Structure elucidation of nanoparticle-bound organic molecules by 1H NMR

Du, Fenfang; Zhou, Hongyu; Chen, Lingxin; Zhang, Bin; Yan, Bing

doi:10.1016/j.trac.2008.10.010

Cited by 30 publications

(18 citation statements)

References 69 publications

(68 reference statements)

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“…However, the more challenging task is the development of analytical methodologies 69,70 to characterize surface chemistry of nanomaterials. The strategy to overcome these difficulties bears some similarity to early analytical issues in combinatorial chemistry.…”

Section: Perspectives and Future Challengesmentioning

confidence: 99%

Nano-Combinatorial Chemistry Strategy for Nanotechnology Research

Yan

2010

J. Comb. Chem.

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Nanotechnology refers to the creation of functional materials, devices, and systems through the control of matter on the nanometer scale, and the exploitation of novel phenomena and properties at that scale. 1 Advances in nanotechnology will have tremendous impacts on every aspect of our society. [2][3][4] The discovery and optimization of novel nanomaterials with unique properties require a time-consuming research effort. Parallel reactions and screenings are deemed to be more efficient than conventional linear operations. Combinatorial chemistry has already revolutionized drug discovery and the discovery of materials, catalysts, polymers, and pesticide. It has recently also made a significant impact on nanotechnology.Combinatorial and high-throughput approaches afford several advantages in discovery research, including decreased costs and increased efficiency. This perspective will review diverse applications of combinatorial and high-throughput approaches in nanotechnology research ( Figure 1). Combinatorial approaches applied in nanotechnology are reviewed in three aspects: First, combinatorial libraries are developed for optimization of synthesis conditions, such as combinatorial catalyst libraries developed to optimize the growth conditions of carbon nanotubes (CNTs). Second, synthesis of library of nanomaterials with different chemical compositions or sizes to discover materials with desired properties, such as combinatorial thin film libraries screened for unique properties. Third, library made by surface chemistry modifications to discover materials with suitable properties for applications in certain field such as medicine and diagnostics. As important as the library synthesis methods, highthroughput screening (HTS) methods have also been developed to evaluate the targeted properties of the libraries efficiently. Significant opportunities and challenges of applying nano-combinatorial chemistry approaches are also discussed. Combinatorial Approaches in Nanomaterial DiscoveryCombinatorial approaches employ parallel and highthroughput methods for discovery of nanomaterials with unique properties. The successful application of combinatorial approaches in nanomaterial discovery are demonstrated in three examples: catalysts for carbon nanotubes growth, thin films, and novel polymer carriers for gene delivery. Combinatorial Catalyst Libraries for Controlling the Growth of CNTs.CNTs are grown mainly by chemical vapor deposition (CVD) on substrates with transition metal catalysts. Controlling the growth of CNTs is essential for their nanoscale manipulation and their applications. 5 The growth of singlewalled carbon nanotubes (SWCNTs) and multiwalled carbon nanotubes (MWCNTs) were optimized by catalyst libraries produced by tuning composition of three components: metal salts as catalysts, SiCl 4 or AlCl 3 as substrate-forming components, and triblock copolymers as "structure-directing agents". 6,7 Another similar study demonstrated that the structuring agent was not controlling the size of the catalyst particle b...

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Section: Perspectives and Future Challengesmentioning

confidence: 99%

Nano-Combinatorial Chemistry Strategy for Nanotechnology Research

Yan

2010

J. Comb. Chem.

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“…However, in reality, building such structures into the desired molecules is a synthetic challenge. Therefore, we found that routine NMR spectroscopy can monitor reaction and the product formation, but is not an ideal method for full structure elucidation of organic molecules on the surface of NPs [24]. …”

Section: Nuclear Magnetic Resonance Spectroscopy (Nmr)mentioning

confidence: 99%

Analytical strategies for characterizing the surface chemistry of nanoparticles

Zhang

Yan

2009

Anal Bioanal Chem

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Chemical modifications of nanoparticle (NP) surface are likely to regulate their activities, remove their toxic effects, and enable them to perform desired functions. It is urgent to develop analytical strategies for acquiring structural and quantitative information on small molecules linked to the surface of NP. Recent progresses on characterizing nanoparticle's surface chemistry using nuclear magnetic resonance spectroscopy (NMR), Fourier transform infrared absorbance spectroscopy (FTIR), liquid chromatography-mass spectroscopy (LC-MS), X-Ray photoelectron spectroscopy (XPS), and combustion elemental analysis are reviewed. Modified NPs need to be characterized rigorously regarding the integrity of the chemistry. However, identification and quantification of small molecules linked to the surface of NPs are very challenging due to the fact that they are solid-phase samples and they are coated with only a small amount of small molecules. This has become a roadblock limiting our ability to do chemical modifications of nanomaterials. For this technical difficulty, many previous publications did not thoroughly characterize modified NPs before doing biological testing. On the other hand, biological experiments require precise quantity/ concentration information to obtain dose-response relationship. The lack of accurate concentration information makes the biological studies qualitative at best.Recently, efforts have been made to fill this gap. In this review, we focus on recent development of multiple analytical techniques, such as nuclear magnetic resonance spectroscopy (NMR), Fourier transform infrared absorbance spectroscopy (FTIR), liquid chromatography-mass spectroscopy (LC-MS), X-Ray photoelectron spectroscopy (XPS), and combustion elemental 901-495-2797, Dr.bingyan@gmail.com. analysis and explain how these techniques help identify and quantify molecules attached to NP's surface. The continued efforts in this field will pave the way to make the wider biomedical application of nanomaterials possible. NIH Public Access

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“…Therefore, the need for accurate identification of molecules bound to nanomaterials is essential. 12 …”

Section: Introductionmentioning

confidence: 99%

Characterizing Covalently Sidewall-Functionalized Single-Walled Carbon Nanotubes by Using¹H NMR Spectroscopy

Nelson

Kumar

2013

J. Phys. Chem. C

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Unambiguous evidence for covalent sidewall functionalization of single-walled carbon nanotubes (SWCNTs) has been a difficult task, especially for nanomaterials in which slight differences in functionality structure produce significant changes in molecular characteristics. Nuclear magnetic resonance (NMR) spectroscopy provides clear information about the structural skeleton of molecules attached to SWCNTs. In order to establish the generality of proton NMR as an analytical technique for characterizing covalently functionalized SWCNTs, we have obtained and analyzed proton NMR data of SWCNT-substituted benzenes across a variety of para substituents. Trends obtained for differences in proton NMR chemical shifts and the impact of o-, p-, and m-directing effects of electrophilic aromatic substituents on phenyl groups covalently bonded to SWCNTs are discussed.

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Structure elucidation of nanoparticle-bound organic molecules by 1H NMR

Cited by 30 publications

References 69 publications

Nano-Combinatorial Chemistry Strategy for Nanotechnology Research

Nano-Combinatorial Chemistry Strategy for Nanotechnology Research

Analytical strategies for characterizing the surface chemistry of nanoparticles

Characterizing Covalently Sidewall-Functionalized Single-Walled Carbon Nanotubes by Using¹H NMR Spectroscopy

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Structure elucidation of nanoparticle-bound organic molecules by 1H NMR

Cited by 30 publications

References 69 publications

Nano-Combinatorial Chemistry Strategy for Nanotechnology Research

Nano-Combinatorial Chemistry Strategy for Nanotechnology Research

Analytical strategies for characterizing the surface chemistry of nanoparticles

Characterizing Covalently Sidewall-Functionalized Single-Walled Carbon Nanotubes by Using1H NMR Spectroscopy

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Characterizing Covalently Sidewall-Functionalized Single-Walled Carbon Nanotubes by Using¹H NMR Spectroscopy