TY - JOUR A1 - Nietzold, Carolin A1 - Dietrich, Paul A1 - Holzweber, M. A1 - Lippitz, Andreas A1 - Kamalakumar, A. A1 - Blanchard, V. A1 - Ivanov-Pankov, S. A1 - Weigel, W. A1 - Panne, Ulrich A1 - Unger, Wolfgang T1 - Surface chemical characterization of model glycan surfaces and shelf life studies of glycan microarrays using XPS, NEXAFS spectroscopy, ToF-SIMS and fluorescence scanning JF - Applied Surface Science N2 - Biomedical applications, including functional biomaterials, carbohydrate-arrays, and glycan-based biosensors. The chemistry of glycan immobilization plays an essential role in the bioavailability and function of surface bound carbohydrate moieties. For biomedical applications the stability over time (shelf life) of glycan arrays is a crucial factor. Herein we report on approaches for surface and interface characterization relevant to the needs of production of glycan microarrays which were tested using model carbohydrate surfaces. For detailed characterization of glycan model surfaces we used a combination of X-ray photoelectron spectroscopy (XPS), near edge X-ray absorption fine structure spectroscopy (NEXAFS) and ToF SIMS which are complementary techniques of surface chemical analysis. Links to fluorescence spectroscopy often used for characterization in the microarray community were established as well. In detail, amine-reactive silicon oxide and glass surfaces were used for anchoring oligosaccharides with an amino linker. The amount of surface bound carbohydrates was estimated by X-ray photoelectron spectroscopy (XPS). Glycan immobilization was investigated using lectins, which are glycan-binding molecules. A shelf life study of model glycan microarrays on epoxy-coated glass surfaces was done over a period of 160 days under different storage conditions utilizing fluorescence, ToF-SIMS and XPS analysis. It was shown that glycan activity of the models used can be maintained at least for half a year of storage at 4 °C. KW - Glycan microarray KW - XPS KW - NEXAFS KW - ToF-SIMS KW - Fluorescence PY - 2018 UR - https://www.sciencedirect.com/science/article/pii/S0169433218320300?via%3Dihub DO - https://doi.org/10.1016/j.apsusc.2018.07.133 SN - 0169-4332 SN - 1873-5584 VL - 459 SP - 860 EP - 873 PB - Elsevier B.V. AN - OPUS4-46212 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Min, Hyegeun A1 - Girard-Lauriault, Pierre-Luc A1 - Gross, Thomas A1 - Lippitz, Andreas A1 - Dietrich, Paul A1 - Unger, Wolfgang T1 - Ambient-ageing processes in amine self-assembled monolayers on microarray slides as studied by ToF-SIMS with principal component analysis, XPS, and NEXAFS spectroscopy JF - Analytical and bioanalytical chemistry N2 - We investigated the ageing of amine-terminated self-assembled monolayers (amine-SAMs) on different silica substrates due to exposure to different ambient gases, pressures, and/or temperatures using time-of-flight secondary ion mass spectrometry (ToF-SIMS) with principal component analysis and complementary methods of surface analysis as X-ray photoelectron spectroscopy (XPS) and near edge X-ray absorption fine structure (NEXAFS). The goal of this study is to examine the durability of primary amine groups of amine-SAMs stored in a user laboratory prior to being used as supports for biomolecule immobilization and other applications. We prepared amine-SAMs on the native oxides of silicon wafers and glass slides using 3- aminopropyl triethoxysilane, by using optimized conditions such as anhydrous organic solvent and reaction time scale of hours to avoid multilayer growth. Selected commercial amine-SAM slides have been investigated, too. When the amine-SAMs are exposed to air, oxygen incorporation occurs, followed by formation of amide groups. The formation of oxygen species due to ageing was proved by ToFSIMS, XPS, and NEXAFS findings such as CNO- secondary ion emission at m/z 42, observation of the N 1s HNC=O component peak at 400.2–400.3 eV in XPS, and, last but not least, by formation of a π*(HNC=O) resonance at 401 eV in the N K-edge X-ray absorption spectrum. It is concluded that the used multi-method approach comprising complementary ToF-SIMS, XPS, and NEXAFS analyses is well suited for a thorough study of chemical aspects of ageing phenomena of amine-SAM surfaces. KW - Amine-SAM KW - Ageing process KW - ToF-SIMS KW - NEXAFS KW - XPS PY - 2012 DO - https://doi.org/10.1007/s00216-012-5862-5 SN - 1618-2642 SN - 1618-2650 VL - 403 IS - 2 SP - 613 EP - 623 PB - Springer CY - Berlin AN - OPUS4-25829 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Girard-Lauriault, P.-L. A1 - Dietrich, Paul A1 - Gross, Thomas A1 - Wirth, Thomas A1 - Unger, Wolfgang T1 - Chemical characterization of the long-term ageing of nitrogen-rich plasma polymer films under various ambient conditions JF - Plasma processes and polymers N2 - Nitrogen rich plasma polymer films (L-PPE:N) were prepared by low-pressure RF plasma using a 1:1 mixture of ethylene and ammonia and aged for 345 d in four different ambient conditions: (i) at room temperature (RT) in air; (ii) at RT in nitrogen; (iii) at -20?°C in air and; (iv) at –20 °C in nitrogen. The films were analyzed by X-ray photoelectron spectroscopy (XPS) and by time-of-flight secondary ion mass spectrometry (ToF-SIMS) at various intervals over the duration of the experiment. The ageing of primary amines, NH2, was followed by chemical derivatization with 4-trifluoromethyl benzaldehyde. Storage at –20 °C, mostly independently of ambient atmosphere, slowed down ageing to almost undetectable levels as evaluated by the analytical methods used for this study. KW - Ageing KW - Plasma polymers KW - Primary amines KW - ToF-SIMS KW - XPS PY - 2013 DO - https://doi.org/10.1002/ppap.201200118 SN - 1612-8850 SN - 1612-8869 VL - 10 IS - 4 SP - 388 EP - 395 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-28006 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Funk, C. A1 - Dietrich, Paul A1 - Gross, Thomas A1 - Min, Hyegeun A1 - Unger, Wolfgang A1 - Weigel, W. T1 - Epoxy-functionalized surfaces for microarray applications: surface chemical analysis and fluorescence labeling of surface species JF - Surface and interface analysis N2 - Methods for characterization of epoxy-functionalized substrates used for microarray applications, prepared by silanization with 3-glycidoxypropyltrimethoxysilane, have been developed. Contact angle measurements, X-ray photoelectron spectroscopy, time of flight secondary ion mass spectrometry and fluorescence based methods have been applied to investigate these epoxy-functionalized microarray substrates. The surface density of epoxy-functionalized glass slides was investigated by fluorescence labeling of surface species utilizing Rhodamine 110 as fluorescence probe. KW - Epoxy silane KW - Microarrays KW - Fluorescence KW - XPS KW - ToF-SIMS KW - Surface analysis PY - 2012 DO - https://doi.org/10.1002/sia.3856 SN - 0142-2421 SN - 1096-9918 VL - 44 IS - 8 SP - 890 EP - 894 PB - Wiley CY - Chichester AN - OPUS4-26342 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dietrich, Paul A1 - Unger, Wolfgang T1 - Charakterisierung von Microarrays durch Anwendung physikalischer Methoden der chemischen Oberflächenanalytik JF - Analytik News KW - Oberflächenmodifizierungen KW - Self-assemblierende Monolagen KW - Thiole KW - Aminierte Oberflächen KW - Microarrays KW - XPS KW - ToF-SIMS PY - 2010 UR - http://www.analytik-news.de/Fachartikel/Volltext/BAM1.pdf SP - 1 EP - 11 PB - Dr. Beyer Internet-Beratung CY - Ober-Ramstadt AN - OPUS4-21834 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dietrich, Paul A1 - Horlacher, T. A1 - Gross, Thomas A1 - Wirth, Thomas A1 - Castelli, R. A1 - Shard, A.G. A1 - Alexander, M. A1 - Seeberger, P.H. A1 - Unger, Wolfgang T1 - Surface analytical characterization of carbohydrate microarrays JF - Surface and interface analysis N2 - Microarrays are a versatile platform for diagnostics and high-throughput analysis. Carbohydrate microarrays are valuable tools to investigate interactions with other molecules since many glycans are involved in fundamental biological processes. A combined X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS) surface analysis was used to investigate the basic steps in the production of carbohydrate microarrays. The preparation included coupling of a thiol-terminated mannoside to maleimide-functionalized glass surfaces derived from γ-aminopropyl silane (GAPS) slides. XPS results clearly demonstrate successful chemical modification in each fabrication step, and ToF-SIMS imaging revealed immobilized carbohydrates in the spotted regions of the final microarray. KW - Carbohydrates KW - Microarrays KW - XPS KW - ToF-SIMS KW - Nona-mannoside KW - Maleimide surfaces KW - Surface analysis PY - 2010 DO - https://doi.org/10.1002/sia.3255 SN - 0142-2421 SN - 1096-9918 VL - 42 SP - 1188 EP - 1192 PB - Wiley CY - Chichester AN - OPUS4-21500 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dietrich, Paul A1 - Horlacher, T. A1 - Girard-Lauriault, Pierre-Luc A1 - Gross, Thomas A1 - Lippitz, Andreas A1 - Min, Hyegeun A1 - Wirth, Thomas A1 - Castelli, R. A1 - Seeberger, P.H. A1 - Unger, Wolfgang T1 - Adlayers of dimannoside thiols on gold: surface chemical analysis JF - Langmuir N2 - Carbohydrate films on gold based on dimannoside thiols (DMT) were prepared, and a complementary surface chemical analysis was performed in detail by X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS), near-edge X-ray absorption fine structure (NEXAFS), FT-IR, and contact angle measurements in order to verify formation of ω-carbohydrate-functionalized alkylthiol films. XPS (C 1s, O 1s, and S 2p) reveals information on carbohydrate specific alkoxy (C–O) and acetal moieties (O–C–O) as well as thiolate species attached to gold. Angle-resolved synchrotron XPS was used for chemical speciation at ultimate surface sensitivity. Angle-resolved XPS analysis suggests the presence of an excess top layer composed of unbound sulfur components combined with alkyl moieties. Further support for DMT attachment on Au is given by ToF-SIMS and FT-IR analysis. Carbon and oxygen K-edge NEXAFS spectra were interpreted by applying the building block model supported by comparison to data of 1-undecanethiol, poly(vinyl alcohol), and polyoxymethylene. No linear dichroism effect was observed in the angle-resolved C K-edge NEXAFS. KW - Carbohydrates KW - Self-assembled monolayer KW - XPS KW - NEXAFS KW - ToF-SIMS KW - Surface chemical analysis PY - 2011 DO - https://doi.org/10.1021/la104038q SN - 0743-7463 SN - 1520-5827 VL - 27 IS - 8 SP - 4808 EP - 4815 PB - American Chemical Society CY - Washington, DC AN - OPUS4-23554 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dietrich, Paul A1 - Horlacher, T. A1 - Girard-Lauriault, Pierre-Luc A1 - Gross, Thomas A1 - Lippitz, Andreas A1 - Min, Hyegeun A1 - Wirth, Thomas A1 - Castelli, R. A1 - Seeberger, P. A1 - Unger, Wolfgang T1 - Multimethod chemical characterization of carbohydrate-functionalized surfaces JF - Journal of carbohydrate chemistry N2 - A combined XPS, NEXAFS, and ToF-SIMS chemical surface characterization of carbohydrate-functionalized gold and glass surfaces is presented. Spot shape and chemical composition across a spot surface are provided by surface-sensitive methods as ToF-SIMS and XPS, used in their imaging modes. Moreover, the feasibility of this multimethod approach to control relevant production steps of a carbohydrate microarray prototype is demonstrated. KW - Carbohydrates KW - Microarrays KW - Self-assembled monolayers KW - XPS KW - NEXAFS KW - ToF-SIMS PY - 2011 DO - https://doi.org/10.1080/07328303.2011.615181 SN - 0732-8303 VL - 30 IS - 4-6 SP - 361 EP - 372 PB - Taylor & Francis CY - London [u.a.] AN - OPUS4-24874 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -