Applicability of Imaging Time-of Flight Secondary Ion MS to the Characterization of Solid-Phase Synthesized Combinatorial Libraries

Jiyun Y. Xu, Robert M. Braun, Nicholas Winograd

Research output: Contribution to journalArticle

10 Citations (Scopus)

Abstract

We employ imaging time-of-flight secondary ion mass spectrometry to perform high-throughput analysis of solid-phase synthesized combinatorial libraries by acquiring mass spectra from arrays of polymer resin particles. To generalize this procedure to various types of resins and their associated chemical linkers, it is necessary to understand the dynamics associated with the analyte molecules during chemical pretreatment steps. Using stearic acid as a model compound, we examine the influence of three classes of linkers-acid or base labile linkers, a thermally labile linker, and a photochemically cleavable linker-all of which are used to anchor one end of the analyte to the polymer resin. With data obtained using secondary ion mass spectrometry, scanning electron microscopy, and X-ray photoelectron spectroscopy, we conclude that an effective treatment of the resin needs to include cleaving the linker and extracting the unbound analyte to the resin surface. We also demonstrate that the hydrophilicity of the polymeric constituents of a resin particle affects the experiments by changing the location of the analyte molecules during resin treatment. With this information, it is possible to utilize imaging TOF-SIMS to assay a range of material supports with assurance that high-quality spectra can be acquired.

Original languageEnglish (US)
Pages (from-to)6155-6162
Number of pages8
JournalAnalytical Chemistry
Volume75
Issue number22
DOIs
StatePublished - Nov 15 2003

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Resins
Ions
Imaging techniques
Secondary ion mass spectrometry
Polymers
Molecules
Hydrophilicity
Anchors
Assays
X ray photoelectron spectroscopy
Throughput
Scanning electron microscopy
Acids
Experiments

All Science Journal Classification (ASJC) codes

  • Analytical Chemistry

Cite this

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title = "Applicability of Imaging Time-of Flight Secondary Ion MS to the Characterization of Solid-Phase Synthesized Combinatorial Libraries",
abstract = "We employ imaging time-of-flight secondary ion mass spectrometry to perform high-throughput analysis of solid-phase synthesized combinatorial libraries by acquiring mass spectra from arrays of polymer resin particles. To generalize this procedure to various types of resins and their associated chemical linkers, it is necessary to understand the dynamics associated with the analyte molecules during chemical pretreatment steps. Using stearic acid as a model compound, we examine the influence of three classes of linkers-acid or base labile linkers, a thermally labile linker, and a photochemically cleavable linker-all of which are used to anchor one end of the analyte to the polymer resin. With data obtained using secondary ion mass spectrometry, scanning electron microscopy, and X-ray photoelectron spectroscopy, we conclude that an effective treatment of the resin needs to include cleaving the linker and extracting the unbound analyte to the resin surface. We also demonstrate that the hydrophilicity of the polymeric constituents of a resin particle affects the experiments by changing the location of the analyte molecules during resin treatment. With this information, it is possible to utilize imaging TOF-SIMS to assay a range of material supports with assurance that high-quality spectra can be acquired.",
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Applicability of Imaging Time-of Flight Secondary Ion MS to the Characterization of Solid-Phase Synthesized Combinatorial Libraries. / Xu, Jiyun Y.; Braun, Robert M.; Winograd, Nicholas.

In: Analytical Chemistry, Vol. 75, No. 22, 15.11.2003, p. 6155-6162.

Research output: Contribution to journalArticle

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