiblement alliés qui sont protégés contre la corrosion grâce à la formation d'une maille d'oxyde de fer et/ou d'hydroxyde nanostructurée ou autre nanostructure. L'acier résistant aux intempéries est disponible dans le commerce, de coût relativement faible et montre, pour les utilisations et procédés de la présente invention, une bonne stabilité par rapport au stockage, un faible coût de production et de faibles niveaux d'ions de fond.
PCT/EP2014/058953 2013-05-02 2014-05-01 Plaques pour échantillon destinées à une spectrométrie de masse à désorption-ionisation laser assistée par matrice WO2014177675A2 (fr)

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