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Updated: Apr 13, 2026
Laser-induced Breakdown Spectroscopy: A New Approach for Nanoparticle's Mapping and Quantification in Organ Tissue
Published on: June 18, 2014
X-ray analysis on the nanogram to microgram scale using porous complexes.
Yasuhide Inokuma1, Shota Yoshioka, Junko Ariyoshi
1Department of Applied Chemistry, Graduate School of Engineering, The University of Tokyo, Hongo, Bunkyo-ku, Tokyo, 113-8656, Japan.
This study introduces a novel X-ray single-crystal diffraction (SCD) method that bypasses the need for sample crystallization. This technique allows for the structural determination of molecules using only nanogram-microgram quantities, significantly reducing sample requirements.
Area of Science:
- Crystallography and Structural Biology
- Analytical Chemistry
- Materials Science
Background:
- Traditional X-ray single-crystal diffraction (SCD) requires obtaining target molecules as single crystals, a process that is often challenging and time-consuming.
- This limitation restricts the application of SCD for analyzing samples that are difficult to crystallize or available in very small quantities.
Purpose of the Study:
- To develop a novel protocol for SCD analysis that eliminates the necessity for sample crystallization.
- To enable the structural characterization of molecules using significantly reduced sample amounts (nanogram-microgram scale).
- To integrate SCD with liquid chromatography for direct analysis of separated fractions.
Main Methods:
- A new protocol involving soaking tiny crystals of porous host complexes in a solution containing the target molecules.
- The porous complexes absorb the target molecules, allowing their structures to be determined within the host framework via SCD.
- Combination of the developed SCD protocol with high-performance liquid chromatography (HPLC) for analyzing multiple eluted fractions.
Main Results:
- Successful structural determination of absorbed guest molecules within host frameworks using SCD without prior crystallization of the target.
- Demonstrated the ability to perform SCD with as little as approximately 80 nanograms of sample.
- Established a direct characterization method for multiple HPLC fractions, termed liquid chromatography SCD analysis.
- Unambiguously determined the structure of a scarce marine natural product using only 5 micrograms of the compound.
Conclusions:
- The developed protocol significantly broadens the applicability of SCD by removing the crystallization prerequisite.
- This method offers a highly sensitive approach for structural analysis, requiring minimal sample mass.
- The integration with HPLC provides a powerful tool for the direct characterization of complex mixtures and scarce compounds.
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