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Issue 31, 2017
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Chromatographic separation and mass spectrometric analysis of N-acetyl-L-cysteine-protected palladium nanoparticles

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In this study, water-soluble N-acetyl-L-cysteine-protected palladium nanoparticles (NAC-PdNPs) were synthesised. The obtained NAC-PdNPs were well characterised by UV-vis absorption spectroscopy, infrared spectroscopy, X-ray photoelectron spectroscopy, and transmission electron microscopy. The as-synthesised NAC-PdNPs were found to be polydisperse in nature with an average particle size of 2.17 ± 0.20 nm. As such, a reverse-phase high-performance liquid chromatographic (RP-HPLC) methodology coupled with UV-vis absorption detection has been developed for separating and analysing this as-synthesised NAC-PdNPs product. A gradient elution program with mobile phase mixtures of methanol/water containing 50 mM tetrabutylammonium fluoride was successfully applied to separate the as-synthesised NAC-PdNPs sample. The spectral characteristics of each RP-HPLC-separated NAC-PdNPs fractions were captured online using a diode array detector. In addition, most major RP-HPLC fractions were collected and further characterised by matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI-TOF MS) in order to elucidate their chemical compositions. The mass spectra suggest that the NAC-PdNPs as-synthesised product is indeed a complex mixture of small PdNPs comprising Pd10(NAC)7, Pd11(NAC)7, Pd11(NAC)8, Pd12(NAC)9, Pd13(NAC)6, Pd13(NAC)9, Pd14(NAC)5, Pd14(NAC)9, Pd15(NAC)9, Pd17(NAC)11, and Pd20(NAC)11. The UV-vis spectral characteristics of the separated NAC-PdNPs are closely related to the number of Pd atoms. This study highlights the values of using high-resolution chromatography together with UV-vis absorption spectroscopy and MALDI-TOF MS for revealing the hidden properties of each individual PdNPs species in a PdNPs product.

Graphical abstract: Chromatographic separation and mass spectrometric analysis of N-acetyl-l-cysteine-protected palladium nanoparticles

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Publication details

The article was received on 05 May 2017, accepted on 07 Jul 2017 and first published on 10 Jul 2017

Article type: Paper
DOI: 10.1039/C7AY01146F
Citation: Anal. Methods, 2017,9, 4539-4546
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    Chromatographic separation and mass spectrometric analysis of N-acetyl-L-cysteine-protected palladium nanoparticles

    L. Zhang, Q. Hu, Z. Li, Y. Zhang, D. Lu, S. Shuang, Martin M. F. Choi and C. Dong, Anal. Methods, 2017, 9, 4539
    DOI: 10.1039/C7AY01146F

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